CN115353166A - Porous efficient photothermal material, preparation method thereof, efficient photothermal water evaporation film, preparation method and application thereof - Google Patents
Porous efficient photothermal material, preparation method thereof, efficient photothermal water evaporation film, preparation method and application thereof Download PDFInfo
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/08—Thin film evaporation
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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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- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention belongs to the technical field of functional materials, and discloses a porous efficient photothermal material, a preparation method thereof, an efficient photothermal water evaporation film, a preparation method and an application thereof. According to the invention, the porous high-efficiency photo-thermal material is prepared by a supermolecule self-assembly method, the specific surface area of the material is increased, and the copper phthalocyanine is loaded on graphite-phase carbon nitride in a sheet manner to form a type I semiconductor, so that the energy band structure is adjusted, the band gap is reduced, the utilization rate of solar spectrum is increased, the transition of a current carrier is regulated and controlled, and the photo-thermal performance is improved. The preparation method has the advantages of simple preparation process, low cost, mild reaction conditions, realization of continuous preparation and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a porous efficient photothermal material, a preparation method thereof, an efficient photothermal water evaporation film, a preparation method thereof and application thereof.
Background
With the increasingly prominent problems of water resource pollution, energy shortage, environmental pollution and the like, the search for an efficient and energy-saving interfacial evaporation technology becomes an urgent demand in economic development and daily life of people. The method for purifying water by utilizing the interfacial water evaporation effect driven by solar energy has the advantage of sustainability, the effect is mainly based on the photothermal conversion effect of a photothermal material, water vapor in sewage or seawater is evaporated, condensed and collected, the purpose of purifying water is achieved, and the method is one of effective ways for solving the crisis of water pollution and water resource shortage.
Photothermal materials require broadband solar absorption and play a key role in heat conversion and steam generation. The booming research has largely expanded the category of photothermal materials, including metal nanoparticles (Nano Energy,2021, 84.), carbon-based materials (Colloids and Surfaces a: physical and Engineering industries, 2022, 632), polymeric materials (Nanomaterials, 2022,12 (5): 859-859.), and semiconductor materials (Applied Surface Science,2021, 555.). The photo-thermal conversion efficiency of the synthesized Graphene (GR)/ZIF-8 composite material can reach 98.35% (plastic science and technology, 2022, 50 (03): 66-69). Despite the high photothermal effect, these metal-based materials are expensive and brittle, often requiring harsh chemicals such as strong acids and bases to control the microscopic morphology. In order to realize a large-scale practical application, development of a novel material which is environmentally friendly, low in cost, and has excellent evaporation efficiency is urgently required. The novel non-metal graphite phase carbon nitride nano material (g-C3N 4) is used as an optical active N-type semiconductor material, and becomes one of the most potential materials in the aspect of photo-thermal conversion by the characteristics of proper band gap, environmental friendliness, visible light excitation, diversified doping and the like. However, the bulk carbon nitride can only absorb the part with the wavelength less than 400nm in the solar spectrum, and does not have good photo-thermal conversion capability, the utilization efficiency of the g-C3N4 carriers is improved by morphological control, doping and defect control, heterojunction construction, addition of an auxiliary active agent and the like at present, but the method is generally used for photocatalysis, and the photo-thermal conversion efficiency of the g-C3N4 is improved by 37.8% by doping and morphological control.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of the application examples of the invention and to briefly introduce some preferred implementations.
Aiming at the defects of the prior art, the invention provides a porous efficient photothermal material, a preparation method thereof, an efficient photothermal water evaporation film, a preparation method and application thereof, and the porous efficient photothermal material is simple in preparation process, low in cost and environment-friendly.
In order to realize the purpose, the invention adopts the technical scheme that:
a porous high-efficiency photothermal material is a composite material of copper phthalocyanine and graphite-phase carbon nitride, and the composite mode is that the copper phthalocyanine is loaded on the graphite-phase carbon nitride in a small sheet form.
