CN111495392A - Preparation method of iron-based piezoelectric catalytic material and application of iron-based piezoelectric catalytic material in water treatment - Google Patents
Preparation method of iron-based piezoelectric catalytic material and application of iron-based piezoelectric catalytic material in water treatment Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 57
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 45
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 34
- 239000003054 catalyst Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000006555 catalytic reaction Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003344 environmental pollutant Substances 0.000 claims description 8
- 231100000719 pollutant Toxicity 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 229910052961 molybdenite Inorganic materials 0.000 claims description 7
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910002113 barium titanate Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910003090 WSe2 Inorganic materials 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims 1
- KAEAMHPPLLJBKF-UHFFFAOYSA-N iron(3+) sulfide Chemical compound [S-2].[S-2].[S-2].[Fe+3].[Fe+3] KAEAMHPPLLJBKF-UHFFFAOYSA-N 0.000 claims 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- GSDSWSVVBLHKDQ-JTQLQIEISA-N Levofloxacin Chemical compound C([C@@H](N1C2=C(C(C(C(O)=O)=C1)=O)C=C1F)C)OC2=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-JTQLQIEISA-N 0.000 description 4
- 229960003376 levofloxacin Drugs 0.000 description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 2
- 238000002306 biochemical method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
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- B01J35/33—
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/049—Sulfides with chromium, molybdenum, tungsten or polonium with iron group metals or platinum group metals
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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 relates to a preparation method of an iron-based piezoelectric catalytic material and application of the iron-based piezoelectric catalytic material in water treatment, belonging to the technical field of preparation and application of novel functional materials. The invention mainly strengthens the environmental application of the composite piezoelectric catalytic material from three aspects. Firstly, promoting the formation of active vacancies by introducing the original taste of a valence-variable element, and preliminarily strengthening the piezoelectric property; secondly, the band gap width of the piezoelectric material is regulated and controlled through element doping, the conductivity of the composite material is increased, the electron migration is accelerated, and the piezoelectric catalytic activity is further improved; and finally, through magnetic construction, the magnetic recovery of the piezoelectric catalytic material in water is realized, the generation of nano pollution is prevented and the environmental engineering application of the piezoelectric material is promoted.
Description
Technical Field
The invention provides a preparation method of an iron-based piezoelectric catalytic material and application thereof in water treatment, relates to a preparation method of an iron-based piezoelectric catalytic material, particularly relates to application thereof in the fields of interface catalytic reaction and water purification, and belongs to the technical field of preparation and application of novel functional materials.
Background
Along with the rapid development of economy and the improvement of living standard of people, the water quality problem faced by China is more and more severe. A range of emerging contaminants occur in aqueous environments such as antibiotics, micro-plastics, personal care products and pharmaceuticals. How to realize the high-efficient purification of pollutants in water is the hot spot of current research. In recent years, various physical, chemical and biochemical methods have been applied to the field of purification of pollutants in water. The physical method mainly comprises an extraction method, an adsorption method, a filtration method and the like, wherein the adsorption method is most widely applied in the field of micro-polluted water purification, but has the problems of solid waste and secondary pollution. The biochemical method can thoroughly degrade organic pollutants into small molecular products without biotoxicity, but has poor applicability to high-concentration organic sewage, and the domestication period of biochemical strains is longer and the process is longer. Compared with the chemical method, the chemical method has wider application in the field of purifying organic matters in water, and particularly advanced oxidation is considered to be one of the most effective methods for treating organic sewage at present. The photocatalysis method is favored by researchers due to the advantages of no chemical addition, complete degradation and the like, and a series of photocatalysis materials are designed to achieve good effects. But limited applicability to water samples with turbidity and high color. In addition, the water treatment plant in China has simple process and is mostly carried out in a dark environment, so that a new purifying material and a purifying method are required to be searched as a support.
The piezoelectric catalysis method is a research field emerging in recent years, and is to utilize a piezoelectric material to generate surface potential under the action of mechanical force and promote the formation of active free radicals through internal potential difference so as to realize the efficient degradation of pollutants in water. At present, many materials such as MoS2、WS2、MoSe2、WSe2、ZnO、BiTiO3、CdS、BaTiO3、Pb(Zr0.52Ti0.48)O3And the like are proved to have piezoelectric activity and can be used as piezoelectric catalytic materials for degrading pollutants in water. However, the degradation efficiency of the method still needs to be improved, so most researches are to realize the high-efficiency degradation of pollutants in water by strengthening photocatalysis through piezoelectric catalysis. Recently, CN109331882A discloses an organic piezoelectric-photocatalytic composite spiral fiber, which realizes continuous generation of piezoelectric potential under the action of water flow, effectively promotes separation of photo-generated electron-hole pairs of a photocatalyst, and significantly improves efficiency of photocatalytic degradation of pollutants. CN108772063A discloses an Ag2O/Bi4Ti3O12The piezoelectric photocatalyst and the synthesis method thereof greatly improve the capability of the catalytic material to degrade organic matters under the condition of ultrasonic-assisted illumination catalysis. CN109529807A is through normal position photogeneration titanium oxide nanoparticle parcel lead zirconate titanate piezoelectric powder obtains composite catalyst material, when through the induction of fluid mechanical energy, can produce the piezoelectric field, and it is obvious to show promotion photocatalytic reaction effect.
