CN115193476A - Photoelectrocatalysis membrane and preparation method and application thereof - Google Patents
Photoelectrocatalysis membrane and preparation method and application thereof Download PDFInfo
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- CN115193476A CN115193476A CN202210830601.XA CN202210830601A CN115193476A CN 115193476 A CN115193476 A CN 115193476A CN 202210830601 A CN202210830601 A CN 202210830601A CN 115193476 A CN115193476 A CN 115193476A
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- 239000012528 membrane Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 36
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 36
- 238000000926 separation method Methods 0.000 claims abstract description 29
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 23
- 239000000178 monomer Substances 0.000 claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 claims abstract description 14
- 238000004132 cross linking Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
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- 238000000034 method Methods 0.000 claims description 21
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- 239000000463 material Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
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- 239000007788 liquid Substances 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 6
- 229920000128 polypyrrole Polymers 0.000 claims description 6
- 229920000123 polythiophene Polymers 0.000 claims description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
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- 239000002033 PVDF binder Substances 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 3
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- 230000008878 coupling Effects 0.000 claims description 3
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- 230000000977 initiatory effect Effects 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
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- 229920000110 poly(aryl ether sulfone) Polymers 0.000 claims description 3
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- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 3
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- 235000006666 potassium iodate Nutrition 0.000 claims description 3
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- 238000007598 dipping method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 21
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 8
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 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 description 4
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- 239000012456 homogeneous solution Substances 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
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- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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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
- B01J27/24—Nitrogen compounds
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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
- 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
- B01J35/33—Electric or magnetic properties
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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
- 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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- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- C02F1/46104—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
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- 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
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
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Abstract
The invention provides a photoelectric catalytic film and a preparation method and application thereof, wherein the photoelectric catalytic film comprises a support film loaded with a functional layer; the functional layer is obtained by cross-linking the carbon nanotube layer and the functional mixed layer which are alternately superposed; the carbon nanotube layer is formed by mixing carbon nanotubesThe rice tube is subjected to suction filtration and loaded on the supporting layer to obtain the rice tube; the functional mixed layer comprises conductive polymer/g-C 3 N 4 Composite, conductive polymer/g-C 3 N 4 The compound is prepared by reacting a polymer monomer with g-C 3 N 4 The interfacial polymerization reaction occurs to obtain the product. The invention overcomes the defects of the existing membrane separation technology and the existing photoelectrocatalysis technology, such as single membrane functionality, low visible light utilization rate and easy recombination of photoproduction electron hole pairs. The photoelectrocatalysis and membrane separation technology can be combined through the photoelectrocatalysis membrane, the photoelectrocatalysis membrane has the characteristics of simple system, no secondary pollution and the like, can realize degradation treatment on organic matters which are difficult to degrade in water, such as phenol, dye molecules and the like in the membrane separation process, and has wide application value in the field of wastewater treatment.
Description
Technical Field
The invention relates to the field of functional membrane separation technology and water treatment, in particular to a photoelectrocatalysis membrane and a preparation method and application thereof.
Background
The membrane separation technology has the advantages of high treatment efficiency, small occupied area, convenient operation and the like, and plays an important role in relieving the problems of water pollution and water resource shortage. However, the conventional membrane separation technology can only separate the pollutants in the water treatment, and cannot completely remove the pollutants. The photoelectrocatalysis technology has important advantages in the aspects of energy application and environmental management, and has the characteristics of simple operation, high degradation efficiency, no secondary pollution and the like. Based on the above, a novel photoelectric membrane material is developed, and a photoelectric technology and a membrane technology are coupled to endow the membrane with new functions (such as pollutant degradation, pollution resistance and the like), so that the method has an important significance for widening the range of the membrane technology in the field of water treatment.
