LU503124B1 - Preparation method and application of bismuth oxysulfide photocatalyst modified by surface iodination - Google Patents
Preparation method and application of bismuth oxysulfide photocatalyst modified by surface iodination Download PDFInfo
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- LU503124B1 LU503124B1 LU503124A LU503124A LU503124B1 LU 503124 B1 LU503124 B1 LU 503124B1 LU 503124 A LU503124 A LU 503124A LU 503124 A LU503124 A LU 503124A LU 503124 B1 LU503124 B1 LU 503124B1
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- photocatalyst
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- bismuth
- oxysulfide
- surface iodination
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- MKKCJTYKJLHFJO-UHFFFAOYSA-N [Bi].S=O Chemical compound [Bi].S=O MKKCJTYKJLHFJO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 230000026045 iodination Effects 0.000 title claims abstract description 33
- 238000006192 iodination reaction Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims abstract description 9
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 20
- 238000007540 photo-reduction reaction Methods 0.000 abstract description 10
- 230000004048 modification Effects 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 10
- 230000009467 reduction Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- -1 iodide modified bismuth oxysulfide Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
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- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
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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
- 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
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- C07C2523/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- C07C2523/18—Arsenic, antimony or bismuth
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Abstract
The invention relates to a preparation method of a bismuth oxysulfide photocatalyst with surface iodination modification for clean energy conversion, belonging to the field of new materials for environmental catalysis. The preparation method of that material comprises the following step: 1, taking bismuth nitrate pentahydrate, thiourea, lithium hydroxide monohydrate, water and potassium iodide as raw materials, and carry out hydrothermal reaction to obtain bismuth oxysulfide photocatalyst with surface iodination modification. The invention has the advantages that the bismuth oxysulfide photocatalyst with surface iodination modification is obtained through a simple and easy preparation process, which has high photo-generated carrier separation efficiency and the ability for the adsorption and activation of CO2, and has excellent photocatalytic performance of visible light-driven CO2 photo-reduction to CH4 under 99% CO2 atmosphere and good cycle stability.
Description
PREPARATION METHOD AND APPLICATION OF BISMUTH HUS03T24
OXYSULFIDE PHOTOCATALYST MODIFIED BY SURFACE IODINATION
The invention relates to a preparation method of a bismuth oxysulfide photocatalyst with surface iodination modification for clean energy conversion, belonging to the field of new materials for environmental catalysis.
The explosive development of modern industry and science and technology has provided unprecedented material life foundation for today's human beings, but it has been followed by the rapid consumption of fossil fuels, intensified greenhouse effect and serious environmental pollution. These problems have seriously restricted the economic and social development of mankind, and have become an important problem and severe test that the world is facing today. It is necessary to develop a green and efficient technology for environmental pollution control and environmental energy conversion. Photocatalytic technology is a new technology which takes clean and endless solar energy as the driving force for reaction. At present, the research and application of photocatalytic technology focus on three aspects: new technologies of pollutant treatment, renewable clean energy conversion and green chemical synthesis, which can fundamentally alleviate the problems of energy crisis, greenhouse effect and environmental pollution. The research core of photocatalysis technology is to design and synthesize efficient and stable semiconductor photocatalyst according to its application environment and object. After being excited by photon energy, these semiconductor photocatalysts generate active free radicals with strong oxidizing and reducing properties on their surfaces. These active substances can not only efficiently degrade pollutants in the environment, but also decompose water to produce hydrogen, convert carbon dioxide into chemical raw materials and fuels such as carbon monoxide, methanol and methane, and reduce nitrogen to produce ammonia. They have broad development space in the fields of environmental treatment, clean energy production and green chemical industry. However, the catalytic activity of HUS03T24 semiconductor photocatalytic materials is usually limited by light utilization rate and photo-generated carrier separation efficiency. Therefore, improving the separation efficiency of photo-generated carriers through microstructure control and developing photocatalyst with broad spectral response are effective means to achieve efficient photocatalysis.
Bismuth oxysulfide layered material Bi20,X (X= S, Se, Te) has also attracted more and more attention recently. Bi2O:S is an orthogonal crystal layered structure with Pnnm space group, and its band gap is about 1.5 eV, which has the characteristics of carrier separation, high transmission efficiency and long carrier life. Bi2OsS is usually prepared by a complex solid-state high-temperature method, which takes a long time, and the purity of the obtained Bi:O2S sample cannot be guaranteed. In addition, Bi:OzS is mainly used in ferroelectric, thermoelectric, photoelectric devices, supercapacitors and other fields, but little research has been done in the field of photocatalysis. Therefore, its microstructure, optical, photoelectric and other properties as a photocatalyst, as well as the mechanism of its participation in photocatalytic reaction need to be explored urgently.