Recently, Liu Zhi Yong of Nanchang aviation university and the like enhance the piezoelectric activity of KN L N ceramic through the load of Ag elementary substance, realize high-efficiency piezoelectric catalytic degradation of dye wastewater (CN 110092440A). The piezoelectric catalytic activity of the material can be obviously enhanced through proper crystal form regulation, whether the band gap regulation of a semiconductor can be realized through introducing element doping, and the separation of electrons and holes is accelerated, so that the piezoelectric catalytic activity of the semiconductor is improved?
In view of the defects of the prior art, the invention aims to provide a preparation method of an iron-based piezoelectric catalytic material and application of the iron-based piezoelectric catalytic material in water treatment. On one hand, the central asymmetry of the piezoelectric catalytic material is increased by element doping, and the generation of irregular distortion under the action of mechanical force is promoted; on the other hand, the forbidden bandwidth of the piezoelectric material is regulated and controlled through the introduction of the valence-variable metal element, the conductivity of the piezoelectric material is regulated and controlled, and the electron migration is accelerated. Thereby obviously enhancing the piezoelectric catalytic activity of the material and realizing the efficient piezoelectric catalytic degradation of organic pollutants. And finally, regulating and controlling the magnetism of the composite material by regulating and controlling the amount of the introduced iron salt, thereby realizing the magnetic recovery of the catalyst sample.
Disclosure of Invention
The invention aims to provide a preparation method of an iron-based piezoelectric catalytic material and application thereof in water treatment, aiming at overcoming the defects of the existing piezoelectric catalytic material and application thereof, wherein element doping is used for adjusting the band gap distribution of the material, meanwhile, in-situ doping is used for forming active vacancies, the non-central symmetry is increased, the piezoelectric catalytic activity of the material is obviously enhanced, the magnetic recovery of a piezoelectric catalyst is realized through magnetic regulation, and the environmental applicability of the piezoelectric material is promoted.
In order to achieve the purpose, the preparation method of the iron-based piezoelectric catalytic material and the application of the iron-based piezoelectric catalytic material in water treatment have the following technical scheme and steps:
1) according to the mole ratio of ferric salt to reactants needed for synthesizing the piezoelectric catalytic material, 1: (50-1000) respectively weighing ferric salt and reactants needed by synthesizing the piezoelectric catalytic material, and uniformly mixing.
2) Adding the mixed powder obtained in the previous step into a polytetrafluoroethylene reaction kettle, and mixing the materials: adding zirconia balls according to the mass ratio of 1:100-500, and ball-milling for 3-5h under the condition of the rotating speed of 500-1500 rpm to obtain the precursor powder of the iron-based composite piezoelectric catalytic material.
3) The precursor powder was placed in a tube furnace at N2Activating at 500 deg.C for 2-5h under atmosphere, and naturally cooling to room temperature.
4) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at 120 ℃ for 5 to 24 hours to obtain the iron-based composite piezoelectric catalyst product.
5) Weighing 0.01-0.5g of iron-based composite piezoelectric catalyst powder, placing the powder in a piezoelectric catalytic system, and testing the performance of the piezoelectric catalytic system, wherein the specific operation is that the iron-based composite piezoelectric catalyst powder with the mass of 0.01-0.5g is weighed, added into a pollutant water sample with the volume of 20-80m L, and mechanical force is introduced to excite the piezoelectric catalytic reaction for 0.01-2 h.
6) The piezoelectric catalyst powder was recovered with a magnet, and the supernatant was taken to measure the concentration of the target contaminant.
The synthetic piezoelectric material reactant can be used for preparing MoS2、WS2、MoSe2、WSe2、ZnO、BiTiO3、CdS、BaTiO3、Pb(Zr0.52Ti0.48)O3And reactants corresponding to the piezoelectric fibers and the piezoelectric ceramics.
The mechanical force initiation method applied to the piezoelectric catalytic reaction system can be a method for providing mechanical force to initiate piezoelectric catalytic reaction for one or more of a ball milling method, an ultrasonic method, a stirring method, an air flow method, a water flow method and the like.
