CN111632611A - Preparation method of bismuth oxyiodide heterojunction photocatalytic material for degrading perfluorinated compounds - Google Patents
Preparation method of bismuth oxyiodide heterojunction photocatalytic material for degrading perfluorinated compounds Download PDFInfo
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- CN111632611A CN111632611A CN201910153880.9A CN201910153880A CN111632611A CN 111632611 A CN111632611 A CN 111632611A CN 201910153880 A CN201910153880 A CN 201910153880A CN 111632611 A CN111632611 A CN 111632611A
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000000593 degrading effect Effects 0.000 title claims abstract description 12
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 150000001875 compounds Chemical class 0.000 title abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 239000011941 photocatalyst Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract 3
- 239000000843 powder Substances 0.000 claims description 11
- 239000011449 brick Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 abstract 3
- 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 abstract 1
- 238000013032 photocatalytic reaction Methods 0.000 abstract 1
- 239000011343 solid material Substances 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 5
- 229910052797 bismuth Inorganic materials 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
Abstract
The invention relates to a preparation method of a bismuth oxyiodide heterojunction photocatalytic material for efficiently catalyzing and degrading perfluorinated compounds. The invention belongs to the technical field of photocatalysis. The method comprises the following specific steps: preparing ethylene glycol precursor solution of bismuth nitrate pentahydrate and potassium iodide, placing the ethylene glycol precursor solution in a reaction kettle for solvothermal reaction, and calcining the obtained solid material at high temperature to obtain BiOI @ Bi5O7I heterojunction photocatalytic material. The photocatalytic material prepared by the preparation method provided by the invention has excellent catalytic performance, can efficiently remove perfluorinated compound PFOA (perfluorooctanoic acid) in water under visible light, and is BiOI @ Bi prepared when the calcination temperature is 390 DEG C5O7The I heterojunction photocatalyst has the best catalytic performance, the degradation rate of 6h is 81.3%, and good material basis and technical support are provided for the application of the photocatalytic reaction in the aspect of wastewater treatment.
Description
The technical field is as follows:
the invention belongs to the technical field of photocatalysis, and particularly relates to BiOI @ Bi capable of catalytically degrading perfluorinated compounds5O7I, a preparation method of the heterojunction photocatalytic material and application research of efficiently degrading perfluorinated compounds.
Background art:
perfluoroalkanoic acids (PFAAs) are synthetic fluorinated products and are widely used in industry, consumer products (e.g. non-stick pan), etc. They are released into the environment, persist, and can accumulate through the biochain, posing a health hazard to humans. Among the PFAAs, the ecotoxicity and health studies of perfluorooctanoic acid (PFOA) and perfluorooctylsulfonic acid (PFOS) are of great interest, and reports have shown that their presence is detected in human blood samples from different continents. Therefore, how to effectively remove PFAAs from environmental media has attracted global attention. In addition, since the PFAAs has a C — F bond with high bond energy, it has excellent thermal and chemical stability, and cannot be effectively removed by the conventional water treatment process. Therefore, finding a technology for efficient and economical environmental elimination of PFAAs is one of the hot spots of current environmental field research. In recent years, a photocatalytic technique has been attracting attention among various water treatment techniques because of its energy saving and low power consumption. The patent tries to prepare a photocatalytic material capable of effectively degrading PFAAs and a matched technology, and provides material and technical support for effectively removing PFAAs in wastewater.
The bismuth-based photocatalyst has the advantages of excellent visible light catalytic performance, matched energy band structure and the like, but the general bismuth oxyiodide has the defect that photoproduction electrons and holes are easy to recombine, so that the utilization rate of electron hole pairs is greatly reduced, and pollutants such as PFOA (Perfluorooctane-fluorooctane-acetic acid) in wastewater cannot be effectively degraded, so that more novel bismuth-based catalysts must be designed, the bismuth-based photocatalyst has a more matched band gap structure, the electron hole pairs are effectively separated, and the catalytic activity of the bismuth-based photocatalyst is improved. In addition, through the reasonable design of the energy band structure, the material can be compounded with the BiOI to form a heterojunction photocatalytic material, so that the photocatalytic activity of the catalyst can be greatly improved. In the scheme, BiOI @ Bi is prepared5O7The I heterojunction is also connected with Bi while making full use of the strong visible light absorption capability of the BiOI5O7I generates a more matched band gap structure, and effectively inhibits the recombination of electron-hole pairs. And, Bi is relative to BiOI5O7I has higher conduction band edge, the generated electrons have stronger reducibility, and O can be effectively generated2 -Thereby directly adding the pollutantsAnd the removal enables the heterojunction catalyst to have more excellent catalytic performance. In the research, the BiOI @ Bi generated by different processes (including calcination temperature) is intensively researched5O7l heterojunction, the difference in the aspects of performance, morphology and the like, and provides a simple and effective synthesis BiOI @ Bi5O7I method of heterojunction composite photocatalyst, and it can effectively degrade typical perfluor compound PFOA, provides a new method for treating waste water and protecting environment
The invention content is as follows:
the invention solves the technical problem of providing the BiOI @ Bi for degrading the perfluorinated compound PFOA which is simple to operate and environment-friendly5O7I, a preparation method of the heterojunction photocatalytic material and application research of efficiently degrading perfluorinated compounds.