At present, traditional semiconductor materials such as TiO are mostly adopted as the photocatalyst 2 、ZnO、SnO 2 、Fe 2 O 3 However, the above method has problems such as a wide band gap and low sensitivity to visible light. In addition, electrons and holes generated by photoexcitation are easy to recombine, so that the quantum yield is low and the photocatalytic effect is poor.
Disclosure of Invention
Based on the above, the invention provides the photoelectrocatalysis membrane and the preparation method and application thereof, the photoelectrocatalysis membrane has the characteristics of simple system, no secondary pollution and the like, can realize degradation treatment on organic matters which are difficult to degrade in water, such as phenol, dye molecules and the like in the membrane separation process, and has wide application value in the field of wastewater treatment.
According to an aspect of the present invention, there is provided a photoelectrocatalytic film comprising a support film supporting a functional layer;
the functional layer is obtained by cross-linking alternately superposed carbon nanotube layers and functional mixed layers;
the carbon nano tube layer is obtained by pumping and filtering carbon nano tubes to load the supporting layer;
the functional mixed layer comprises conductive polymer/g-C 3 N 4 Composite of the above conductive polymer/g-C 3 N 4 The compound is prepared by reacting a polymer monomer with g-C 3 N 4 The interfacial polymerization reaction is carried out to obtain the product.
According to the embodiment of the invention, the material of the supporting membrane comprises one or more of polyvinylidene fluoride, polyethersulfone, phenolphthalein type non-sulfonated polyarylethersulfone, polyacrylonitrile and bisphenol a type polysulfone.
According to an embodiment of the present invention, the polymer monomer includes one of polyaniline, polypyrrole, polythiophene, polyaniline derivative, polypyrrole derivative, or polythiophene derivative.
According to an embodiment of the present invention, the carbon nanotube includes one of a single-walled carbon nanotube, a double-walled carbon nanotube, or a multi-walled carbon nanotube;
the surface of the carbon nano tube is provided with one or more of amino groups, hydroxyl groups or carboxyl groups.
According to an embodiment of the present invention, the initiator for initiating the interfacial polymerization reaction comprises one of ammonium persulfate, hydrogen peroxide, potassium dichromate, potassium iodate, ferric chloride, ferric tetrachloride, aluminum trichloride, manganese dioxide, and benzoyl peroxide.
According to an embodiment of the present invention, wherein the initiator is in combination with the above-mentioned g-C 3 N 4 In a molar ratio of 1:10-1:100.
according to another aspect of the present invention, there is provided a method for preparing the above-mentioned photoelectrocatalytic film, comprising:
mixing the above g-C 3 N 4 Dispersing into a solution containing the above initiator to obtain g-C 3 N 4 A dispersion liquid;
mixing the dispersion of the polymer monomer with the above g-C 3 N 4 Mixing the dispersion to complete interfacial polymerization to form conductive polymer/g-C 3 N 4 A complex;
mixing the pretreated carbon nanotubes with the conductive polymer/g-C 3 N 4 Loading the composite on the supporting layer through vacuum filtration to respectively obtain the carbon nanotube layer and the functional mixed layer;
and carrying out cross-linking treatment on the carbon nanotube layer and the functional mixed layer which are alternately loaded on the supporting layer to obtain the photoelectric catalytic film.
According to an embodiment of the present invention, the pretreatment of the carbon nanotube may be strong acid or strong alkali treatment.
According to an embodiment of the present invention, the cross-linking of the carbon nanotube layer and the functional mixed layer alternately supported on the support layer to obtain the photoelectrocatalysis membrane includes:
adopting hydrochloric acid solution dipped in glutaraldehyde to obtain the photoelectrocatalysis membrane;
or
And thermally crosslinking for 8-15h by adopting a heating mode at 120-200 ℃ to obtain the photoelectrocatalysis membrane.
According to another aspect of the present invention, there is provided a method using the above-mentioned photoelectrocatalytic film, comprising:
the photoelectrocatalysis membrane is used as an anode, and a conductive material is used as a cathode, and is used for degrading organic matters in the membrane separation process under photoelectric coupling.
