CN114210353B - Preparation method of bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material - Google Patents
Preparation method of bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 33
- -1 bismuth oxide carbonate-bismuth sulfide Chemical compound 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- GACUIHAEKGVEIC-UHFFFAOYSA-L [Bi+2]=O.C([O-])([O-])=O Chemical compound [Bi+2]=O.C([O-])([O-])=O GACUIHAEKGVEIC-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 6
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 230000004298 light response Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 239000011941 photocatalyst Substances 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 6
- FTEBQCHXMALOGR-UHFFFAOYSA-N [Bi]=S.[Bi]=O Chemical compound [Bi]=S.[Bi]=O FTEBQCHXMALOGR-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
- FWIZHMQARNODNX-UHFFFAOYSA-L dibismuth;oxygen(2-);carbonate Chemical compound [O-2].[O-2].[Bi+3].[Bi+3].[O-]C([O-])=O FWIZHMQARNODNX-UHFFFAOYSA-L 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229940036358 bismuth subcarbonate Drugs 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The application discloses a preparation method of a bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material, which comprises the following steps: (1) Adding urea into deionized water, stirring to dissolve, and adding Bi (NO) 3 ) 3 ·5H 2 Continuously stirring O, and then adding sodium sulfide to obtain a mixed solution; (2) Stirring the mixed solution, then performing airtight reaction, naturally cooling to room temperature after the reaction is completed, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material. The application can effectively solve the problem of insufficient ultraviolet light response of bismuth oxide carbonate serving as a photocatalytic material, and compared with other bismuth oxide carbonate-bismuth sulfide heterojunction, the preparation method is simple, low in cost and easy for mass production.
Description
Technical Field
The application relates to the technical field of photocatalyst synthesis, in particular to a preparation method of a bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
Background
In the research of the photocatalytic technology, a semiconductor photocatalyst has been attracting attention, and degradation of organic matters is effectively performed by using visible light having the largest ratio in the solar spectrum, which is one of the very promising technologies for solving the energy problem.
Nanometer titanium dioxide is always focused on as a typical semiconductor photocatalyst, and has the characteristics of high photocatalytic activity, high stability, low cost, no toxicity and the like, but because the band gap energy of the titanium dioxide is relatively large, the titanium dioxide can only be excited by ultraviolet light with short wavelength, most of visible light cannot be effectively utilized, electrons and holes generated after the photocatalysis of the titanium dioxide are extremely easy to be compounded, so that the efficiency of photon-generated carriers of the titanium dioxide is greatly reduced, and the application value of the titanium dioxide material in actual life is limited to a certain extent. Therefore, it is particularly urgent to find a semiconductor photocatalyst capable of responding to a wide range of solar spectrum and having high stability and high catalytic activity.
Bi-based semiconductor photocatalytic materials have been attracting attention in recent two years, wherein bismuth oxyhalide series catalysts also exhibit good photocatalytic activity, and various attempts have been made to further improve the photocatalytic activity thereof, such as doping, morphology adjustment, and carrier transfer distance shortening. However, bismuth oxide carbonate is used as a photocatalytic material, which causes the problem of insufficient response to ultraviolet light, and Bi is found in the process of trying 2 O 2 CO 3 /Bi 2 S 3 The heterojunction can utilize more visible light and can effectively realize photoinduced electron hole recombination, so that the catalytic effect of the photocatalyst is greatly improved, but Bi in various researches at present 2 O 2 CO 3 /Bi 2 S 3 Almost all the preparation of the catalyst is prepared by taking bismuth oxide carbonate as a precursor in two steps. In order to solve the problem of insufficient response of bismuth oxide carbonate to ultraviolet light, the catalytic effect of the heterojunction containing bismuth oxide carbonate is further improved, and the preparation method of the heterojunction containing bismuth oxide carbonate is simplified, so that the heterojunction containing bismuth oxide carbonate can be widely applied.
Disclosure of Invention
Aiming at the prior art, the application aims to provide a preparation method of a bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material. The application can effectively solve the problem of insufficient ultraviolet light response of bismuth oxide carbonate serving as a photocatalytic material. Compared with other bismuth oxide-bismuth sulfide heterojunction preparation methods, the preparation method provided by the application adopts a one-step synthesis method, and compared with the existing two-step preparation method, the preparation method provided by the application is simpler, low in cost and easy for mass production.
In order to achieve the above purpose, the application adopts the following technical scheme:
in a first aspect of the application, a preparation method of a bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material is provided, comprising the following steps:
(1) Adding urea into deionized water, stirring to dissolve, and adding Bi (NO) 3 ) 3 ·5H 2 Continuously stirring O, and then adding sodium sulfide to obtain a mixed solution;
(2) Stirring the mixed solution, then performing airtight reaction, naturally cooling to room temperature after the reaction is completed, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
Preferably, in step (1), the urea is mixed with Bi (NO 3 ) 3 ·5H 2 The mol ratio of O is (6-10) to (1-3).
Preferably, in step (1), the Bi (NO) 3 ) 3 ·5H 2 O and Na 2 S 3 The molar ratio of (1-3) to (1-4).