The invention adopts the following technical scheme for solving the technical problems, namely the BiOI @ Bi for degrading the perfluorinated compound PFOA5O7The preparation method of the I heterojunction photocatalytic material is characterized by comprising the following specific steps:
preparation of BiOI photocatalyst
1) 0.97g of Bi (NO)3)3·5H2O is dispersed in 30ml of ethylene glycol and is subjected to ultrasonic treatment for 30min to form a colorless solution A.
2) 0.40gKI was dispersed in 30ml of ethylene glycol and sonicated for 30min to form a pale yellow solution B.
3) And dropwise adding the solution B into the solution A, and continuously stirring for 30min to obtain an orange solution C.
4) Then transferring the solution C into a 100mL polytetrafluoroethylene stainless steel high-pressure reaction kettle, carrying out hydrothermal treatment at 120 ℃ for 12h, then carrying out centrifugation to obtain brick red powder solid, washing with deionized water and ethanol twice respectively, and finally drying in an oven at 80 ℃ overnight.
2BiOI@Bi5O7Preparation of the photocatalyst
Calcining the brick red powder obtained in the step 4) in a muffle furnace at 350 ℃, 370 ℃, 390 ℃ and 410 ℃. It is noted that the powder solid must be put in after the temperature of the muffle furnace is raised to the design temperature, and then taken out after being calcined for 2h, and then cooled at room temperature, otherwise the material cannot be obtained.
More preferably, the BiOI @ Bi obtained in the step 2 when the calcination temperature is 390 DEG C5O7The performance of the composite photocatalyst is optimal.
The invention has the beneficial effects that the simple and feasible preparation method is adopted to prepare the BiOI @ Bi capable of effectively degrading the perfluorinated compound PFOA5O7The I heterojunction photocatalyst has the characteristic of effectively degrading a perfluorinated compound PFOA at normal temperature; a method is provided for obtaining a heterojunction photocatalyst material by a simple green preparation process.
Description of the drawings:
FIG. 1 is an SEM (a.control; b.390 ℃; c.410 ℃) chart of the photocatalyst prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of the photocatalyst prepared in example 1 of the present invention;
FIG. 3 is a graph showing the effect of a series of catalysts prepared in example 1 on the degradation of a perfluorocompound PFOA in simulated sunlight.
The specific implementation mode is as follows:
the present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1:
1) 0.97g of Bi (NO)3)3·5H2Dispersing O in 30ml of ethylene glycol, and carrying out ultrasonic treatment for 30min to form a colorless solution A.
2) 0.40g KI was dispersed in 30ml ethylene glycol and sonicated for 30min to form a pale yellow solution B.
3) And dropwise adding the solution B into the solution A, and continuously stirring for 30min to obtain an orange solution C.
4) Then transferring the solution C into a 100mL stainless steel high-pressure reaction kettle made of polytetrafluoroethylene, carrying out hydrothermal treatment at 120 ℃ for 12h, then carrying out centrifugation to obtain brick red powder solid, washing the brick red powder solid with deionized water and ethanol twice respectively, and finally drying the brick red powder solid in an oven at 80 ℃ overnight.
5) Calcining the brick red powder obtained in the step 4) in a muffle furnace at 350 ℃, 370 ℃, 390 ℃ and 410 ℃. It is worth noting that the powder solid must be put in after the temperature of the muffle furnace is raised to the design temperature, and after 2h of calcination, the powder solid is taken out and put at room temperature for cooling.