According to the technical scheme, the conductive polymer/graphite phase carbon nitride photoelectrocatalysis film, and the preparation method and the application thereof have the following beneficial effects:
the invention overcomes the defects of the existing membrane separation technology and the existing photoelectrocatalysis technology, such as single membrane functionality, low utilization rate of visible light and easy recombination of photo-generated electron hole pairs. The photoelectrocatalysis and membrane separation technology can be combined through the photoelectrocatalysis membrane, the photoelectrocatalysis membrane has the characteristics of simple system, no secondary pollution and the like, can realize degradation treatment on organic matters which are difficult to degrade in water, such as phenol, dye molecules and the like in the membrane separation process, and has wide application value in the field of wastewater treatment.
The photoelectrocatalysis membrane provided by the invention can combine a photoelectricity technology with a membrane separation technology, so that the membrane can simultaneously realize the oxidative degradation of pollutants in the separation process, and the problem that the traditional powder catalyst is not easy to recover is solved, so that the photoelectrocatalysis membrane has a very wide application prospect in the field of wastewater treatment.
Drawings
FIG. 1 is a flow chart illustrating the preparation of a photocatalytic film according to an embodiment of the present invention;
FIG. 2 is a diagram showing an embodiment of a photocatalytic film produced in example 1 of the present invention;
FIG. 3 is a schematic structural diagram of a membrane module using a photoelectrocatalytic membrane in example 2 of the present invention;
FIG. 4 is a graph showing the effect of degrading methylene blue by using a membrane module of a photoelectrocatalytic membrane in example 2 of the present invention.
The figure includes:
1-a working anode;
2-water inlet pipe;
3-a counter electrode;
4-water outlet pipe;
5-a photoelectrocatalysis film;
6-xenon lamp light source.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
At present, traditional semiconductor materials such as TiO are mostly adopted as the photocatalyst 2 、ZnO、SnO 2 、Fe 2 O 3 However, the above method has problems such as a wide band gap and low sensitivity to visible light. In addition, the inventive method is characterized in thatElectrons and holes generated by photoexcitation are easy to recombine, so that the quantum yield is low and the photocatalytic effect is poor.
In recent years, graphite phase carbon nitride (g-C) 3 N 4 ) Has attracted wide attention as a promising new photocatalytic material driven by visible light. The composite material has a unique planar structure, good electrical, optical and stability performances, various preparation means, short process flow and low requirement on equipment. At present, the potential value in the fields of energy, catalysis and environment is continuously developed. However, g-C 3 N 4 Due to the defects of low specific surface area, small active points, high recombination of photogenerated electron-hole pairs and the like in the photocatalysis process, the catalytic efficiency is low.
Conductive polymers such as Polyaniline (PANI) have a pi conjugated structure, have a high specific surface area and good carrier mobility. Mixing a conductive polymer with g-C 3 N 4 Compounding, using the carrier conduction capability of the conductive polymer per se to transfer g-C 3 N 4 The photoproduction electrons can promote the photoproduction electron-hole pairs to form effective separation, and improve the electron transmission capacity, the visible light utilization rate and the photocatalysis capacity. At present, conductive polymers and g-C are used 3 N 4 The preparation of the photoelectric catalytic film by the composite material is not reported.
The conductive polymer/graphite phase carbon nitride (g-C) is used herein 3 N 4 ) The composite is used as a photocatalyst, and the carbon nano tube with good conductivity is used as a conductive material to prepare a novel photoelectric catalytic film which is used in the water treatment process. The photoelectrocatalysis membrane combines membrane filtration and photoelectrocatalysis, light energy is introduced into the water treatment process, and the separation of photoproduction electrons and holes can be further promoted under the action of external voltage, so that the photoelectrocatalysis capability is improved. Through the synergistic effect of membrane separation/photoelectrocatalysis, not only can the mass transfer of pollutants be enhanced, and the problem that the traditional powder catalyst is not easy to recover is reduced, but also the high-efficiency degradation of organic pollutants in the membrane separation process can be realized, and the pollution problem is fundamentally solved.
