CN111804318A - Adsorption photocatalyst and preparation method and application thereof - Google Patents
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- molybdenum disulfide
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 claims description 36
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 34
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 33
- 230000001699 photocatalysis Effects 0.000 claims description 16
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 11
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- 235000018660 ammonium molybdate Nutrition 0.000 description 6
- 239000011609 ammonium molybdate Substances 0.000 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 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
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- 238000003756 stirring Methods 0.000 description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
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- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 3
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- 229910016523 CuKa Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
-
- B01J35/39—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention discloses an adsorption photocatalyst and a preparation method and application thereof. The preparation process of the adsorption photocatalyst is simple, large-scale equipment is not needed, and the synthesis condition is simple.
Description
Technical Field
The invention belongs to the technical field of environment function photocatalytic materials, and particularly relates to a MoS2/MoO3/BiPO4An adsorption photocatalyst and a preparation method thereof.
Background
According to the statistical data of the world health organization, at least 500 ten thousand people die each year because of drinking unsafe water and lack of sanitary water; 248 ten thousand people can cause diseases such as apoplexy, cardiovascular diseases, respiratory tract diseases or lung cancer and the like because of inhaling the particle. The problem of environmental pollution treatment has become a difficult problem to be solved urgently. Since Fujishima et al reported that hydrogen is produced by water photolysis for the first time in 1972, the photocatalytic technology provides a new idea for people to treat environmental pollutants by fully utilizing the advantages of solar energy, capability of mineralizing most organic pollutants in sewage and the like, and the photocatalytic material which is high in degradation efficiency, good in stability, low in cost and non-toxic becomes a research hotspot of people.
In 2010, Pangolin first reported bismuth phosphate (BiPO)4) Used for photocatalytic degradation of organic matters and is found to have excellent ultraviolet photocatalytic activity and bismuth phosphate (BiPO)4) The photocatalyst has the advantages of low price, no toxicity, easy preparation, easy separation and the like, has potential application value in the field of photocatalysis, but has limited further development and application due to the defects of low utilization rate of visible light, low quantum efficiency, photo-generated carrier recombination and the like. Practically speaking, bismuth phosphate (BiPO)4) The modification is carried out to improve the efficiency, and has important significance for industrial application.
In order to solve the problems, on one hand, the photocatalytic activity can be improved by regulating and controlling the micro-morphology and the structure of the photocatalyst; on the other hand, the photoresponse range of the photocatalyst can be expanded through doping or compounding, and the quantum efficiency is improved. Wherein between different semiconductorsIn addition, the light absorption range can be expanded, and the separation and migration efficiency of photoproduction holes and electrons can be improved by forming a heterojunction, so that the photocatalytic activity is improved. However, molybdenum disulfide has a certain specific surface area as a semiconductor promoter, and no document exists at present about MoS2/MoO3/BiPO4Reports of adsorbed photocatalysts.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the MoS with dual functions of adsorption and photocatalysis2/MoO3/BiPO4The composite catalyst and the preparation method and application thereof have the advantages of simple and easy preparation process, no need of large-scale equipment and simple and easy synthesis conditions.
The technical purpose of the invention is realized by the following technical scheme:
an adsorption photocatalyst and a preparation method thereof are prepared according to the following steps: grinding and uniformly mixing bismuth phosphate and molybdenum disulfide, heating to 280-300 ℃ from room temperature at the speed of 5-10 ℃ per minute in an air atmosphere, preserving heat for 1-5 hours, naturally cooling to room temperature, and grinding to obtain an adsorption photocatalyst; the mass ratio of the molybdenum disulfide to the bismuth phosphate is (0.05-0.3): 1.
and the mass ratio of the molybdenum disulfide to the bismuth phosphate is (0.1-0.2): 1.
and after the bismuth phosphate and the molybdenum disulfide are uniformly mixed, the temperature is raised to 290-300 ℃ from room temperature at the speed of 8-10 ℃ per minute, and the temperature is kept for 1-2 hours.
The adsorption photocatalyst prepared by the invention is characterized, and the crystal form of the sample is tested by adopting a German Bruker D8 advanced X-ray diffractometer. The analysis was carried out using CuKa rays (. lamda. times.0.154 nm), and the voltage was 40kv and the current was 40 mA. The scanning step is 0.01 °. BiPO prepared by XRD (X-ray diffraction) for detection4/MoO3/MoS2Crystal structure and phase information of the heterojunction photocatalyst. In FIG. 1, MoO is shown from bottom to top3(JCPDS 05-0508) and BiPO4(JCPDS No.15-0767) XRD Standard Pattern. Due to MoO3Shows a weak crystallinityPeak intensity, however, MoO3The XRD patterns of (A) are still attributable to MoO3Characteristic peaks of (110), (040) and (021) crystal planes of (1). BiPO4The three strong peaks, pointing to the (200), (120), (012) crystal planes, appeared at 2 θ values of 27.07 °, 29.02 °, 31.15 °, indicating efficient synthesis of BiPO4 and high crystallinity. Due to MoS2The doping amount is low, and MoO3 is produced by oxidation in the calcining process, so that MoS is obviously found in an XRD diffraction pattern2Diffraction peaks, but a small amount of MoS was present in view of the dark grey colour of the catalyst2And (4) doping. XRD patterns showed mixed phases (bismuth phosphate, molybdenum disulfide and MoO)3) Successful preparation of heterojunctions is demonstrated; from SEM, the catalyst prepared by using bismuth phosphate and molybdenum disulfide as raw materials has a uniform overall appearance although a little agglomeration phenomenon occurs.