The heterojunction catalyst prepared in example 1 was morphologically characterized by SEM and phase analyzed by XRD. As shown in fig. 1, the initially prepared material has a complete spherical structure, and as the calcination temperature is increased, the surface of the spherical structure is gradually crushed, even a crack structure is formed, the structure is loosened, and when the temperature reaches 410 ℃, relatively uniform pellets gradually become different in size, and a fused hole structure is formed, and the complete spherical structure is broken. As shown in FIG. 2, when the material was not calcined, the material was also BiOI, corresponding to card No.10-0445, and as the temperature increased, the XRD peak appeared to be shifted to the left, while when the temperature was 410 deg.C, the material was corresponding to Bi5O7I, the card is No.40-0548, no other crystal phase structure material appears between 350-410 ℃, and the existence of characteristic crystal faces of the two materials can be found in the crystal structure of the obtained material when the calcination temperature is 390 ℃, thereby also proving that the Bi @ OI Bi is5O7And I, generating a heterojunction photocatalyst.
Example 2:
preparing perfluorooctanoic acid (PFOA) aqueous solution with the concentration of 15mg/L by deionized water, adding 40ml into a quartz tube for light reaction, then adding 20mg of prepared photocatalyst, adding a magnetic stirrer, putting the mixture into a light reaction device, opening condensed water to control the reaction temperature to be 25 ℃, then turning on a power supply, turning on a stirring button, firstly carrying out dark reaction to achieve adsorption and desorption balance, then turning on a lamp with the power of 800W xenon, measuring the concentration of PFOA before and after the reaction by liquid chromatography, and obtaining the result shown in figure 3, wherein when the calcination temperature is 390 ℃, the prepared BiOI @ Bi is5O7The catalytic performance of the heterojunction photocatalyst is optimal, the degradation rate of 6h is 81.3%, compared with the degradation rate prepared at other temperatures34% (uncalcined, labeled control), 65.8% (calcining temperature 350 ℃, labeled 350 ℃), 68.4% (calcining temperature 370 ℃, labeled 370 ℃), 81.3% (calcining temperature 390 ℃, labeled 390 ℃), 74.6% (calcining temperature 410 ℃, labeled 410 ℃), respectively, reported TiO2When PFOA is degraded by ultraviolet light irradiation, the degradation rate is only 35% in 8h, and when PFOA is degraded by a Pb-BFO/rGO photocatalyst, the degradation rate is only 48% in 8 h. Description of BiOI @ Bi5O7The I heterojunction photocatalyst has very good catalytic degradation performance for PFOA.
Claims (4)
1. A preparation method of bismuth oxyiodide heterojunction photocatalytic material for degrading perfluorocompounds PFOA comprises the following specific steps:
1) 0.97g of Bi (NO)3)3·5H2Dispersing O in 30ml of ethylene glycol, and carrying out ultrasonic treatment for 30min to form a colorless solution A.
2) 0.40g KI was dispersed in 30ml ethylene glycol and sonicated for 30min to form a pale yellow solution B.
3) And dropwise adding the solution B into the solution A, and continuously stirring for 30min to obtain an orange solution C.
4) Transferring the solution C into a 100mL polytetrafluoroethylene stainless steel high-pressure reaction kettle, carrying out hydrothermal treatment at 120 ℃ for 12h, then centrifuging to obtain brick red powder solid, washing with deionized water and ethanol twice respectively, and drying in an oven at 80 ℃ overnight.
5) And (3) respectively placing the brick red powder obtained in the step (4) into a muffle furnace at 390 ℃ for calcination, and immediately taking out the crucible and cooling at room temperature after 2 hours of calcination.
2. The BiOI @ Bi of claim 15O7The preparation method of the I heterojunction photocatalytic material is characterized by comprising the following steps: the generated BiOI @ Bi at the calcination temperature of 390 ℃ in the step 5)5O7The catalytic performance of the heterojunction photocatalyst is optimal.
3. The BiOI @ Bi of claim 15O7I heterojunction photocatalystThe preparation method of the chemical material is characterized by comprising the following steps: and 5) the prepared precursor can be put in after the temperature in the muffle furnace rises to the set temperature.
4. The BiOI @ Bi of claim 15O7The preparation method of the I heterojunction photocatalytic material is characterized by comprising the following steps: and 5) calcining for 2h, taking out immediately after timing is finished, and cooling at room temperature.
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Cited By (2)
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| CN112371143A (en) * | 2020-12-02 | 2021-02-19 | 南开大学 | Preparation method of bismuth oxyfluoride photocatalytic material with controllable shape and defects for degrading perfluorinated compounds |
| CN115999587A (en) * | 2023-02-20 | 2023-04-25 | 河南农业大学 | Photocatalytic material and preparation method and application thereof |
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| CN115999587A (en) * | 2023-02-20 | 2023-04-25 | 河南农业大学 | Photocatalytic material and preparation method and application thereof |
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