According to an aspect of the present general inventive concept, there is provided a photocatalytic film including a support film supporting a functional layer;
the functional layer is obtained by cross-linking alternately superposed carbon nanotube layers and functional mixed layers;
the carbon nano tube layer is obtained by pumping and filtering the carbon nano tubes to load the supporting layer;
the functional mixed layer comprises conductive polymer/g-C 3 N 4 Composite, conductive polymer/g-C 3 N 4 The compound is prepared by reacting a polymer monomer with g-C 3 N 4 The interfacial polymerization reaction is carried out to obtain the product.
The invention overcomes the defects of the existing membrane separation technology and the existing photoelectrocatalysis technology, such as single membrane functionality, low visible light utilization rate and easy recombination of photoproduction electron hole pairs. The photoelectrocatalysis and membrane separation technology can be combined through the photoelectrocatalysis membrane, the photoelectrocatalysis membrane has the characteristics of simple system, no secondary pollution and the like, can realize degradation treatment on organic matters which are difficult to degrade in water, such as phenol, dye molecules and the like in the membrane separation process, and has wide application value in the field of wastewater treatment.
According to the embodiment of the invention, the material of the support membrane comprises one or more of polyvinylidene fluoride, polyethersulfone, phenolphthalein type non-sulfonated polyarylethersulfone, polyacrylonitrile and bisphenol A type polysulfone.
According to the embodiment of the invention, the material of the support film can also be made of other materials with better mechanical strength and compatibility.
According to an embodiment of the present invention, wherein the polymer monomer includes one of polyaniline, polypyrrole, polythiophene, polyaniline derivative, polypyrrole derivative, or polythiophene derivative.
According to an embodiment of the invention, wherein the carbon nanotubes comprise one of single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes;
the surface of the carbon nano tube is provided with one or more of amino groups, hydroxyl groups or carboxyl groups.
According to an embodiment of the present invention, the initiator for initiating the interfacial polymerization reaction comprises one of ammonium persulfate, hydrogen peroxide, potassium dichromate, potassium iodate, ferric trichloride, ferric tetrachloride, aluminum trichloride, manganese dioxide, and benzoyl peroxide.
According to an embodiment of the invention, wherein the initiator is reacted with g-C 3 N 4 In a molar ratio of 1:10-1:100.
according to the embodiment of the present invention, for example, the molar concentration ratio of the oxidizing agent to the polymeric monomer may be 1.
According to the embodiment of the invention, the molar concentration ratio of the initiator to the high molecular monomer is 1:0.5-1:3.
according to embodiments of the present invention, for example, the molar concentration ratio of the oxidant to the polymeric monomer may be 1.
FIG. 1 is a flow chart of the preparation of the photoelectrocatalytic film of the embodiment of the invention.
According to another aspect of the present invention, as shown in fig. 1, there is provided a method of preparing a photocatalytic film, comprising:
the method comprises the following steps: g to C 3 N 4 Dispersing into a solution containing an initiator to obtain g-C 3 N 4 A dispersion liquid;
step two: mixing the dispersion of the high molecular monomer with g-C 3 N 4 Mixing the dispersion to complete interfacial polymerization to form conductive polymer/g-C 3 N 4 A complex;
step three: mixing the pretreated carbon nanotubes with a conductive polymer/g-C 3 N 4 Loading the composite on the supporting layer through vacuum filtration to respectively obtain a carbon nanotube layer and a functional mixed layer;
step four: and carrying out cross-linking treatment on the carbon nanotube layer and the functional mixed layer which are alternately loaded on the supporting layer to obtain the photoelectric catalytic membrane.
