CN112973464A - Preparation method and application of photocatalytic sewage treatment membrane - Google Patents
Preparation method and application of photocatalytic sewage treatment membrane Download PDFInfo
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- CN112973464A CN112973464A CN202110188798.7A CN202110188798A CN112973464A CN 112973464 A CN112973464 A CN 112973464A CN 202110188798 A CN202110188798 A CN 202110188798A CN 112973464 A CN112973464 A CN 112973464A
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- photocatalytic
- membrane
- sewage treatment
- mercaptoguanosine
- polydopamine
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 87
- 239000012528 membrane Substances 0.000 title claims abstract description 71
- 239000010865 sewage Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 230000015556 catabolic process Effects 0.000 claims abstract description 24
- 238000006731 degradation reaction Methods 0.000 claims abstract description 24
- 229920001690 polydopamine Polymers 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 229920002301 cellulose acetate Polymers 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 53
- KZELNMSPWPFAEB-UMMCILCDSA-N 2-amino-9-[(2r,3r,4s,5r)-3,4-dihydroxy-5-(hydroxymethyl)oxolan-2-yl]-8-sulfanylidene-3,7-dihydropurin-6-one Chemical compound C1=2NC(N)=NC(=O)C=2NC(=S)N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O KZELNMSPWPFAEB-UMMCILCDSA-N 0.000 claims description 20
- UJHZBYGCKHWQJT-UHFFFAOYSA-N 5-(sulfanylmethyl)-1h-pyrimidine-2,4-dione Chemical compound SCC1=CNC(=O)NC1=O UJHZBYGCKHWQJT-UHFFFAOYSA-N 0.000 claims description 11
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 11
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 11
- 230000003197 catalytic effect Effects 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 9
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007853 buffer solution Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229920006221 acetate fiber Polymers 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
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- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229960003638 dopamine Drugs 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 15
- 238000000926 separation method Methods 0.000 abstract description 15
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 11
- 230000004907 flux Effects 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 22
- CSEBQCRCMWJLGU-UHFFFAOYSA-N ctk8g9296 Chemical compound C1=CC2=CC=C3SC4=CC=CC=C4CC3=C2C2=C1C(=O)OC2=O CSEBQCRCMWJLGU-UHFFFAOYSA-N 0.000 description 16
- 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 14
- 229940043267 rhodamine b Drugs 0.000 description 14
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 6
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- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
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- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- 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 1
- 229910002703 Al K Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- -1 O four elements Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 1
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- 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
- 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
-
- 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
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- 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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method and application of a photocatalytic sewage treatment membrane, and relates to the technical field of sewage treatment. The preparation method of the photocatalytic sewage treatment membrane comprises the step of modifying 8-mercaptoguanosine-polydopamine in a reduced pressure suction filtration modeNature g-C3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4And (5) performing suction filtration on the cellulose acetate membrane. The photocatalytic sewage treatment membrane prepared by the invention has excellent membrane flux, improves the interception of organic pollutants, enhances the degradation of the organic pollutants under the condition of visible light, effectively prevents the problem of membrane pollution, improves the membrane flux, enhances the membrane separation performance, especially has excellent separation effect in the aspect of oil-water separation, and has huge application prospect in the aspect of water purification treatment.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a preparation method and application of a photocatalytic sewage treatment membrane.
Background
With the development of world industrialization, water pollution is becoming more serious, pollutants in water also show a diversified trend, and common pollutants comprise toxic heavy metals, natural toxins, medicines, organic pollutants and the like. Common purification techniques are chlorine, ozone and ultraviolet disinfection as well as filtration, adsorption, standing, etc., but these methods are often not very effective for new pollutants and may lead to secondary pollution. In recent years, due to the characteristics of no pollution, safety and the like of the photocatalytic technology, the treatment and degradation of pollutants by the photocatalytic technology has become a research hotspot in the environmental field.