A preparation method of a porous high-efficiency photothermal material takes copper phthalocyanine, melamine and cyanuric acid as raw materials, and is prepared by a thermal polycondensation method after a supermolecule self-assembly method is used in water;
the supermolecule self-assembly method specifically comprises the following steps: mixing copper phthalocyanine, melamine, cyanuric acid and ultrapure water, magnetically stirring for 10-12 h, centrifugally filtering, and freeze-drying at-49-41 ℃ for 20-24 h;
wherein the mol ratio of melamine, cyanuric acid to copper phthalocyanine is 1:1:0.033.
the thermal polycondensation method specifically comprises the following steps: grinding the substances obtained by the supermolecule self-loading method, and then polycondensing for 4 hours in a muffle furnace at 500-550 ℃, wherein the heating rate is 10 ℃/min.
A high-efficiency photothermal water evaporation film comprises a carrier and a porous high-efficiency photothermal material on the surface of the carrier.
A preparation method of a high-efficiency photo-thermal water evaporation film comprises the steps of dispersing 20mg of porous high-efficiency photo-thermal material in 40ml of 0.2wt% of PVA water solution, carrying out ultrasonic treatment on the mixed solution for 1 hour, and carrying out suction filtration on a carrier to obtain the high-efficiency photo-thermal water evaporation film.
The preparation method of the PVA aqueous solution comprises the following steps: adding polyvinyl alcohol crystal and ultrapure water into a round-bottom flask, connecting the round-bottom flask with a condenser pipe, putting the round-bottom flask into an oil bath pan at 90-95 ℃, and heating for 3-4 h in the oil bath.
The carrier is an aqueous filtering membrane with the pore size of 200 nm.
An efficient photo-thermal water evaporating film for seawater evaporation features that a xenon lamp is used as the light source for simulating the sun, and the irradiance is 1000 W.m -2 The seawater is prepared artificial seawater.
The application of the efficient photothermal water evaporation film in degrading rhodamine B dye is characterized in that the irradiance of the adopted artificial light source is 600W/m 2 The concentration of the rhodamine B dye is 10 -5 mol/L。
The high-efficiency light and hot water evaporation film is a square with the side length of 2 cm.
The application of the porous efficient photothermal material in sterilization is characterized in that a strain is escherichia coli with an OD value of 0.018, and the irradiance of an artificial light source adopted is 600W/m 2 。
Compared with the prior art, the invention has the following beneficial effects:
the preparation method comprises the steps of firstly preparing the porous high-efficiency photothermal material by using a supermolecule self-assembly method, increasing the specific surface area of the material, loading copper phthalocyanine on graphite-phase carbon nitride in a sheet manner to form a type I semiconductor, adjusting an energy band structure, reducing a band gap, increasing the utilization rate of a solar spectrum, regulating and controlling the transition of a current carrier, and improving the photothermal performance; the preparation method has the advantages of simple preparation process, low cost, mild reaction conditions, realization of continuous preparation and wide application prospect.
The invention uses porous high-efficiency photo-thermal material in the sterilization field. Namely: in the process of sterilizing by utilizing the porous high-efficiency photothermal material, the survival rate of bacteria is 0 percent by 7.5 weight percent of the copper phthalocyanine doped material group, and the sterilizing effect is obvious.
The invention uses the high-efficiency photo-thermal water evaporation film in the field of interface evaporation. Namely: in the process of evaporating seawater by using the high-efficiency photothermal water evaporation film, the area of the square film is only 4cm 2 The evaporation rate was 1.71kg · m -2 ·h -1 The photo-thermal conversion efficiency is as high as 98.5%.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) cross-section of a high efficiency light hot water evaporation thin film prepared in application example 5 of the present invention.
Fig. 2 is a graph of (a) an ultraviolet-visible absorption spectrum (UV-VIS) and (b) a photoluminescence spectrum (PL) prepared by the application examples 1, 2, 3, 4.
Fig. 3 is a graph showing time profiles of evaporation of seawater prepared in application examples 5, 6, 7, and 8.
FIG. 4 is a bar graph showing the survival rate of E.coli prepared in application examples 1, 2, 3 and 4.