Compared with other technologies, the invention has the advantages that: (1) the iron-based composite piezoelectric catalyst provided by the invention is simple in operation process, low in cost and easy for batch production. (2) The synthesized iron-based composite piezoelectric catalyst has high piezoelectric catalytic activity and can quickly degrade organic pollutants in water. (3) The iron-based composite piezoelectric catalyst prepared by the invention has magnetism, can be quickly separated through magnetism, promotes the catalyst to be recycled, prevents pollution, and can meet the requirements of environmental engineering application.
Drawings
FIG. 1 shows an iron-based WS prepared by the present invention2Transmission electron microscope photograph and element distribution diagram of the composite material.
FIG. 2 shows an iron-based WS prepared by the present invention2The effect curve of the composite material piezoelectric catalytic degradation levofloxacin.
FIG. 3 is an iron-based MoS prepared according to the present invention2Material piezoelectric force microscopy images.
FIG. 4 is an iron-based MoS prepared according to the present invention2The material is used for carrying out piezoelectric catalysis to rapidly degrade rhodamine.
FIG. 5 shows Fe @ BaTiO iron base prepared according to the present invention3The effect diagram of the material piezoelectric catalytic degradation of methyl orange.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
1) Weighing tungsten dioxide, thiourea and ferric trichloride according to the mass ratio of 1: 10: 0.1, and placing the tungsten dioxide, thiourea and ferric trichloride in a polytetrafluoroethylene ball-milling reaction kettle with the thickness of 100m L.
2) Adding 100g of zirconia balls into the system in the step 1), and ball-milling for 3 hours under the condition of 800 r/min to obtain the iron-based WS2And compounding the piezoelectric catalytic material precursor powder.
3) Putting the precursor powder obtained in the step 4) into a tube furnace, and performing reaction in a reactor under N2Activating at 450 deg.C for 2h under atmosphere, and naturally cooling to room temperature.
4) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder for 10 hours at 120 ℃ to obtain the iron-based composite piezoelectric catalyst product, wherein the transmission electron microscope characterization result of the iron-based composite piezoelectric catalyst product is shown in the attached figure 1.
5) Weighing 50m L water sample containing 100 mg/L levofloxacin, adding 0.05g of iron-based composite piezoelectric catalyst powder, placing in a polytetrafluoroethylene ball-milling reaction kettle, and ball-milling for 60min at the rotating speed of 1000 r/min.
6) Separating the catalyst powder with magnet, collecting supernatant to determine the concentration of levofloxacin, and removing effect is shown in figure 2.
7) The prepared iron-based WS can be known from the scanning electron microscope image of the attached figure 12The composite material is of a three-dimensional lamellar structure, and the EDX-Mapping chart shows that W, S, Fe elements are uniformly distributed on the surface of the material. As can be seen from FIG. 2, the prepared iron-based WS2The composite material can effectively remove the levofloxacin in water under the action of ball milling.
Example 2
1) Ammonium molybdate, thiourea and ferrous sulfate are weighed according to the mass ratio of 1: 10: 0.05 and are placed in a polytetrafluoroethylene ball-milling reaction kettle with the thickness of 100m L.
2) According to the materials: adding zirconia balls according to the mass ratio of 1:100, and ball-milling for 3 hours under the condition of 1000 revolutions per minute to obtain the precursor powder of the iron-based composite piezoelectric catalytic material.
3) Putting the precursor powder obtained in the step 3) into a tube furnace, and performing reaction in a reactor N2Activating at 500 deg.C for 3h under atmosphere, and naturally cooling to room temperature.
4) Collecting the cooled powder, washing with deionized water to neutrality, and drying at 120 deg.C for 10 hr to obtain iron-based MoS2The piezoelectric catalytic activity of the composite piezoelectric catalyst product is analyzed by an atomic force microscope, and is shown in figure 3.
5) 50m of L rhodamine water sample containing 100 mg/L is measured, 0.05g of iron-based composite piezoelectric catalyst powder is added, and the mixture is placed in a beaker and reacted for 5min under the condition that the power is 200 HZ.
6) Collecting iron-based composite piezoelectric catalyst powder with magnet, and collecting supernatant to determine rhodamine concentration, wherein the piezoelectric catalytic purification effect is shown in figure 4.
7) The piezoelectric performance test of the attached figure 3 shows that the iron-based MoS2The material has obvious piezoelectric response, and when an external force is applied, the composite material can generate 62.5mV surface potential. It can be seen from FIG. 4 that within 50 cycles, the iron-based MoS2The rhodamine B can be rapidly degraded, and when the reaction time is 2 minutes, the rhodamine B can be thoroughly decolorized.
Example 3:
1) 4g of tetrabutyl titanate is weighed out and dissolved in the ethanol solution, and stirred at 500 revolutions per minute.
2) 2g of barium acetate were weighed out and dissolved in 20m L of deionized water.