The combined process of photocatalytic oxidation and membrane technology has been developed in recent years. Such devices formed using photocatalytic-membrane composite techniques are often referred to as photocatalytic membrane reactors. Since the membrane technology can simply and effectively separate the photocatalyst particles, the photocatalytic-membrane composite technology or photocatalytic membrane reactor has been greatly regarded and rapidly developed in recent years, and has occupied an important position in the research field of photocatalytic oxidation. The photocatalytic film in the prior art generally has the problems of uneven photocatalyst loading, easy agglomeration, low catalytic activity and the like, and has the defects of poor heat resistance of a matrix, difficulty in effective recycling and the like.
Polymer graphite phase carbon nitride (g-C)3N4) The graphene-like catalyst has a graphene-like structure, and can be used as a catalyst for solar energy conversion and environmental pollutant degradation due to excellent chemical stability and a unique electronic band structure. And g-C3N4The preparation of the raw materials is convenientThe photocatalyst is easy to obtain, has a simple preparation method, and can be used as a cheap, stable and metal-free visible light photocatalyst to be applied to the fields of photocatalytic degradation of pollutants, hydrogen and oxygen production through water decomposition and organic synthesis. However, photo-generated charges are easily recombined, so that g-C3N4The catalytic activity of (a) has not yet been satisfactory for large-scale applications.
Disclosure of Invention
The invention aims to provide a preparation method and application of a photocatalytic sewage treatment membrane, the photocatalytic sewage treatment membrane has excellent membrane flux, improves the interception of organic pollutants, enhances the photocatalytic degradation performance, and has good oil-water separation effect.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a photocatalytic material comprises 8-mercaptoguanosine-polydopamine modified g-C3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4. g-C modified by 8-mercaptoguanosine-polydopamine or 5-mercaptomethyluracil-polydopamine3N4The energy gap of the material is reduced, the absorption of visible light is further improved, the photoelectron transfer is accelerated, the combination of holes and electrons is avoided, the adsorption degradation capability of organic dye is enhanced, the degradation rate is improved, and the catalytic degradation capability of carbon nitride is further improved.
The invention also discloses the application of the photocatalytic material in the fields of sewage treatment or water decomposition hydrogen and oxygen production or organic synthesis.
Preferably, the 8-mercaptoguanosine and/or 5-mercaptomethyluracil is used for reducing the energy gap of the photocatalytic material, improving the removal rate of organic dye and enhancing the catalytic degradation performance.
The preparation method of the photocatalytic material comprises the following steps:
adding g-C into dopamine hydrochloride3N4Stirring and mixing the suspension evenly; and adding a Tris-HCl buffer solution containing 8-mercaptoguanosine or 5-mercaptomethyluracil, adjusting the pH value, heating for reaction, centrifuging, washing and drying to obtain the photocatalytic material.
Preferably, the dopamine hydrochloride is reacted withg-C3N4The mass ratio of (1): 10-12; the mass ratio of dopamine hydrochloride to 8-mercaptoguanosine or 5-mercaptomethyluracil is 1: 1 to 1.5; the solid-to-liquid ratio of 8-mercaptoguanosine or 5-mercaptomethyluracil to the Tris-HCl buffer solution is 1 g: 2-3.5 mL; g-C3N4The concentration of the suspension is 4-6 mg/mL.
Preferably, the pH is adjusted to 8-9, the reaction temperature is 60-65 ℃, and the reaction time is 20-24 h.
Preferably, in g-C of the above photocatalytic material3N4Doped with benzothioxanthene dicarboxylic anhydride, wherein the benzothioxanthene dicarboxylic anhydride is in g-C3N40.8-2% of the mass. The benzothioxanthene dicarboxylic anhydride has good thermodynamic stability, is an excellent electron acceptor, is introduced into a chemical framework of the carbon nitride material, and can reduce the degree of order of a carbon nitride material sheet layer by optimizing a conjugated structure of the carbon nitride material, further improve the photocatalytic performance of the composite material and enhance the degradation of organic dye; and the doped benzothioxanthene dicarboxylic anhydride can effectively improve the conductivity of the material.