The invention overcomes the defects of the existing membrane separation technology and the existing photoelectrocatalysis technology, such as single membrane functionality, low visible light utilization rate and easy recombination of photoproduction electron hole pairs. The photoelectrocatalysis and membrane separation technology can be combined through the photoelectrocatalysis membrane, the photoelectrocatalysis membrane separation technology has the characteristics of simple system, no secondary pollution and the like, can realize degradation treatment on organic matters which are difficult to degrade in water, such as phenol, dye molecules and the like in the membrane separation process, and has wide application value in the field of wastewater treatment.
The photoelectrocatalysis membrane prepared by the process can combine the photoelectricity technology with the membrane separation technology, so that the membrane can simultaneously realize the oxidative degradation of pollutants in the separation process, and the problem that the traditional powder catalyst is not easy to recycle is solved, so that the photoelectrocatalysis membrane has a very wide application prospect in the field of wastewater treatment.
According to an embodiment of the present invention, in step two, the dispersion of the polymeric monomer is mixed with g-C 3 N 4 Mixing the dispersion at 0-25 deg.C for 4-24 hr, and performing interfacial polymerization reaction between water phase and organic phase to obtain conductive polymer/g-C 3 N 4 And (3) a compound.
According to the embodiment of the present invention, in the second step, the dispersion of the polymer monomer is obtained by dispersing the polymer monomer corresponding to the conductive polymer in the organic solvent.
According to an embodiment of the present invention, in the second step, the organic solvent may be one of dichloromethane, chloroform, carbon tetrachloride, benzene, toluene, xylene, pentane, cyclohexane, n-hexane, and mineral oil.
According to the embodiment of the present invention, the pretreatment of the carbon nanotubes may be one of strong acid treatment and strong alkali treatment.
According to an embodiment of the present invention, the strong acid may be a mixed acid of concentrated nitric acid and concentrated sulfuric acid in a volume ratio of 1.
According to the embodiment of the invention, the cross-linking treatment is performed on the carbon nanotube layer and the functional mixed layer which are alternately loaded on the support layer, so as to obtain the photoelectric catalytic film, and the method comprises the following steps:
dipping in hydrochloric acid solution of glutaraldehyde to obtain a photoelectrocatalysis membrane;
or
And thermally crosslinking for 8-15h by adopting a heating mode at 120-200 ℃ to obtain the photoelectric catalytic membrane.
According to an embodiment of the present invention, the heating temperature may be 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃ or the like.
According to the embodiment of the invention, the crosslinking time can be 8h, 9h, 10h, 11h, 12h, 13h, 14h and 15h.
According to another aspect of the present invention, there is provided a method of using a photoelectrocatalytic film, comprising:
the photoelectric catalytic membrane is used as an anode, and the conductive material is used as a cathode for realizing the degradation of organic matters in the membrane separation process under the photoelectric coupling.
According to an embodiment of the present invention, the method of using the photoelectrocatalytic film may be: the conductive polymer/g-C 3 N 4 The photoelectrocatalysis membrane is coupled with photoelectricity to realize the degradation of organic matters in the membrane separation process.
According to the embodiment of the invention, the method for utilizing the photoelectrocatalysis film specifically comprises the following steps: connecting the prepared photoelectric catalytic membrane as an anode with a positive electrode of a direct current power supply, connecting a conductive material as a cathode with a negative electrode of the direct current power supply, connecting the electrodes by using a lead, and controlling the working voltage to be 0-30V; simulating natural illumination conditions in experiments by using a xenon lamp, wherein the illumination power of the xenon lamp is 0-300W, and the distance between the light source and the photoelectrocatalysis film is 0-5 cm; one of cross flow or dead-end filtration is adopted, and the stock solution to be filtered permeates through the photoelectric catalytic membrane under the action of transmembrane pressure difference, so that the photoelectric auxiliary membrane filtration process is realized.