3) The barium acetate solution obtained in step 2) was added dropwise to the tetrabutyl titanate-ethanol solution in step 1) at a rate of 0.1m L/min with magnetic stirring at 500 revolutions/min.
4) Weighing ferric trichloride and ferrous sulfate with the molar ratio of 1:2, adding the ferric trichloride and the ferrous sulfate into the system obtained in the step 3), placing the system into a ball milling reaction kettle, and carrying out ball milling for 3 hours under the condition of 1000 revolutions per minute to obtain precursor powder of the iron-based composite piezoelectric catalytic material.
5) Putting the precursor powder obtained in the step 2) into a tube furnace, and performing reaction in a reactor under N2Activating at 1000 deg.C for 5h under atmosphere, and naturally cooling to room temperature.
6) Collecting the cooled powder, washing with deionized water to neutrality, and drying at 120 deg.C for 10 hr to obtain Fe @ BaTiO3A composite piezoelectric catalyst product.
7) 50m of L water sample containing 100 mg/L methyl orange is measured, 0.05g of iron-based composite piezoelectric catalyst powder is added, and the mixture is placed in a beaker and stirred for 60min under the condition of 1000 revolutions/min.
8) The catalyst powder was collected with a magnet, and the supernatant was collected to determine the concentration of methyl orange, the removal effect of which is shown in FIG. 5.
9) As can be seen from FIG. 4, Fe @ BaTiO was prepared3The material can rapidly degrade rhodamine B under the stirring action, and when the reaction time is 60min, the removal rate of methyl orange is close to 100%.
Claims (6)
1. A preparation method of an iron-based piezoelectric catalytic material and application thereof in water treatment are characterized by comprising the following specific steps:
1) according to the mole ratio of ferric salt to reactants needed for synthesizing the piezoelectric catalytic material, 1: (50-1000) respectively weighing ferric salt and reactants needed by synthesizing the piezoelectric catalytic material, and uniformly mixing.
2) Adding the mixed powder obtained in the previous step into a polytetrafluoroethylene reaction kettle, and mixing the materials: adding zirconia balls according to the mass ratio of 1:100-500, and ball-milling for 3-5h under the condition of the rotating speed of 500-1500 rpm to obtain the precursor powder of the iron-based composite piezoelectric catalytic material.
3) The precursor powder was placed in a tube furnace at N2Activating at 300-1000 deg.C for 2-5h in atmosphere, and naturally cooling to room temperature.
4) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at 120 ℃ for 5 to 24 hours to obtain the iron-based composite piezoelectric catalyst product.
5) Weighing 0.01-0.5g of iron-based composite piezoelectric catalyst powder, placing the powder in a piezoelectric catalytic system, and testing the performance of the piezoelectric catalytic system, wherein the specific operation is that the iron-based composite piezoelectric catalyst powder with the mass of 0.01-0.5g is weighed, added into a pollutant water sample with the volume of 20-80m L, and mechanical force is introduced to excite the piezoelectric catalytic reaction for 0.01-2 h.
6) The piezoelectric catalyst powder was recovered with a magnet, and the supernatant was taken to measure the concentration of the target contaminant.
The synthetic piezoelectric material reactant can be used for preparing MoS2、WS2、MoSe2、WSe2、ZnO、BiTiO3、CdS、BaTiO3、Pb(Zr0.52Ti0.48)O3And reactants corresponding to the piezoelectric fibers and the piezoelectric ceramics.
The mechanical force initiation method applied to the piezoelectric catalytic reaction system can be a method for providing mechanical force to initiate piezoelectric catalytic reaction for one or more of a ball milling method, an ultrasonic method, a stirring method, an air flow method, a water flow method and the like.
2. The method of claim 1, wherein the iron salt in step 1) is one or a mixture of two or more of ferric chloride, ferric sulfate, ferric nitrate, ferrous sulfate and ferric sulfide.
3. The method of claim 1, wherein the synthetic piezoelectric material reactant of step 1) is for preparing MoS2、WS2、MoSe2、WSe2、ZnO、BiTiO3、CdS、BaTiO3、Pb(Zr0.52Ti0.48)O3Piezoelectric fiber and piezoelectric ceramic elementThe corresponding reactants.
4. The method according to claim 1, wherein the mass ratio of the iron salt in the step 2) to the piezoelectric material precursor is controlled to be 1: 50-1: 1000.
5. The method according to claim 1, wherein the mass ratio of the materials used in the ball milling process of step 3) to the zirconia balls is 1:100 to 1: 500.
6. The method as claimed in claim 1, wherein the piezo-electric catalytic reaction system of step 5) is applied by a mechanical force initiation method such as ball milling, ultrasonic method, stirring, gas flow, water flow, etc.
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