More preferably, g-C3N4The preparation method of the middle-doped benzothioxanthene dicarboxylic anhydride comprises the following steps: dissolving benzothioxanthene dicarboxylic anhydride in a solvent, adding g-C3N4Stirring, heating to remove the solvent, then placing the solid in an alumina crucible, and calcining for 4-5 hours at 500-550 ℃.
A photocatalytic sewage treatment membrane, which comprises the 8-mercaptoguanosine-polydopamine modified g-C3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4. The prepared photocatalytic material is applied to the sewage treatment membrane, can effectively improve the retention amount of the sewage treatment membrane on organic pollutants, enhances the degradation of the organic pollutants under the condition of visible light illumination, effectively prevents the problem of membrane pollution, improves the membrane flux, enhances the membrane separation performance, especially has excellent separation effect in the aspect of oil-water separation, and has huge application prospect in the aspect of water purification treatment. 8-mercaptoguanosine-polydopamine modified g-C3N4And 5-Thiomethyl-pyrimidine-Polydopamine modified g-C3N4The synergistic use has an enhancement effect on the improvement of the performance of the sewage treatment membrane.
Preferably, the photocatalytic sewage treatment membrane further comprises an acetate fiber membrane.
The preparation method of the photocatalytic sewage treatment membrane comprises the step of modifying the g-C by 8-mercaptoguanosine-polydopamine in a decompression suction filtration mode3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4And (5) performing suction filtration on the cellulose acetate membrane.
The invention also discloses the application of the photocatalytic sewage treatment membrane in the field of sewage treatment.
Compared with the prior art, the invention has the following beneficial effects:
modification of g-C with 8-mercaptoguanosine-polydopamine3N4Or 5-mercaptomethyluracils-polydopamine modified g-C3N4The material energy gap is effectively reduced, the absorption of visible light is improved, the photoelectron transfer is accelerated, the combination of holes and electrons is avoided, the adsorption degradation capability of organic pollutants is enhanced, the degradation rate is improved, and the catalytic degradation capability of the photocatalytic material is further improved. In g-C3N4The benzothioxanthene dicarboxylic anhydride is doped, so that the photocatalytic performance of the composite material is further improved, and the degradation of organic dye is enhanced; and the doped benzothioxanthene dicarboxylic anhydride can effectively improve the conductivity of the material. The photocatalytic material prepared by the invention is applied to a sewage treatment membrane, can effectively improve the retention amount of the sewage treatment membrane on organic pollutants, can enhance the degradation of the organic pollutants under the condition of visible light, effectively prevents the problem of membrane pollution, improves the membrane flux, enhances the membrane separation performance, especially has excellent separation effect in the aspect of oil-water separation, and has huge application prospect in the aspect of water purification treatment.
Therefore, the invention provides a preparation method and application of the photocatalytic sewage treatment membrane, and the photocatalytic sewage treatment membrane has excellent membrane flux, improves the interception of organic pollutants, enhances the photocatalytic degradation performance, and has good oil-water separation effect.
Drawings
FIG. 1 shows the results of XPS test in test example 1 of the present invention;
FIG. 2 is a diagram showing the result of measuring the forbidden band width of the photocatalytic material in experimental example 1 of the present invention;
FIG. 3 shows the results of the electrochemical performance test in test example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
g-C used in the examples of the invention3N4The product is ordered from the Bailingwei technology, and the purity is more than or equal to 99 percent; the cellulose acetate membrane used was purchased from chemical reagents of national drug group, ltd.
Example 1:
preparation of photocatalytic material:
500mg of g-C are weighed3N4Adding into a 250mL beaker filled with 100mL deionized water to form a suspension and performing ultrasonic dispersion for 30 min; adding dopamine hydrochloride (dopamine hydrochloride and g-C)3N4The mass ratio of (1): 11.5), stirring for 60min under magnetic force at room temperature to mix evenly; then, a Tris-HCl buffer solution (the solid-to-liquid ratio of 8-mercaptoguanosine to the Tris-HCl buffer solution is 1 g: 2.5mL) containing 8-mercaptoguanosine (the mass ratio of dopamine hydrochloride to 8-mercaptoguanosine is 1: 1.3) is added, the pH value is adjusted to 8.5 by using a 1M NaOH solution, and the mixture is magnetically stirred and reacted for 24 hours at the temperature of 60 ℃. And cooling the reacted suspended sample to room temperature, centrifuging for 10min (4000r/min) by using a centrifugal machine, collecting a solid sample, washing for 3 times by using deionized water, and drying for 12h at the temperature of 60 ℃ to obtain the photocatalytic material.