FIG. 5 is a graph showing the change in light absorption of degraded rhodamine B solutions prepared in application examples 5, 6, 7 and 8.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make those skilled in the art better understand the technical solutions of the present invention.
Reagents and instrumentation: all reagents used in the invention are analytically pure, and all the reagents are purchased and directly used without further treatment.
Application example 1
A preparation method of a porous high-efficiency photothermal material comprises the following steps:
(1) 5040mg melamine powder, 5160mg cyanuric acid powder and 765mg copper phthalocyanine powder are dissolved in 200ml deionized water and magnetically stirred at room temperature of 550r/min for 12h to obtain a precursor.
(2) And (2) centrifuging the precursor in the step (1), putting the precipitate into a plastic culture dish, coating the precipitate with a sealing film, pricking a plurality of small holes on the sealing film, and putting the precipitate into a freeze drying oven to be freeze-dried for 24 hours at the temperature of-49 ℃ to obtain a blue solid.
(3) And (3) grinding the blue solid in the step (2), placing the ground blue solid in a crucible of 50m, placing the crucible in a muffle furnace, raising the temperature to 550 ℃ at a heating rate of 10 ℃/min, and preserving the temperature for 4 hours to obtain the porous efficient photo-thermal material marked as CUPC-CN-7.5%.
Application example 2
A preparation method of a porous high-efficiency photothermal material is disclosed in application example 1, except that: 5040mg of melamine powder, 5160mg of cyanuric acid powder and 135mg of copper phthalocyanine powder were taken in step (1) and dissolved in 200ml of deionized water. The obtained porous high-efficiency photothermal material is marked as CUPC-CN-1.5%.
Application example 3
A preparation method of a porous high-efficiency photothermal material is disclosed in application example 1, except that: 5040mg of melamine powder, 5160mg of cyanuric acid powder and 76.5mg of copper phthalocyanine powder were taken in step (1) and dissolved in 200ml of deionized water. The obtained porous high-efficiency photothermal material is marked as CUPC-CN-0.75%.
Application example 4
A preparation method of a graphite phase carbon nitride material comprises the following steps:
(1) Dissolving 5040mg of melamine powder and 5160mg of cyanuric acid powder in 200ml of deionized water, and magnetically stirring at room temperature of 550r/min for 12h to obtain a precursor.
(2) And (2) centrifuging the precursor in the step (1), putting the precipitate into a plastic culture dish, coating the precipitate with a sealing film, pricking a plurality of small holes on the sealing film, and putting the precipitate into a freeze drying oven to be freeze-dried for 24 hours at the temperature of-49 ℃ to obtain a white solid.
(3) And (3) grinding the white solid in the step (2), placing the ground white solid in a 50ml crucible, placing the crucible in a muffle furnace, heating to 550 ℃ at the heating rate of 10 ℃/min, and preserving heat for 4h to obtain a graphite phase carbon nitride material sample labeled CN.
Application example 5
A preparation method of a high-efficiency photothermal water evaporation film comprises the following steps:
(1) 5040mg melamine powder, 5160mg cyanuric acid powder and 765mg copper phthalocyanine powder are dissolved in 200ml deionized water and magnetically stirred at room temperature of 550r/min for 12h to obtain a precursor.
(2) And (2) centrifuging the precursor in the step (1), putting the precipitate into a plastic culture dish, coating the precipitate with a sealing film, pricking a plurality of small holes on the sealing film, and putting the precipitate into a freeze drying oven to be freeze-dried for 24 hours at the temperature of-49 ℃ to obtain a blue solid.
(3) And (3) grinding the blue solid in the step (2), placing the ground blue solid in a 50ml crucible, placing the crucible in a muffle furnace, heating to 550 ℃ at the heating rate of 10 ℃/min, and preserving heat for 4 hours to obtain the porous efficient photo-thermal material.