Preferably, in the step (2), the stirring is magnetic stirring, and the stirring time is 15-60min.
Preferably, in the step (2), the temperature of the airtight reaction is 150-240 ℃ and the reaction time is 12-48h.
Preferably, in the step (2), the temperature of the centrifugation is 4-25 ℃, the rotational speed of the centrifugation is 4000-12000rpm, and the time of the centrifugation is 5-15min.
In a second aspect of the application, the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material prepared by the preparation method is provided.
Preferably, in the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material, the bismuth oxide carbonate is in a block shape, and the bismuth sulfide is in a rod shape.
In a third aspect, the application provides an application of the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material in photocatalytic degradation of plasticizers.
The application has the beneficial effects that:
(1) The application adopts Bi (NO) 3 ) 3 ·5H 2 O is used as a raw material, water is used as a solvent, and bismuth oxide-bismuth sulfide carbonate (Bi 2 O 2 CO 3 /Bi 2 S 3 ) The heterostructure photocatalytic material is a composite substance of rod-shaped bismuth sulfide and blocky bismuth oxide carbonate. Bi in various researches at present 2 O 2 CO 3 /Bi 2 S 3 The preparation method almost uses bismuth oxide carbonate as a precursor to prepare the binary composite material in two steps, and the binary composite material is synthesized by adopting a one-step method, so that the process flow is simpler, and the preparation method has the characteristics of low cost and easiness in large-scale production.
(2) Bi prepared by the application 2 O 2 CO 3 /Bi 2 S 3 The heterojunction has the following advantages through testing: the optical properties of the prepared sample are verified through UV-Vis diffuse reflection spectrum, the light absorption capacity of bismuth subcarbonate is greatly enhanced after bismuth sulfide is added, the absorption band is widened to the visible light range, and the photocatalytic performance of the product is obviously improved. The bismuth sulfide heterojunction can accelerate the separation of electrons and holes and prolong the service life of photo-generated electrons or holes, so that the photo-catalytic activity of the photocatalyst is effectively improved. Therefore, bismuth oxide carbonate and bismuth sulfide can play a synergistic role, so that the photocatalytic capability of the material is further improved, and pollutants such as plasticizers are effectively degraded.
Drawings
FIG. 1 shows Bi prepared in example 2 2 O 2 CO 3 /Bi 2 S 3 XRD pattern of the heterostructure photocatalytic material.
FIG. 2 shows the preparation of Bi from example 2 2 O 2 CO 3 /Bi 2 S 3 SEM photographs of heterostructure photocatalytic materials.
FIG. 3 is a graph showing the degradation of DBP content versus time of bismuth sulfide alone and bismuth oxycarbonate alone after xenon irradiation of the product prepared in example 2.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The test materials used in the examples of the present application are all conventional in the art and are commercially available.
Example 1:
0.5g of urea was added to deionized water, and after stirring to dissolve, 2.75mmol of Bi (NO) 3 ) 3 ·5H 2 And O, mechanically stirring. After completion of the stirring, 3mmol of sodium sulfide was further added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30min. Transferring the mixed solution into a polytetrafluoroethylene lining, and placing the lining in a reaction kettle for reaction at 200 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
The XRD pattern of the bismuth oxide-bismuth sulfide heterostructure photocatalytic material is shown in fig. 1, and it can be seen from fig. 1 that the bismuth oxide-bismuth sulfide heterojunction is actually prepared in this example. The SEM image of the bismuth oxide-bismuth sulfide heterostructure photocatalytic material is shown in fig. 2, and as can be seen from fig. 2, in the bismuth oxide-bismuth sulfide heterostructure photocatalytic material, bismuth oxide is in a block shape, and bismuth sulfide is in a rod shape. And the particle size of the bismuth oxide carbonate-bismuth sulfide heterojunction is found to be between 200 and 800nm through SEM, TEM and other tests.
Example 2
0.5g of urea was added to deionized water, and after stirring to dissolve, 2.75mmol of Bi (NO) 3 ) 3 ·5H 2 And O, mechanically stirring. After completion of the stirring, 4mmol of sodium sulfide was further added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30min. Transferring the mixed solution into a lining made of polytetrafluoroethylene, and placing the lining in a reaction kettle at 200 DEG CPreserving the temperature for 24 hours under the piece for reaction; and after the reaction is finished, naturally cooling to room temperature, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
Example 3
0.5g of urea was added to deionized water, and after stirring to dissolve, 2.75mmol of Bi (NO) 3 ) 3 ·5H 2 And O, mechanically stirring. After completion of the stirring, 4mmol of sodium sulfide was further added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30min. Transferring the mixed solution into a polytetrafluoroethylene lining, and placing the lining in a reaction kettle for reaction at 180 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
Comparative example 1: preparation of bismuth oxide carbonate photocatalyst
0.5g of urea was added to deionized water, and after stirring to dissolve, 2.75mmol of Bi (NO) 3 ) 3 ·5H 2 And O, mechanically stirring. After completion of the stirring, a mixed solution was obtained. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30min. Transferring the mixed solution into a polytetrafluoroethylene lining, and placing the lining in a reaction kettle for reaction at 200 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate photocatalytic material.