In the invention, bismuth phosphate is a bismuth phosphate nanorod, and the bismuth phosphate nanorod is prepared by a hydrothermal method, and specifically, the bismuth phosphate nanorod can be obtained by reference documents (controllable synthesis and photocatalytic performance of the bismuth phosphate nanorod, Liu Yan Fang, Ma Xin, Yixin, Zhu Yong method, Physics and chemistry report (Wuli Huaxue Xuebao) Acta Phys. -Chim.sin.2012, 28(3), 654-: adding 2-4mmol/L bismuth nitrate pentahydrate into 120mL deionized water to prepare a bismuth nitrate pentahydrate aqueous solution, adding 10-12mmol sodium dihydrogen phosphate, stirring for 1h, transferring into a high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal treatment at 160 ℃ for 18-24 h, cooling the reaction kettle to room temperature, centrifuging at the rotation speed of 8000-.
In the invention, the molybdenum disulfide is molybdenum disulfide nano-microspheres, and the molybdenum disulfide is prepared by a hydrothermal method, and the specific references (synthesis of the spheroidal molybdenum disulfide and the electrochemical properties thereof by the hydrothermal method, Li Meijuan, Shenshu Yi, Luo Guo Qiang, Zhang alliance, inorganic chemistry bulletin, 9 months in 2017, 9 th vol 33, 1521 and 1526): adding 0.4-0.5g of ammonium molybdate into 40ml of deionized water to prepare an ammonium molybdate solution, adding 0.5-0.6g of thiourea, stirring for dissolving, performing ultrasonic treatment for 30min, transferring into 50ml of a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 200 ℃ for 18-24 h, cooling the reaction kettle to room temperature, centrifuging at the rotating speed of 8500 and 9500r/min, alternately washing the product with deionized water and absolute ethyl alcohol for 3-4 times, and drying at 45 ℃ for 10-13 h.
Compared with the prior art, the invention has the following beneficial effects: (1) MoS in the invention2/MoO3/BiPO4The preparation process of the adsorption photocatalyst is simple, large-scale equipment is not needed, and the synthesis condition is simple; (2) the photocatalytic material is used for degrading methylene blue simulated dye wastewater, and shows certain adsorption capacity and photocatalytic degradation effect; (3) the invention obtains the best adsorption and photocatalysis effects by adjusting the proportion of the bismuth phosphate and the molybdenum disulfide.
Drawings
FIG. 1 is an XRD spectrum of an adsorbed photocatalyst of the present invention.
FIG. 2 is an SEM photograph of an adsorbed photocatalyst of the present invention.
FIG. 3 is a graph comparing the degradation of methylene blue by adsorption using the adsorption photocatalyst of the present invention and bismuth phosphate alone.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Example 1
And 3, weighing 0.5g and 0.05g of the bismuth phosphate in the step 1 and the molybdenum disulfide in the step 2 respectively, fully grinding the mixture for 20 minutes by using an agate mortar, and then putting the mixture into a muffle furnace to set the temperature of 300 ℃ for calcining for 1 hour to obtain MoS2/MoO3/BiPO4Adsorbing the photocatalyst, naturally cooling the product to room temperature, and fully grinding the product for 20 minutes again by using an agate mortar to obtain the final product.
Example 2
And 3, weighing 0.5g and 0.1g of the bismuth phosphate in the step 1 and the molybdenum disulfide in the step 2 respectively, fully grinding the mixture for 20 minutes by using an agate mortar, and then putting the mixture into a muffle furnace to set the temperature of 300 ℃ for calcining for 1 hour to obtain MoS2/MoO3/BiPO4Adsorbing the photocatalyst, naturally cooling the product to room temperature, and fully grinding the product for 20 minutes again by using an agate mortar to obtain the final product.
MoS prepared as in examples 1 and 22/MoO3/BiPO4And (3) carrying out an adsorption photocatalysis experiment test on the methylene blue adsorption degradation condition by using the adsorption photocatalyst according to the bismuth phosphate prepared by the reference.