(4) And (3) dissolving 20mg of the porous high-efficiency photothermal material in the step (3) in 40ml of PVA aqueous solution with the concentration of 0.2wt%, performing ultrasonic dispersion for 30min to obtain dispersion liquid, and performing suction filtration on the dispersion liquid to obtain a high-efficiency photothermal water evaporation Film sample with the pore diameter of 200nm, wherein the sample is marked as Film-7.5%.
Application example 6
A method for preparing a high-efficiency photothermal water evaporation film as described in application example 5, except that: 5040mg of melamine powder, 5160mg of cyanuric acid powder and 135mg of copper phthalocyanine powder in step (1) were dissolved in 200ml of deionized water. The obtained sample of the high-efficiency photothermal water evaporation Film is marked as Film-1.5%.
Application example 7
A method for preparing a high-efficiency photothermal water evaporation film as described in application example 5, except that: 5040mg of melamine powder, 5160mg of cyanuric acid powder and 76.5mg of copper phthalocyanine powder were taken in step (1) and dissolved in 200ml of deionized water. The obtained sample of the high-efficiency photothermal water evaporation Film is marked as Film-0.75 percent.
Application example 8
A preparation method of a graphite phase carbon nitride water evaporation film comprises the following steps:
the material 20mg CN of the application example 4 is dissolved in 40ml of PVA water solution with the concentration of 0.2wt%, ultrasonic dispersion is carried out for 30min to obtain dispersion liquid, and the dispersion liquid is filtered and filtered on a water-based filter membrane with the aperture of 200nm to obtain a graphite-phase carbon nitride water evaporation Film sample which is marked as Film-CN.
Comparative example 1
Using the prior art, yang Jin et al used MXene, polydopamine and melamine foams to make evaporation films (Journal of Colloid and Interface Science 614 (2022) 345-354).
Performance testing
The samples prepared in comparative examples 1 to 4 were tested for photothermal conversion efficiency while maintaining a constant sunlight, and the test results are shown in table 1.
TABLE 1
The seawater evaporation efficiency of each sample was tested while maintaining a constant sunlight, and the test results are shown in table 2.
TABLE 2
The samples prepared in comparative examples 1 to 4 were kept at a light intensity of 600W/m 2 Each sample was tested for E.coli survival without change, the results of which are shown in Table 3.
TABLE 3
The samples prepared in comparative examples 5 to 8 were kept at a light intensity of 600W/m 2 Under the condition of no change, the absorbance of the rhodamine B solution of each sample is tested, and the test result is shown in the table 4.
TABLE 4
The overall analysis was as follows:
the graphite phase carbon nitride is doped with copper phthalocyanine in different weight ratios (0.15 wt%, 1.5wt% and 7.5 wt%) to form a typical type I heterojunction, so that the transition of carriers is promoted, and the absorption of red light and infrared light regions is obviously enhanced. Meanwhile, the self-cleaning capability of graphite-phase carbon nitride is kept, and trace copper is generated by reduction, so that the antibacterial self-cleaning is facilitated. It can be found from application examples 1 to 4 that the photothermal conversion efficiency and the sterilization ability are optimal for the 7.5wt% doping concentration effect, and it can be found from application examples 5 to 8 that the evaporation rate and the carbon nitride degradation ability are optimal for the 7.5wt% doping concentration effect, and both are also superior to those of the prior art at the present stage.
FIG. 1 is a Transmission Electron Microscope (TEM) cross-section of a high efficiency light hot water evaporation thin film prepared in application example 5 of the present invention. It can be seen from the figure that application example 5 retains the porous structure of graphite phase carbon nitride, and finally has a three-dimensional sheet stacking structure.
Fig. 2 is a uv-vis absorption spectrum and a photoluminescence spectrum prepared in application examples 1, 2, 3, and 4. Compared with application example 4, application examples 1, 2 and 3 have almost full spectrum absorption, and are similar to application example 4 in ultraviolet to 460nm, and the light absorption at 600-1100nm is due to the Q absorption band of copper phthalocyanine material. In (b), the photoluminescence emission intensity of application examples 1, 2, and 3 was significantly reduced, and the fluorescence emission was red-shifted. These differences indicate that with the type i heterojunction semiconductors formed in examples 1, 2, and 3, electrons on the conduction band of graphite phase carbonitride transition to the conduction band of copper phthalocyanine, and holes on the valence band of graphite phase carbonitride transition to the valence band of copper phthalocyanine, resulting in non-radiative transitions, releasing heat.
