CN113042077A - Photo-thermal-photochemical cooperative conversion hydrogel material and preparation method and application thereof - Google Patents
Photo-thermal-photochemical cooperative conversion hydrogel material and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a photo-thermal-photochemical cooperative conversion hydrogel material and a preparation method and application thereof, and belongs to the technical field of photo-thermal and photochemical conversion. Interpenetration polymerization of photo-thermal photocatalyst with chitosan and polyvinyl alcoholCombining the substances to prepare a hydrogel material with the synergistic effect of photo-thermal degradation and photocatalytic degradation; the photo-thermal photocatalyst is MXene and La0.5Sr0.5CoO3Or La0.5Sr0.5CoO3-MXene. In the hydrogel, the photocatalyst can absorb short-wave photons in a solar spectrum to generate a photo-generated carrier, so that a photocatalytic degradation reaction is generated, and the photo-thermal material can convert long-wave photons in the solar spectrum into heat energy, so that water evaporation is efficiently performed, photochemical reaction kinetics are accelerated, photocatalytic degradation is promoted, and efficient water production is realized. The hydrogel material has simple preparation process and wide application prospect in the fields of sewage treatment, seawater desalination and the like.
Description
Technical Field
The invention belongs to the technical field of photothermal and photochemical conversion, and particularly relates to a photothermal-photochemical cooperative conversion hydrogel material, and a preparation method and application thereof.
Background
In recent years, solar energy is a renewable energy source with huge development potential due to abundant resources, sustainability and no pollution. At present, fresh water resources are increasingly in short supply in the global scope, and the technology of driving seawater desalination by solar energy is widely concerned by people. Therefore, the exploration of efficient solar energy conversion technologies and materials is crucial to the utilization of solar energy. The solar energy conversion approaches mainly include photochemical conversion and photothermal conversion. Photochemical conversion generates photon-generated carriers by capturing solar energy, and the photon-generated carriers and pollutant molecules have migration and degradation reactions, so that the photochemical conversion has great potential in the aspects of environmental pollution treatment, chemical production, fuel development and the like. However, the feasibility of the application of photochemical transformations is severely limited due to the limited absorption of uv-visible light and the slow transfer of photocharges.
Compared with photochemical conversion, photothermal conversion, which is a direct conversion path of solar energy, represents a significant advantage in the utilization of the full band of the solar spectrum. The photothermal material can absorb the infrared region in the solar spectrum to carry out efficient photothermal conversion, and the generated heat energy can be used for evaporating water and promoting photochemical conversion, so the photothermal material has application prospects in the aspects of seawater desalination, fuel catalytic production, environmental management and the like. Under the background, development of a photo-thermal synergistic photocatalytic material is urgently needed, so that the photo-thermal material provides kinetic energy for transmission of photo-generated carriers driven by ultraviolet-visible solar light while utilizing heat energy converted from visible light to near infrared region to generate steam, the photodegradation process is promoted, and efficient utilization of the full spectrum of the solar spectrum is realized.
Disclosure of Invention
In view of the problems in the prior art, one technical problem to be solved by the present invention is to provide a photothermal-photochemical cooperative conversion hydrogel material. The invention aims to solve another technical problem of providing a preparation method of a photo-thermal-photochemical cooperative conversion hydrogel material. The invention also aims to solve the technical problem of providing an application of the photo-thermal-photochemical cooperative conversion hydrogel material in efficient photo-thermal water evaporation and photocatalytic degradation of tetracycline pollutants. The material has outstanding full solar spectrum utilization rate, photo-thermal steam conversion and photo-degradation efficiency.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of hydrogel by photo-thermal-photochemical cooperative conversion comprises combining photo-thermal photocatalyst with interpenetrating network polymer of chitosan and polyvinyl alcohol to obtain hydrogel material degraded by photo-thermal cooperative photocatalysis; the photo-thermal photocatalyst is a two-dimensional MXene sheet and nano La0.5Sr0.5CoO3Particles and La0.5Sr0.5CoO3-MXene composite material. The method comprises the following steps:
(1) respectively preparing a polyvinyl alcohol aqueous solution, a chitosan aqueous solution, a glutaraldehyde solution and a hydrochloric acid solution;
(2) mixing the polyvinyl alcohol solution obtained in the step (1) with a chitosan solution to form a precursor solution;
(3) in N2Adding the photo-thermal photocatalytic mixed powder into the precursor solution under the atmosphere protection, and stirring at a low speed to uniformly mix the photo-thermal photocatalytic mixed powder; then, willSlowly dripping glutaraldehyde solution and hydrochloric acid solution into the precursor solution, mixing and stirring to generate gel reaction; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid when the sample is completely gelatinized;
(4) and (3) sucking water on the surface of the gel by using filter paper, freezing in a refrigerator, unfreezing in warm water, and repeating freezing-temperature returning operation for several times to obtain the hydrogel material.