The technical problem to be solved by the invention is to provide a preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion, aiming at the shortcomings of the prior art. The bismuth oxysulfide photocatalyst modified by surface iodination prepared by the method has excellent photocatalytic performance of reducing CO: into CH4 under 99% CO: atmosphere irradiated by visible light, and the preparation and operation process are simple.
The invention relates to a preparation method of a bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion, which comprises the surface iodide modified bismuth oxysulfide photocatalyst with the mass fraction of potassium iodide of 0.5 wt.%, 2.0 wt.% and 8.0 wt.%.
In order to realize the above invention, the technical scheme adopted by the HUS03T24 invention is as follows:
A preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion comprises: (1) weighing 1.9403 g of bismuth nitrate pentahydrate and 0.1522 g of thiourea and dissolving in 60 ml of deionized water, and fully stirring; (2) weighing 12 g of lithium hydroxide monohydrate, adding into the mixed solution of (1), and fully stirring; (3) weighing 0.5 wt.%, 2.0 wt.% and 8.0 wt.% potassium iodide into the mixed solution of (2) and fully stirring; (4) transferring the mixed solution in (3) into a hydrothermal autoclave, performing hydrothermal reaction at 200°C for 72 hours, and cooling to obtain a purple-black precipitate; and (5) washing and drying the reaction product obtained in (4) to obtain the bismuth oxysulfide photocatalyst modified by surface iodination.
In the above scheme, the volume of the solution is 60 ml.
In the above scheme, the mass of lithium hydroxide monohydrate is 12 g.
In the above scheme, the mass fraction of potassium iodide added is 0.5 wt.%, 2.0 wt.% and 8.0 wt.%.
In the above scheme, the hydrothermal temperature is 200°C.
In the above scheme, the hydrothermal time is 72 h.
Compared with the prior art, the invention has the following beneficial effects:
The preparation of bismuth oxysulfide photocatalyst modified by surface iodination adopts hydrothermal method, which is relatively simple, safe, efficient. The obtained bismuth oxysulfide photocatalyst modified by surface iodination has high photo-generated carrier separation efficiency and the adsorption and activation ability for CO», and has excellent photocatalytic performance of CO» photo-reduction to CH4 and good cycle stability under 99% CO; atmosphere irradiated by visible light.
BRIEF DESCRIPTION OF THE FIGURES 009128
Fig. 1 is the XRD spectra of 0.5%IBOS, 2.0%IBOS, 8.0%IBOS of bismuth oxysulfide photocatalyst modified by surface iodination and BIOS bismuth oxysulfide photocatalyst unmodified by different surface iodination contents in Examples 1 to 3.
Fig. 2 shows the photo-reduction effects of 0.5%IBOS, 2.0%IBOS, 8.0%IBOS and bismuth oxysulfide photocatalyst BiOS unmodified by different surface iodination contents in Examples 1-3, respectively, to convert CO, into CH4 under visible light irradiation of 99% CO» atmosphere.
Fig. 3 is the effect diagram of the cyclic experiment of the best bismuth oxysulfide photocatalyst modified by surface iodination 2.0%IBOS in the visible light irradiation of 99% CO, atmosphere to convert CO; into CHa.
Fig. 4 is the SEM image of 2.0%IBOS of bismuth oxysulfide photocatalyst modified by best surface iodination in this embodiment.
In order to better understand the present invention, the content of the present invention will be further illustrated in the following examples, but the content of the present invention is not limited to the following examples.
The specific operation steps for testing the photocatalytic CO» reduction performance of the prepared photocatalyst in 99% CO; atmosphere are as follows: add 30 mg of photocatalyst to be measured into a glass culture dish with a diameter of about 5 cm, then add 2 ml of deionized water into it, then put the culture dish in an ultrasonic instrument for ultrasonic treatment for 5 min, so that the samples to be measured are uniformly dispersed in the culture dish, and finally put the culture dish in an oven with a temperature of 70°C for drying, so that the dried samples are uniformly distributed on the culture dish; put the dried Petri dish containing samples on the upper layer of a 200 ml reactor with quartz glass window, then add 1.2 g anhydrous Na,COs to the bottom of the reactor, and further seal the reactor with vacuum grease; then, pump out the air in the reactor by vacuum pump, and then introduce nitrogen into the reactor to completely remove the air in the reactor; after the air in the reactor is removed, inject 2 ml H>SO4(1:1) into the reactor to generate HUS03T24
CO; gas; when Na:CO; reacts with H,SO4 completely, turn on the light source (300
W xenon lamp/420 nm filter) for photocatalytic CO; reduction reaction. The product and its content of the photocatalytic reduction of CO; are detected by GC-7820 of 5 Zhongkehuifen, and the average value was obtained after three tests each time.