Preparation of a photocatalytic sewage treatment membrane:
4mL of the photocatalytic material suspension solution (1mg/mL) prepared above was pipetted into a beaker, diluted to 100mL with deionized water and ultrasonically dispersed for 15 min. 25mL of the dispersion was measured, and a sample was filtered onto an acetate fiber membrane (filter diameter 4X 4cm, average pore diameter 0.22 μm) by vacuum (-0.1MPa) filtration using a sand core filtration apparatus to form a photocatalytic sewage treatment membrane.
Example 2:
photocatalytic materialThe preparation of the batch differed from example 1 in that: dopamine hydrochloride and g-C3N4The mass ratio of (1): 10; the mass ratio of dopamine hydrochloride to 8-mercaptoguanosine is 1: 1; the solid-to-liquid ratio of the 8-mercaptoguanosine to the Tris-HCl buffer solution is 1 g: 2 mL; g-C3N4The concentration of the suspension was 4.5 mg/mL.
A photocatalytic wastewater treatment membrane was prepared in the same manner as in example 1.
Example 3:
the photocatalytic material was prepared differently from example 1 in that: dopamine hydrochloride and g-C3N4The mass ratio of (1): 11; the mass ratio of dopamine hydrochloride to 8-mercaptoguanosine is 1: 1.4; the solid-to-liquid ratio of the 8-mercaptoguanosine to the Tris-HCl buffer solution is 1 g: 3 mL; g-C3N4The concentration of the suspension was 5.4 mg/mL.
A photocatalytic wastewater treatment membrane was prepared in the same manner as in example 1.
Example 4:
the photocatalytic material was prepared differently from example 1 in that: 5-mercaptomethyluracils were used instead of 8-mercaptoguanosine.
A photocatalytic sewage treatment membrane was prepared in a manner different from that of example 1 in that: the photocatalytic material was prepared in this example.
Example 5:
preparation of a photocatalytic sewage treatment membrane:
2mL each of the photocatalytic material suspension solutions of example 1 and example 4 (1mg/mL) were pipetted into a beaker, diluted to 100mL with deionized water and ultrasonically dispersed for 15 min. 25mL of the dispersion was measured, and the sample was filtered onto a cellulose acetate membrane filter (filter diameter 4X 4cm, average pore size 0.22 μm) by vacuum (-0.1MPa) filtration using a sand core filtration apparatus to form a photocatalytic sewage treatment membrane.
Example 6:
benzothioxanthene dicarboxylic acid anhydride doped g-C3N4The preparation of (1):
dissolving benzothioxanthene dicarboxylic anhydride in a solvent, adding g-C3N4Stirring, heating to remove solventThen placing the solid in an alumina crucible, and calcining for 5 hours at 500 ℃. Wherein the benzothioxanthene dicarboxylic anhydride is in the g-C range3N41.2% of the mass.
The photocatalytic material was prepared differently from example 1 in that: g-C doped with benzothioxanthene dicarboxylic acid anhydride3N4Substitution of g-C3N4。
A photocatalytic sewage treatment membrane was prepared in a manner different from that of example 1 in that: the photocatalytic material was prepared in this example.
Example 7:
benzothioxanthene dicarboxylic acid anhydride doped g-C3N4Was prepared as in example 6.
The photocatalytic material was prepared differently from example 4 in that: g-C doped with benzothioxanthene dicarboxylic acid anhydride3N4Substitution of g-C3N4。
A photocatalytic sewage treatment membrane was prepared in the following manner, in contrast to example 4: the photocatalytic material was prepared in this example.