According to an embodiment of the present invention, the cathode conductive material is made of one or two of titanium, platinum, stainless steel, graphite sheet or carbon fiber cloth.
The technical solutions of the present invention are described in detail by the following preferred embodiments, and it should be noted that the following specific embodiments are only for examples and are not intended to limit the present invention.
Example 1: and (4) preparing a sample.
FIG. 2 is a schematic diagram of the photocatalytic film prepared in example 1 of the present invention.
2.28mg of ammonium persulfate was dissolved in 10mL of a hydrochloric acid (1 mol/L) solution, sufficiently dissolved and stirred, and 22.8mg of g-C was added thereto 3 N 4 By ultrasonic divisionThe powder is prepared into a homogeneous solution to obtain g-C 3 N 4 And (3) dispersing the mixture.
0.93mg of aniline monomer was dissolved in 10mL of an n-hexane solution, and dispersed into a homogeneous solution by stirring or ultrasonic wave to obtain a dispersion liquid containing a polymer monomer.
G to C 3 N 4 Transferring the dispersion liquid and the dispersion liquid of the high molecular monomer into a beaker, and reacting for 24 hours at 4 ℃ to generate PANI/g-C 3 N 4 And (3) a compound. After the reaction is finished, the obtained product is washed for 3-5 times by using ethanol and deionized water and then dried for later use.
And (2) acidizing the carbon nano tube by using a mixed acid solution of 70wt% of concentrated nitric acid and concentrated sulfuric acid in a volume ratio of 1.
Ultrasonically dispersing the prepared acidified carbon nano tube into 100mL of deionized water to prepare a homogeneous solution with the concentration of 0.2 g/L.
The dispersion is filtered to the surface of a supporting layer (a polyvinylidene fluoride micro-filtration membrane with the aperture of 0.1 mu m) by vacuum filtration, and then is washed for 3 to 5 times by deionized water and dried in a vacuum oven at 40 ℃ for standby.
Mixing the above prepared PANI/g-C 3 N 4 The composite is dispersed into 100mL of deionized water by ultrasonic wave to prepare a homogeneous solution with the concentration of 0.2 g/L. Dispersing the PANI/g-C 3 N 4 And loading on the surface by using a vacuum filtration mode. And cleaning with deionized water and drying. The prepared membrane is thermally crosslinked for 10 hours in a vacuum oven at 180 ℃ to obtain the photoelectrocatalysis membrane shown in figure 2.
Example 2: and (3) application of the sample.
FIG. 3 is a schematic structural diagram of a membrane module using a photoelectrocatalytic membrane in example 2 of the present invention.
FIG. 4 is a graph showing the effect of degrading methylene blue by using a membrane module of a photoelectrocatalytic membrane in example 2 of the present invention.
With the photocatalytic membrane provided in example 1, a filtration experiment was performed in a self-made membrane module, as shown in fig. 3, the membrane module includes a working anode 1, a water inlet tube 2, a counter electrode 3, a water outlet tube 4, and a xenon lamp light source 6.
The photoelectrocatalysis membrane 5 is connected with a conductive material to jointly form a working anode 1, the working anode 1 is connected with the positive electrode of a direct current power supply, a titanium mesh is used as a counter electrode 3 and is connected with the negative electrode of the direct current power supply, the working anode 1 and the counter electrode 3 are placed in parallel, the distance between the working anode 1 and the counter electrode 3 is 2cm, and the working anode 1 and the counter electrode 3 are respectively connected with the positive electrode and the negative electrode of the direct current power supply through copper wires.
The working power of the xenon lamp light source 6 is 300W, and the distance between the xenon lamp light source 6 and the surface of the photoelectrocatalysis film 5 is 2cm.
Before the system runs, the photoelectrocatalysis membrane 5 is immersed in simulated wastewater for 2 hours under dark condition to reach adsorption saturation, and then a photoelectrocatalysis experiment is carried out.