Comparative example 2: preparation of bismuth sulfide photocatalyst
0.73g Bi (NO) 3 ) 3 Adding into 5mL of ethylene glycol, stirring with a stirrer for 5min to obtain clear solution A, and dissolving Na with mass of 1.5g 2 S·9H 2 Dissolving O in 10mL of deionized water to obtain a solution B, slowly and dropwise dripping the solution B into the solution A, and continuously and rapidly stirring to form a black precursor; finally, 0.76g of CO (NH) is added to the precursor 2 ) 2 Preparing 30mL of solution (the volume ratio of deionized water to organic solution is 5:1), pouring into 50mL of polytetrafluoroethylene-containing solutionPlacing the reaction kettle in a stainless steel reaction kettle with lining, heating at constant temperature in an incubator at 120 ℃ for 12 hours, washing the product with deionized water for several times after the reaction is finished, and drying at 80 ℃ for 6 hours (Liu Yun, the name of China is strong, zhu Gangjiang. The ratio of sulfur to bismuth is compared with the hydrothermal synthesis of Bi) 2 S 3 Influence of powder morphology [ J]University of science and technology report of Shaanxi (Nature science edition), 2010,28 (02): 40-44.)
Application example: application of composite photocatalyst in degradation of organic pollutant DBP under visible light
50mg of the catalyst prepared in example 2 and comparative examples 1-2 are respectively placed in a 100mL beaker, 25mL of ultrapure water is added, the catalyst is uniformly dispersed by ultrasonic treatment for 20min, 25mL of 20mg/L of DBP solution is added into the uniform solution after ultrasonic treatment, and the catalyst with a photocatalytic system of 10mg/L of DBP solution and 0.5g/L of catalyst is obtained. Placing on a magnetic stirrer for stirring. The beaker is placed on a magnetic stirrer, and dark reaction is carried out under the stirring condition, so that the catalyst is uniformly dispersed in the system and reaches adsorption equilibrium.
After the dark reaction (sampling 2 mL), the beaker was enclosed by a self-made ice bag, and a xenon lamp light source was turned on to perform a visible light catalytic degradation experiment. In the photocatalytic reaction process, 2mL of the solution is sampled every 20min, and the reaction time is 3h.
Centrifuging the mixture for 5min at 10000 rpm, separating solid from liquid, recovering catalyst, filtering the liquid with 0.45 μm filter head (organic system), and storing in chromatographic bottle at 4deg.C.
And measuring the pollutant concentration of the prepared sample by using high performance liquid chromatography, so as to judge the degradation efficiency of the composite material. As can be seen from fig. 3, the catalyst prepared in example 2 can effectively degrade DBP, and the retention rate of DBP after degradation is only about 30%; the retention rate of DBP is about 80% after the bismuth oxide carbonate in comparative example 1 degrades DBP; after degradation of DBP by bismuth sulfide of comparative example 2, the retention of DBP was about 60%. Therefore, the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material prepared by the application can realize effective degradation of plasticizers such as DBP.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (2)
1. The bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material is characterized in that bismuth oxide carbonate is in a block shape and bismuth sulfide is in a rod shape in the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material;
is prepared by the following method:
adding 0.5. 0.5g urea into deionized water, stirring for dissolving, adding 2.75mmol Bi (NO) 3 ) 3 ·5H 2 O, mechanically stirring; adding 4mmol of sodium sulfide after stirring to obtain a mixed solution;
placing the mixed solution on a magnetic stirrer for mechanical stirring for 30 min; transferring the mixed solution into a polytetrafluoroethylene lining, and placing the lining in a reaction kettle to perform reaction under the condition of 200 ℃ and heat preservation of 24 h; and after the reaction is finished, naturally cooling to room temperature, centrifuging the product, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material.
2. The use of the bismuth subcarbonate-bismuth sulfide heterostructure photocatalytic material of claim 1 in photocatalytic degradation of DBP.
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| CN202210054172.1A CN114210353B (en) | 2022-01-18 | 2022-01-18 | Preparation method of bismuth oxide carbonate-bismuth sulfide heterostructure photocatalytic material |
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| CN102275987A (en) * | 2011-05-25 | 2011-12-14 | 中国地质大学（武汉） | Nano/micro-scale sheet bismuthyl carbonate material and preparation method thereof |
| CN108745393A (en) * | 2018-04-28 | 2018-11-06 | 西安前沿材料研究院有限公司 | A kind of bismuth-bismuthyl carbonate heterojunction structure catalysis material and preparation method thereof |
| CN110575841A (en) * | 2019-09-11 | 2019-12-17 | 哈尔滨理工大学 | Novel photocatalyst material for degrading methylene blue light and preparation method thereof |
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| CN102275987A (en) * | 2011-05-25 | 2011-12-14 | 中国地质大学（武汉） | Nano/micro-scale sheet bismuthyl carbonate material and preparation method thereof |
| CN108745393A (en) * | 2018-04-28 | 2018-11-06 | 西安前沿材料研究院有限公司 | A kind of bismuth-bismuthyl carbonate heterojunction structure catalysis material and preparation method thereof |
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