Example 8:
a photocatalytic sewage treatment membrane was prepared in the following manner, in contrast to example 5: the photocatalytic materials were prepared as in examples 6 and 7.
Comparative example 1:
a photocatalytic sewage treatment membrane was prepared in a manner different from that of example 1 in that: with g-C3N4Instead of photocatalytic material.
Comparative example 2:
the photocatalytic material was prepared differently from example 1 in that: no 8-mercaptoguanosine was added.
A photocatalytic wastewater treatment membrane was prepared in the same manner as in example 1.
Test example 1:
characterization and Performance testing of photocatalytic materials
1. XPS test
The surface chemical element composition of the sample was subjected to photoelectron spectroscopy using an XSAM800 type multifunctional X photoelectron spectrometer (KRATOS), with Al K α as a radiation, and the charge effect was corrected using contaminated carbon C1s (284.6 eV).
The photocatalytic materials obtained in example 1, example 4 and comparative example 2 were subjected to the above-described tests, and the results are shown in FIG. 1. As can be seen from the analysis of the graph, in comparative example 2, the content of N is lower than that of C due to the adhesion of polydopamine to g-C3N4Surface, thus reducing g-C3N4The detected N content. Compared with comparative example 2, the photocatalytic materials prepared in examples 1 and 4 contain S, C, N, O four elements, and C, N, O has a higher content, indicating that 8-mercaptoguanosine and 5-mercaptomethyluracyl pyrimidine are successfully grafted on polydopamine.
2. Ultraviolet visible spectrum analysis (UV-vis)
The ultraviolet visible spectrum is generated by valence electron transition, and can be used for researching the light absorption performance of materials, the structures, oxidation states, coordination states, symmetry and the like of transition metal ions and complexes thereof. Based on the Kubelka-munk formula, the [ F (R) is obtained by respectively using an ultraviolet visible diffraction spectrum and an absorption spectrum∞)hν]2And (3) calculating the forbidden bandwidth of the photocatalyst according to a vs.
The above-described tests were performed on the samples obtained in comparative example 2, example 1 and example 4, and the results are shown in FIG. 2. As can be seen from the analysis of the figure, the forbidden band width of the sample prepared in example 1 is 1.92eV, the forbidden band width of the sample prepared in example 4 is 1.99eV, which is obviously smaller than the forbidden band width of 2.13eV of comparative example 2, and the results show that the modified g-C of 8-mercaptoguanosine-polydopamine or 5-mercaptomethyluramidopyrimidine polydopamine3N4The forbidden band width can be reduced, and the modification on the surface of the semiconductor material can promote light absorption and accelerate proton coupling electron separation so as to improve the photocatalysis effect.
3. Test for catalytic Performance
And (3) evaluating the performance of photocatalytic degradation on a sample at room temperature by taking rhodamine B (RhB) in the printing and dyeing wastewater as a target. During the experiment, the degradation substances passed through the photocatalytic material in a flowing state. A sample (0.2g) was placed in the quartz tube. Initial RhB concentration of 1X 10-5mol/L, peristaltic pump flow 1.33mL/min. In addition, the samples were tested for photocatalytic activity under xenon lamp illumination (300W, plsxe 300, Beijing philiae technology co., ltd., China). In the illumination process, the distance from the xenon lamp light source to the sample is 10cm and is kept consistent all the time. Samples were taken every 30min and absorbance values of RhB solutions at different times were determined using an ultraviolet-visible spectrophotometer (UV-6300 PC). The solution after the test is finished is poured back into the original beaker again. The photocatalytic activity of a sample can be quantitatively evaluated by the amount of target that degrades over time. And finally, calculating the concentration of the RhB solution at the corresponding moment according to the measured absorbance value by drawing a standard curve, drawing a concentration change curve, and further calculating to obtain the removal rate.