The preparation method of the photo-thermal-photochemical cooperative conversion hydrogel comprises the following steps: adding polyvinyl alcohol with alcoholysis degree of 87.0-89.0% into hot deionized water according to the mass concentration of 10 wt%, heating in water bath at 100 ℃, and stirring at high speed until the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol solution.
The preparation method of the photo-thermal-photochemical cooperative conversion hydrogel comprises the following steps: adding polyvinyl alcohol into 2 wt% acetic acid solution according to the mass concentration of 5 wt%, and stirring at high speed until the polyvinyl alcohol is completely dissolved to obtain chitosan solution.
According to the preparation method of the photo-thermal-photochemical cooperative conversion hydrogel, the concentration of the hydrochloric acid solution is 1mol/L, and the mass concentration of the glutaraldehyde solution is 4%.
The preparation method of the photo-thermal-photochemical synergetic conversion hydrogel comprises the steps of mixing the polyvinyl alcohol solution, the chitosan solution and the photo-thermal photocatalytic powder according to the weight ratio of 4:1.4:0.018, and then adding 3.25 wt% of glutaraldehyde solution and 6.5 wt% of hydrochloric acid solution.
The photo-thermal-photochemical cooperative conversion hydrogel material prepared by the method.
The photo-thermal-photochemical cooperative conversion hydrogel material is applied to photo-thermal evaporation and purification of seawater, heavy metals, dyes and strong-acid-base wastewater.
The photo-thermal-photochemical synergetic conversion hydrogel material is applied to efficient water evaporation and synergetic photocatalytic degradation of tetracycline pollutants.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) the photo-thermal-photochemical cooperative conversion hydrogel has a structure of up to 92 under the standard sunlight irradiationPhotothermal conversion efficiency of 3% and 2.24kg m-2h-1The water evaporation rate of (2) has a high photo-degradation rate of 97% for tetracycline hydrochloride.
(2) The photo-thermal evaporation system formed by the hydrogel disclosed by the invention can have remarkable photo-thermal purification capability in saline water, heavy metals, dyes and strong-acid and alkaline wastewater.
(3) The hydrogel material has outstanding light evaporation rate and efficiency and light degradation efficiency, is simple in preparation process, and has wide application prospects in the fields of seawater desalination, sewage treatment and the like.
Drawings
FIG. 1 shows MXene/La of the present invention0.5Sr0.5CoO3Schematic diagram of embedded photo-thermal-photochemical cooperative conversion hydrogel material;
FIG. 2 shows MXene/La of the present invention (2a)0.5Sr0.5CoO3Transmission electron microscope images of (a); (2b) scanning electron microscope images of the MLH-2 hydrogel after freeze drying; (2c) la0.5Sr0.5CoO3LM-10, LM-20;
FIG. 3 is a graph showing the measurement of the saturated water content in various hydrogels according to the present invention (3 a); (3b) measuring the surface hydrophilicity of MLH-2 hydrogel; (3c) dynamic mechanical analysis of the storage modulus (G ') and loss modulus (G') of MLH-1 and MLH-2; (3d) elasticity test of MLH-1 and MLH-2;
FIG. 4 shows the absorption spectra of various hydrogels of the present invention (4a) in the wavelength range of 250-2500nm sunlight; (4b) water evaporation weight loss of different hydrogels under one sunlight illumination intensity; (4c) under the illumination intensity of sunlight, the water evaporation rate and the evaporation efficiency of different hydrogels are improved; (4d) under the irradiation of sunlight, carrying out a cycle stability test on the evaporation performance of MLH-2 in seawater;
FIG. 5 is a schematic view showing the purification of waste water by photothermal evaporation of hydrogel according to (5a) of the present invention; (5b) MLH-2 hydrogel photothermal evaporation dye wastewater (methyl orange MA and methylene blue MB) front and back solution ultraviolet visible absorption spectrograms; (5c) ion concentration changes in seawater and wastewater before and after MLH-2 hydrogel photothermal evaporation; (5d) the pH change of water measured before and after the MLH-2 hydrogel photothermal evaporation;
FIG. 6 shows the temperature change during photodegradation under non-circulating water and circulating water conditions according to the present invention (6 a); (6b) the photodegradation rate of the LM photocatalyst to tetracycline hydrochloride under the non-circulating water condition; (6c) the photodegradation rate of the LM photocatalyst to tetracycline hydrochloride under the circulating water condition; (6d) the research on the photodegradation reaction kinetics of the LM photocatalyst on tetracycline hydrochloride under the non-circulating water condition; (6e) the research on the photodegradation reaction kinetics of tetracycline hydrochloride by the LM photocatalyst under the circulating water condition; (6f) the degradation stability of the LM photocatalyst in the photochemical degradation process was studied 10 times.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A preparation method of hydrogel adopting photo-thermal-photochemical cooperative conversion comprises the following steps:
(1) weighing 10g of polyvinyl alcohol (PVA), pouring the PVA into a beaker, adding 90mL of hot deionized water, heating the PVA in a water bath at 100 ℃, and stirring the PVA at a high speed until the PVA is completely dissolved to obtain a 10 wt% polyvinyl alcohol solution;
(2) adding 2mL of acetic acid into 98mL of deionized water to form an acetic acid solution; 5g of Chitosan (CS) was weighed into a beaker, and 95mL of acetic acid solution was added and dissolved by high-speed stirring to obtain a 5 wt% chitosan solution.
(3) Mixing 4g of polyvinyl alcohol solution with 1.4g of chitosan solution to form a precursor solution;
(4) slowly dripping glutaraldehyde (195 mu L, 4 wt%) and HCl (400 mu L, 0.1 wt%) into the precursor solution in sequence, mixing and stirring to generate a gel reaction, and completely gelatinizing the sample within 6 h; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid; finally, the water on the gel surface was blotted with filter paper, frozen in a refrigerator (-24 ℃ C.), thawed in warm water (40 ℃ C.), and the freeze-thaw operation was repeated 10 times to obtain a hydrogel material (designated as MLH-1).
MLH-1 had better water absorption by the test of saturated water content (FIG. 3 a). MLH-1 has certain mechanical strength and elasticity by dynamic mechanical analysis (FIG. 3c) and elasticity test (FIG. 3 d).
The absorption rate of MLH-1 to light with the wavelength of 250-2500nm was 75.97% as determined by UV-visible near-IR absorption spectrum analysis (FIG. 4 a). Under the irradiation of standard sunlight, the evaporation rate of a photothermal evaporation system consisting of MLH-1 can reach 0.96kg m-2h-1(FIG. 4b), the photothermal conversion efficiency was 47.4% (FIG. 4c), which is significantly superior to the evaporation performance of pure water.
Example 2
A preparation method of hydrogel adopting photo-thermal-photochemical cooperative conversion comprises the following steps:
(1) weighing 0.5g Ti3AlC2(MAX) powder, soaking it in NH4F (2.96g) and HCl (20mL) mixed solution, heated to 60 ℃ in water bath, and stirred at low speed for 48 h; after the reaction is finished, centrifuging at the rotating speed of 3000rpm and washing with deionized water, and repeating for multiple times until the pH value of the upper layer solution is 6; performing ultrasonic treatment, taking supernatant, and freeze-drying for 12h to obtain MXene nanosheets;
(2) weighing 0.220g of MXene nanosheet, 1.083g of lanthanum nitrate hexahydrate, 0.532g of strontium nitrate hexahydrate, 1.455g of cobalt nitrate hexahydrate and 3.92g of KOH, pouring into a three-necked round bottom flask, adding 80mL of deionized water, and ultrasonically stirring for 2 hours; then, transferring the mixed solution to a hydrothermal reaction kettle (100mL), and putting the hydrothermal reaction kettle into an oven to perform solvothermal reaction for 48 hours at 180 ℃; subsequently, the solution was centrifuged at 8000rpm and washed with 75% ethanol and deionized water, and after repeating the operation 3 times, the precipitate was freeze-dried to obtain La0.5Sr0.5CoO3-MXene complex (denoted LM-10);
(3) weighing 10g of polyvinyl alcohol (PVA), pouring the PVA into a beaker, adding 90mL of hot deionized water, heating the PVA in a water bath at 100 ℃, and stirring the PVA at a high speed until the PVA is completely dissolved to obtain a 10 wt% polyvinyl alcohol solution;
(4) adding 2mL of acetic acid into 98mL of deionized water to form an acetic acid solution; weighing 5g of Chitosan (CS), pouring the Chitosan (CS) into a beaker, adding 95mL of acetic acid solution, and stirring at a high speed to dissolve the Chitosan (CS) to obtain 5 wt% of chitosan solution;
(5) mixing 4g of polyvinyl alcohol solution with 1.4g of chitosan solution to form a precursor solution;
(6) in N2Adding 18mg of LM-10 into the precursor solution under the protection of atmosphere, and stirring at low speed to uniformly mix the precursor solution; then, slowly dripping glutaraldehyde (195 mu L, 4 wt%) and HCl (400 mu L, 1mol/L) into the precursor solution in sequence, mixing and stirring to generate a gel reaction, and completely gelatinizing the sample within 6 h; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid; finally, the water on the gel surface was blotted with filter paper, frozen in a refrigerator (-24 ℃) and thawed in warm water (40 ℃), and the freeze-thaw operation was repeated 10 times to obtain a hydrogel material (designated as MLH-2) (FIG. 1).