Example 1
A preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion includes the following steps: (1) weighing 1.9403 g of bismuth nitrate pentahydrate and 0.1522 g of thiourea and dissolving in 60 ml of deionized water, and fully stirring; (2) weighing 12 g of lithium hydroxide monohydrate, adding into the mixed solution of step (1), and fully stirring; (3) weighing 0.5 wt.% potassium iodide, adding it into the mixed solution of step (2), and fully stirring; (4) transferring the mixed solution in step (3) into a hydrothermal autoclave, performing hydrothermal reaction at 200°C for 72 hours, and cooling to obtain a purple-black precipitate; and (5) washing and drying the reaction product obtained in the step (4) to obtain the bismuth oxysulfide photocatalyst with surface iodination modification.
Fig. 1 is the XRD pattern of 0.5%IBOS of bismuth oxysulfide photocatalyst prepared by the present invention. The XRD diffraction peak position of 0.5%IBOS sample is the same as the standard peak position of BiOS (PDF No. 34-1493), which indicates that the phase of BiOS in the modified photocatalyst has not changed, and no other impurities have been generated.
In the photocatalytic CO» reduction experiment of 0.5%IBOS catalyst synthesized in this example in 99% CO, atmosphere, the light source is 300 W xenon lamp with visible light, and the yield of CO, photoreduction to CH4 in 90 min is 72.78 umol/g; however, the yield of CO, photoreduction to CH4 in the unmodified BiOS is 23.59 umol/g (see Fig. 2), which indicates that the bismuth oxysulfide photocatalyst
0.5%IBOS prepared by this method has good photocatalytic activity for CO» 509724 reduction under 99% CO», atmosphere irradiated by visible light.
Example 2
A preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion includes the following steps: (1) weighing 1.9403 g of bismuth nitrate pentahydrate and 0.1522 g of thiourea and dissolving in 60 ml of deionized water, and fully stirring; (2) weighing 12 g of lithium hydroxide monohydrate, adding into the mixed solution of step (1), and fully stirring; (3) weighing 2.0 wt.% potassium iodide, adding it into the mixed solution of step (2), and fully stirring; (4) transferring the mixed solution in step (3) into a hydrothermal autoclave, performing hydrothermal reaction at 200°C for 72 hours, and cooling to obtain a purple-black precipitate; and (5) washing and drying the reaction product obtained in the step (4) to obtain the bismuth oxysulfide photocatalyst with surface iodination modification.
Fig. 1 is the XRD pattern of 2.0%IBOS of bismuth oxysulfide photocatalyst prepared by the present invention. The XRD diffraction peak position of 2.0%IBOS sample is the same as the standard peak position of BiOS (PDF No. 34-1493), which indicates that the phase of BiOS in the modified photocatalyst has not changed, and no other impurities have been generated.
In the photocatalytic CO» reduction experiment of 2.0%IBOS catalyst synthesized in this example in 99% CO, atmosphere, the light source is 300 W xenon lamp with visible light, and the yield of CO; photoreduction to CH4 in 90 min is 80.50 umol/g; however, the yield of CO, photoreduction to CH4 in the unmodified BiOS is 3.59 umol/g (see Fig. 2), which indicates that the bismuth oxysulfide photocatalyst 2.0%IBOS prepared by this method has good photocatalytic activity for CO, reduction under 99% CO» atmosphere irradiated by visible light.
Example 3 LU503124
A preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion includes the following steps: (1) weighing 1.9403 g of bismuth nitrate pentahydrate and 0.1522 g of thiourea and dissolving in 60 ml of deionized water, and fully stirring; (2) weighing 12 g of lithium hydroxide monohydrate, adding into the mixed solution of step (1), and fully stirring; (3) weighing 8.0 wt.% potassium iodide, adding it into the mixed solution of step (2), and fully stirring; (4) transferring the mixed solution in step (3) into a hydrothermal autoclave, performing hydrothermal reaction at 200°C for 72 hours, and cooling to obtain a purple-black precipitate; and (5) washing and drying the reaction product obtained in the step (4) to obtain the bismuth oxysulfide photocatalyst with surface iodination modification.
Fig. 1 is the XRD pattern of 8.0%IBOS of bismuth oxysulfide photocatalyst prepared by the present invention. The XRD diffraction peak position of 8.0%IBOS sample is the same as the standard peak position of BiOS (PDF No. 34-1493), which indicates that the phase of BiOS in the modified photocatalyst has not changed, and no other impurities have been generated.