Preparing a methylene blue solution, and measuring a standard curve; a lamp source: ultraviolet mercury with power of 25W and wavelength of 254nmA lamp; 50mg of catalyst and 150mL of methylene blue solution with the concentration of 10PPM are weighed in beakers, ultrasonic treatment is carried out for 20 minutes under the Dark condition, and because the material has better adsorption effect, independent photocatalysis experiments are not significant, so that one beaker is wrapped by tinfoil to be protected from Light for comparison (marked as Dark), and the other beaker is used for continuing the photocatalysis experiments under an ultraviolet lamp (marked as Light). Sampling 5ml at regular intervals, centrifuging (6000rpm, 4min), collecting supernatant, measuring absorbance at 654nm, converting into concentration according to standard curve, and concentrating with C/C0To evaluate, C and C0The concentration of methylene blue at the time of reaction t and before the reaction, respectively.
As can be seen from the curve 1 in FIG. 3, the single bismuth phosphate does not show obvious adsorption performance when undergoing photocatalytic degradation, but can degrade the methylene blue dye wastewater by 75% within 30 min;
it can be known from curves 2 and 3 in fig. 3 that when the bismuth phosphate-based catalyst is subjected to photocatalytic degradation, it can be found that the absorbance of the methylene blue dye wastewater is respectively reduced by 50% and 80% after dark treatment for 20min, which indicates that the composite material has a certain adsorption capacity and the degradation concentration continues to be reduced;
compared with the curves 2, 4, 3 and 5, the concentration of the methylene blue solution is reduced under the dark treatment condition, which further indicates that the material has the adsorption property, and the concentration of the solution is reduced more after the ultraviolet lamp is added for irradiation, thereby indicating that the catalyst has certain photocatalytic performance, namely the application of the catalyst in adsorbing photocatalytic methylene blue.
The preparation of the adsorption photocatalyst can be realized by adjusting the process parameters according to the content of the invention, and the adsorption photocatalyst shows the performance basically consistent with the invention. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. An adsorption photocatalyst is characterized in thatThe preparation method comprises the following steps: grinding and uniformly mixing bismuth phosphate and molybdenum disulfide, heating to 280-300 ℃ from room temperature at the speed of 5-10 ℃ per minute in an air atmosphere, preserving heat for 1-5 hours, naturally cooling to room temperature, and grinding to obtain an adsorption photocatalyst; the mass ratio of the molybdenum disulfide to the bismuth phosphate is (0.05-0.3): 1, bismuth phosphate, molybdenum disulfide and MoO are present in the catalyst3Mixing the phases.
2. An adsorbing photocatalyst as claimed in claim 1, wherein the mass ratio of molybdenum disulfide to bismuth phosphate is (0.1-0.2): 1.
3. an adsorbing photocatalyst as claimed in claim 1 or 2, wherein the bismuth phosphate and molybdenum disulfide are mixed uniformly, and then heated from room temperature to 290-300 ℃ at a rate of 8-10 ℃ per minute and held for 1-2 hours.
4. The adsorptive photocatalyst as claimed in claim 1 or 2, wherein the bismuth phosphate is bismuth phosphate nanorods and is prepared by hydrothermal method.
5. An adsorbing photocatalyst as claimed in claim 1 or 2, wherein the molybdenum disulfide is a molybdenum disulfide nanoparticle prepared by a hydrothermal method.
6. The preparation method of the adsorption photocatalyst is characterized by comprising the following steps of: grinding and uniformly mixing bismuth phosphate and molybdenum disulfide, heating to 280-300 ℃ from room temperature at the speed of 5-10 ℃ per minute in an air atmosphere, preserving heat for 1-5 hours, naturally cooling to room temperature, and grinding to obtain an adsorption photocatalyst; the mass ratio of the molybdenum disulfide to the bismuth phosphate is (0.05-0.3): 1.
7. the method of claim 6, wherein the mass ratio of the molybdenum disulfide to the bismuth phosphate is (0.1-0.2): 1.
8. the method of claim 6 or 7, wherein the temperature of the mixture is increased from room temperature to 290-300 ℃ at a rate of 8-10 ℃ per minute and maintained for 1-2 hours after the bismuth phosphate and the molybdenum disulfide are mixed uniformly.
9. The method of claim 6, wherein the bismuth phosphate is a bismuth phosphate nanorod, and the molybdenum disulfide is a molybdenum disulfide nanosphere, both prepared by hydrothermal method.
10. Use of an adsorbing photocatalyst according to any one of claims 1 to 5 for adsorbing photocatalytic methylene blue.
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| CN113501504A (en) * | 2021-07-21 | 2021-10-15 | 苏州普轮电子科技有限公司 | Novel semiconductor material with micro-nano structure and preparation method thereof |
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Application publication date: 20201023 |