The results of the above tests on the photocatalytic materials prepared in comparative examples 1 to 2, examples 1 to 4, and examples 6 to 7 are shown in Table 1:
TABLE 1 RhB removal Rate
As can be seen from the analysis in Table 1, the photocatalytic material prepared in example 1 has significantly higher degradation rate to RhB than comparative examples 1 and 2 and significantly higher degradation rate to comparative examples 1 and 2 after being irradiated by light for 60min and 90min, and the effect of example 4 is equivalent to that of example 1, indicating that the modified g-C of 8-mercaptoguanosine-polydopamine or 5-mercaptomethuramidopyrimidine polydopamine3N4The degradation rate of the photocatalytic material to organic pollutants can be effectively improved, and the degradation rate is accelerated. The results of examples 6 to 8 were better than those of examples 1, 4 and 5, respectively, and show that g-C was doped with benzothioxanthene dicarboxylic anhydride3N4Has the function of enhancing the catalytic performance. The effect of example 5 is significantly better than that of examples 1 and 4, indicating that the photocatalytic materials containing 8-mercaptoguanosine and 5-mercaptomethyluracil synergistically act as an enhancement.
4. Electrochemical testing
The test was carried out using an RSC type electrochemical workstation. Firstly, 10mg of catalyst is dispersed in 5mL of water by ultrasound, and is evenly coated on ITO glass with the thickness of 3 multiplied by 4cm at 70 DEG CPre-drying under the condition, and calcining at 200 ℃ for 10 min. In order to fix the illumination area of the catalyst, the edge of the ITO glass is covered by an insulating tape, so that the effective illumination area is 1cm2. Selecting a Pt motor as a counter electrode, a KCl standard calomel electrode as a reference electrode, ITO glass coated with a catalyst as a working electrode, and 0.1M NaSO4 solution as an electrolyte, and carrying out a photoelectrochemical test on the catalyst under the condition of-0.2V applied voltage, wherein the total test time is 400s, and the test interval (lamp switching interval) is 40s, so as to obtain a relation curve of transient photocurrent of the material and time.
The photocatalytic materials obtained in example 1, example 4 and example 6 were subjected to the above-described tests, and the results are shown in fig. 3. As can be seen from the graph, the photocurrent value of the material prepared in example 6 is significantly higher than that of example 1, the photocurrent value of the material prepared in example 7 is higher than that of example 4, and example 4 is equivalent to example 1, which proves that benzothioxanthene dicarboxylic anhydride is doped with g-C3N4Effectively improving the conductivity of the material.
Test example 2
Performance testing of Sewage treatment membranes
Preparation of oil-water emulsion and organic dye
Mixing oil and water according to the weight ratio of 1: 100 volume ratio in a 250mL beaker, and weighing a certain mass of emulsifier SDS (0.2 mg/mL in emulsion) in the beaker, stirring for 1h by ultrasonic, and then stirring for 4h by magnetic force. Standing the emulsified mixture for 12h, and removing residual floating oil. A diesel/water emulsion was prepared in the above manner.
Photocatalytic performance of photocatalytic sewage treatment membrane and separation and purification test of RhB-oil-water emulsion
The photocatalytic efficiency of the membrane was evaluated by degradation of RhB solution. 2.5mg of the sample was placed in a beaker containing 100mL of a methylene blue solution (5 mg/L); under the condition of room temperature, a long-arc xenon lamp of 500W is used as a lamp source, the distance between the lamp source and the illumination is 35cm, after 5 hours of illumination, 3mL of liquid is measured, an ultraviolet-visible spectrophotometer is used for testing the absorbance curve of the liquid, and the absorbance value (A) at the highest absorption peak is recorded. Catalytic experiments with the addition of the co-catalyst hydrogen peroxide (1mL, 30 wt%) to the solution were also performed according to the experimental procedure above. Wherein the degradation efficiency equation of the fuel is as follows:
degradation efficiency (%) ═ C0-Ct)/C0×100％＝(A0-At)/A0×100％
Wherein, C0、CtAnd A0、AtThe concentration and absorbance of the solution at reaction time 0 and t, respectively.