Methylene blue is used as a simulated pollutant, the concentration of the pollutant is 1mg/L, and Na is adopted 2 SO 4 (10 mmol/L) as electrolyte.
The filtration mode in the system is dead-end filtration, and the filtration flow rate of the simulated wastewater is 4mL/min.
As shown in FIG. 4, the current density was 40mA/m 2 When the system voltage is 7V, the degradation effect of the system on methylene blue is 98%, and the system shows good photocurrent responsiveness and visible light catalytic activity.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A photoelectrocatalysis membrane comprises a support membrane loaded with a functional layer;
the functional layer is obtained by cross-linking alternately superposed carbon nanotube layers and functional mixed layers;
the carbon nanotube layer is obtained by pumping and filtering carbon nanotubes and loading the carbon nanotubes on the supporting layer;
the functional mixed layerComprising a conductive polymer/g-C 3 N 4 Composite of the electrically conductive polymer/g-C 3 N 4 The compound is prepared by reacting a polymer monomer with g-C 3 N 4 The interfacial polymerization reaction occurs to obtain the product.
2. The photoelectrocatalysis membrane of claim 1, wherein the material of the support membrane comprises one or more of polyvinylidene fluoride, polyethersulfone, phenolphthalein type non-sulfonated polyarylethersulfone, polyacrylonitrile and bisphenol A type polysulfone.
3. The photoelectrocatalytic film of claim 1, wherein the polymeric monomer comprises one of polyaniline, polypyrrole, polythiophene, polyaniline derivatives, polypyrrole derivatives, or polythiophene derivatives.
4. The photoelectrocatalytic film of claim 1, wherein the carbon nanotubes comprise one of single-walled carbon nanotubes, double-walled carbon nanotubes, or multi-walled carbon nanotubes;
the surface of the carbon nano tube is provided with one or more of amino groups, hydroxyl groups or carboxyl groups.
5. The photoelectrocatalytic membrane of claim 1, wherein an initiator for initiating the interfacial polymerization reaction comprises one of ammonium persulfate, hydrogen peroxide, potassium dichromate, potassium iodate, ferric trichloride, ferric tetrachloride, aluminum trichloride, manganese dioxide, and benzoyl peroxide.
6. The photocatalytic film according to claim 1, wherein the initiator reacts with the g-C 3 N 4 The molar concentration ratio of (1): 10-1:100.
7. a method of making the photoelectrocatalytic film of any one of claims 1-6, comprising:
subjecting said g-C to 3 N 4 Dispersing into a solution containing said initiator to obtain g-C 3 N 4 A dispersion liquid;
mixing a dispersion of a polymer monomer with said g-C 3 N 4 Mixing the dispersion to complete interfacial polymerization to form conductive polymer/g-C 3 N 4 A complex;
mixing the pretreated carbon nanotubes with the conductive polymer/g-C 3 N 4 Loading the composite on the supporting layer through vacuum filtration to respectively obtain the carbon nanotube layer and the functional mixed layer;
and carrying out cross-linking treatment on the carbon nanotube layer and the functional mixed layer which are alternately loaded on the supporting layer to obtain the photoelectric catalytic membrane.
8. The method of claim 7, wherein the carbon nanotubes are pretreated by one of strong acid or strong base treatment.
9. The method of claim 7, wherein the cross-linking the carbon nanotube layer and the functional mixed layer alternately supported on the support layer to obtain the photoelectrocatalytic film comprises:
dipping in a hydrochloric acid solution of glutaraldehyde to obtain the photoelectrocatalysis membrane;
or
And thermally crosslinking for 8-15h by adopting a heating mode of 120-200 ℃ to obtain the photoelectrocatalysis membrane.
10. A method of using the photoelectrocatalytic membrane of any one of claims 1-6, comprising:
the photoelectrocatalysis membrane is used as an anode, and a conductive material is used as a cathode, and is used for degrading organic matters in the membrane separation process under photoelectric coupling.
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