In the photocatalytic CO» reduction experiment of 8.0%IBOS catalyst synthesized in this example in 99% CO, atmosphere, the light source is 300 W xenon lamp with visible light, and the yield of CO, photoreduction to CH4 in 90 min is 19.56 umol/g; however, the yield of CO, photoreduction to CH4 in the unmodified BiOS is 3.59 umol/g (see Fig. 2), which indicates that the bismuth oxysulfide photocatalyst 8.0%IBOS prepared by this method has good photocatalytic activity for CO» reduction under 99% CO» atmosphere irradiated by visible light.
Fig. 1 is the XRD spectra of 0.5%IBOS, 2.0%IBOS, 8.0%IBOS of bismuth oxysulfide photocatalyst modified by surface iodination and BiOS bismuth oxysulfide photocatalyst unmodified by different surface iodination contents. The XRD diffraction peak position of bismuth oxysulfide photocatalyst sample modified by iodination is the same as the standard peak position of BIOS(PDFNo. 34-1493), which HUS03T24 indicates that the BiOS phase of the modified photocatalyst has not changed and no other impurities have been generated.
Fig. 2 shows the photo-reduction effects of 0.5%IBOS, 2.0%IBOS, 8.0%IBOS and bismuth oxysulfide photocatalyst BIOS unmodified by different surface iodination contents in Examples 1-3, respectively, to convert CO, into CH4 under visible light irradiation of 99% CO, atmosphere. Fig. 2 shows that the bismuth oxysulfide photocatalyst modified by surface iodination prepared by this method has good photocatalytic CO; reduction activity under 99% CO, atmosphere irradiated by visible light, which is higher than that of unmodified BIOS.
Fig. 3 is the effect diagram of the cyclic experiment of the best bismuth oxysulfide photocatalyst modified by surface iodination 2.0%IBOS in the visible light irradiation of 99% CO, atmosphere to convert CO; into CHs. Fig. 3 shows that the bismuth oxysulfide photocatalyst prepared by this method has good photocatalytic
CO» reduction cycle stability under visible light irradiation.
Fig. 4 is the SEM image of 2.0%IBOS of bismuth oxysulfide photocatalyst modified by best surface iodination in this embodiment. As shown in Figure 4, the 2.0%IBOS sample has a regular brick-like morphology.
Obviously, the above-mentioned embodiment is only an example for clear explanation, and is not a limitation to the implementation. For those of ordinary skill in the art, other changes or variations can be made on the basis of the above description. It is not necessary and impossible to exhaust all the embodiments here.
Therefore, the extended obvious changes or variations are still within the scope of protection of the invention.
Claims (6)
1. À preparation method of bismuth oxysulfide photocatalyst modified by surface iodination for clean energy conversion, characterized by comprising: (1) weighing 1.9403 g of bismuth nitrate pentahydrate and 0.1522 g of thiourea, dissolving in 60 ml of deionized water, and fully stirring; (2) weighing 12 g of lithium hydroxide monohydrate, adding into the mixed solution of (1), and fully stirring; (3) weighing 0.5 wt.%, 2.0 wt.% and 8.0 wt.% potassium iodide into the mixed solution of (2) and fully stirring; (4) transferring the mixed solution in (3) into a hydrothermal autoclave, performing hydrothermal reaction at 200°C for 72 hours, and cooling to obtain a purple-black precipitate; and (5) washing and drying the reaction product obtained in (4) to obtain the bismuth oxysulfide photocatalyst modified by surface iodination.
2. The preparation method according to claim 1, characterized in that in (1), the volume of the solution is 60 ml.
3. The preparation method according to claim 1, characterized in that in (2), the mass of lithium hydroxide monohydrate is 12 g.
4. The preparation method according to claim 1, characterized in that in (3), the mass fraction of potassium iodide added is 0.5 wt.%, 2.0 wt.% and 8.0 wt.%.
5. The preparation method according to claim 1, characterized in that in (4), the hydrothermal temperature is 200°C.
6. The preparation method according to claim 1, characterized in that in (4), the hydrothermal time is 72 h.
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| CN118454695A (en) * | 2024-07-10 | 2024-08-09 | 中国市政工程西北设计研究院有限公司 | Heterojunction composite material for catalyzing hydrogen evolution and preparation method and application thereof |
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| CN118454695A (en) * | 2024-07-10 | 2024-08-09 | 中国市政工程西北设计研究院有限公司 | Heterojunction composite material for catalyzing hydrogen evolution and preparation method and application thereof |
| CN118454695B (en) * | 2024-07-10 | 2024-09-03 | 中国市政工程西北设计研究院有限公司 | Heterojunction composite material for catalyzing hydrogen evolution and preparation method and application thereof |
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