Fig. 3 is a time curve of evaporation of seawater prepared in application examples 5, 6, 7, and 8. As can be seen from fig. 3, the amount of change in seawater prepared in application example 5 was the largest, 1.7 times as large as that prepared in comparative example 8. The reason is that the high-efficiency photo-thermal material prepared by the application example of the invention forms an I-type heterojunction, and can synergistically promote the transition of a photon-generated carrier.
FIG. 4 is a bar graph showing the survival rate of E.coli prepared in application examples 1, 2, 3 and 4. As can be seen from FIG. 4, the survival rate of E.coli prepared in application example 1 was 0%, which is different from that of comparative example 4 by 74.2%. The reason is that the high-efficiency photothermal material prepared by the application example of the invention forms trace copper, and can synergistically promote and kill escherichia coli.
FIG. 5 is a graph showing the change in light absorption of degraded rhodamine B solutions prepared in application examples 5, 6, 7, and 8. From fig. 3, it can be seen that the degradation capability of the film prepared by application example 8 is the best, and after copper phthalocyanine is doped, a typical type i heterojunction is formed, electron transfer is mostly used for generating non-radiative transition to release heat, electrons used for generating oxygen free radicals are reduced, the degradation capability of the material is reduced, but the degradation capability of graphite phase carbon nitride is retained, so that the prepared film has dual-effect films with good photo-thermal capability and certain self-cleaning capability.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. The porous high-efficiency photothermal material is a composite material of copper phthalocyanine and graphite-phase carbon nitride, and the copper phthalocyanine is loaded on the graphite-phase carbon nitride in a small lamellar mode.
2. The method for preparing the porous high-efficiency photothermal material according to claim 1, wherein copper phthalocyanine, melamine and cyanuric acid are used as raw materials, and the material is prepared by a thermal polycondensation method after a supermolecule self-assembly method is used in water;
the supermolecule self-assembly method specifically comprises the following steps: mixing copper phthalocyanine, melamine, cyanuric acid and ultrapure water, magnetically stirring for 10-12 h, centrifugally filtering, and freeze-drying at-49-41 ℃ for 20-24 h;
wherein the mol ratio of melamine, cyanuric acid to copper phthalocyanine is 1:1:0.033;
the thermal polycondensation method specifically comprises the following steps: grinding the substances obtained by the supermolecule self-loading method, and then polycondensing for 4h in a muffle furnace at 500-550 ℃, wherein the heating rate is 10 ℃/min.
3. The efficient photothermal water evaporation film is characterized by comprising a carrier and a porous efficient photothermal material on the surface of the carrier.
4. The method for preparing a high efficiency photothermal water evaporation film according to claim 3, wherein the porous high efficiency photothermal material is dispersed in a 0.2wt% aqueous solution of PVA, and the mixed solution is subjected to ultrasound for 1 hour and then is suction-filtered on the support to obtain the high efficiency photothermal water evaporation film.
5. The production method according to claim 6, wherein the carrier is an aqueous filtration membrane having a pore size of 200 nm.
6. Use of the high efficiency photothermal water evaporation membrane of claim 3 in seawater evaporation, said seawater being prepared as artificial seawater.
7. The use of the porous high-efficiency photothermal material as claimed in claim 1 in sterilization, wherein the bacterial species is Escherichia coli with OD of 0.018, and the irradiance of artificial light source is 600W/m 2 。
8. The application of the high-efficiency photothermal water evaporation film as claimed in claim 3 in degrading rhodamine B dye, wherein the irradiance of an artificial light source is 600W/m 2 The concentration of the rhodamine B dye is 10 -5 mol/L。
9. Use according to any of claims 6 to 8, wherein the high efficiency photothermal evaporation film is a square with a side length of 2 cm.
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