The 15mL of the diesel/water emulsion prepared above and a 15mL of the LRhB (5mg/L) solution were transferred and mixed uniformly, and the mixture was separated and purified under visible light irradiation and vacuum filtration using a 1mg sample membrane. The collected filtrate, RhB concentration and oil content of the filtrate were measured using a visible-ultraviolet spectroscopy and TOC-Vcph analyzer, respectively. Water and oil flux (J)w) The oil and RhB retention (R) equations are as follows:
Jw＝V/(A×T)
R＝(1-Cp/Cf)×100％
wherein JwIs the membrane permeation flux of water and emulsion; v is the volume of liquid (L); a is the effective area (m) of the film2) (ii) a T is the suction filtration time (h); r is the oil and RhB retention. CfAnd CpInitial concentrations of oil and RhB and filtered concentrations (mg/L) were respectively.
The results of the above tests on films prepared in comparative examples 1 to 2 and examples 1 to 8 are shown in Table 2:
table 2 film performance test results
As can be seen from Table 2, the degradation efficiency of the membrane prepared in example 1 on RhB is obviously higher than that of comparative example 1 and comparative example 2, the water and oil flux is obviously improved, the retention rate on organic RhB and oil is obviously improved, the effect of example 4 is equivalent to that of the example, and the results show that the membrane prepared in example 2 has the same effect as that of the example, and the membrane prepared in example 4 has the effect of modifying g-C-polydopamine by 8-mercaptoguanosine-polydopamine or 5-mercaptomethyluracil polydopamine3N4The catalytic performance and the separation performance of the membrane can be effectively improved, and the oil-water separation effect is enhanced. Example 5 is remarkably goodIn examples 1 and 4, it is shown that the photocatalytic materials containing 8-mercaptoguanosine and 5-mercaptomethyluracil act synergistically to enhance the effect.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A photocatalytic material comprises 8-mercaptoguanosine-polydopamine modified g-C3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4。
2. Use of the photocatalytic material of claim 1 in the fields of wastewater treatment or water decomposition for hydrogen production and oxygen production or organic synthesis.
3. Use according to claim 2, characterized in that: the 8-mercaptoguanosine and/or 5-mercaptomethyluracil is used for reducing the energy gap of a photocatalytic material, improving the removal rate of organic dye and enhancing the catalytic degradation performance.
4. A method for preparing the photocatalytic material according to claim 1, comprising:
adding g-C into dopamine hydrochloride3N4Stirring and mixing the suspension evenly; and adding a Tris-HCl buffer solution containing 8-mercaptoguanosine or 5-mercaptomethyluracil, adjusting the pH value, heating for reaction, centrifuging, washing and drying to obtain the photocatalytic material.
5. The method for preparing a photocatalytic material according to claim 4, characterized in that: the dopamine hydrochloride and g-C3N4The mass ratio of (1): 10-12; the mass ratio of dopamine hydrochloride to 8-mercaptoguanosine or 5-mercaptomethyluracil is 1: 1 to 1.5; the solid-to-liquid ratio of 8-mercaptoguanosine or 5-mercaptomethyluracil to the Tris-HCl buffer solution is 1 g: 2-3.5 mL; g-C3N4The concentration of the suspension is 0.8-1.2 mg/mL.
6. A photocatalytic sewage treatment membrane comprising the 8-mercaptoguanosine-polydopamine modified g-C of claim 13N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4。
7. The photocatalytic sewage treatment membrane of claim 6, characterized in that: the photocatalytic sewage treatment membrane also comprises an acetate fiber membrane.
8. The method for preparing the photocatalytic sewage treatment membrane as recited in claim 7, comprising modifying the g-C with 8-mercaptoguanosine-polydopamine by means of reduced pressure suction filtration3N4And/or 5-mercaptomethyluramidopyrimidine-polydopamine modified g-C3N4And (5) performing suction filtration on the cellulose acetate membrane.
9. Use of a photocatalytic sewage treatment membrane as defined in claim 6 or claim 7 in the field of sewage treatment.
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