As is evident from the transmission electron microscope image (FIG. 2a) and the X-ray diffraction pattern (FIG. 2c) of LM-10, La in LM-100.5Sr0.5CoO3Nanoparticles were successfully grown on MXene nanoplates. By scanning electron microscopy characterization of the hydrogel after freeze-drying treatment (FIG. 2b), a microporous framework of the MLH-2 surface was found.
MLH-2 exhibited excellent hydrophilicity as measured by saturated water content (FIG. 3a) and hydrogel surface contact angle (FIG. 3 b). Compared with MLH-1, MLH-2 has excellent mechanical strength and elasticity through dynamic mechanical analysis and elasticity test.
The ultraviolet visible near-infrared absorption spectrum analysis shows that MLH-1 has good absorption capacity to the spectrum with the wavelength of 250-2500nm, and the absorption rate is 94.13% (FIG. 4 a). Compared with other hydrogel systems, the photothermal evaporation system consisting of MLH-2 shows the most excellent photothermal evaporation characteristics under the irradiation of standard sunlight, and the evaporation rate can reach 2.73kg m- 2h-1(fig. 4b), the photothermal conversion efficiency was 92.3% (fig. 4 c).
Under the irradiation of a light source of a solar simulator with an AM1.5 optical filter, the model shown in figure 5a is used as a photo-thermal purification device, MLH-2 is used as a photo-thermal material, and seawater and wastewater containing heavy metals, dyes and strong acidity and alkalinity are subjected to photo-thermal evaporation and condensed water is collected. By inductively coupled plasma-mass spectrometry (ICP-MS)) The concentration, pH value and composition of each ion in the water before and after purification are tested by methods such as a pH meter, an ultraviolet-visible spectrum and the like, the purification effect is shown in figure 5, the characteristic absorption peaks of the dyes (methyl orange and methylene blue) in the purified water collected after photo-thermal evaporation treatment completely disappear, the pH value of the water is close to neutral, and Pb is2+，Cu2+，Zn2+，Na+The ion concentration meets the drinking water standard regulated by the world health organization.
And (3) carrying out a photocatalytic degradation test on the tetracycline by using an XPA system photochemical reactor. 40mg of LM-10 photocatalyst was added to a tetracycline solution (TC, 10mg/L, 40mL), stirred under dark field conditions for 60min to reach adsorption equilibrium, and then the reaction vessel was placed in a water tank surrounded by circulating water. Under the two conditions of circulating water and non-circulating water, the TC concentration is measured by using an ultraviolet-visible spectrophotometer every 30min, and the obtained photodegradation performance is shown in figure 6. Under the condition of non-circulating water, the temperature of a photodegradation environment is raised by heat generated by photo-heat, the photodegradation performance is obviously improved, the LM-10 presents the best photodegradation performance and excellent circulating stability, and the photodegradation rate can reach 97%.
Example 3
A preparation method of hydrogel adopting photo-thermal-photochemical cooperative conversion comprises the following steps:
(1) weighing 0.5g Ti3AlC2(MAX) powder, soaking it in NH4F (2.96g) and HCl (20mL) mixed solution, heated to 60 ℃ in water bath, and stirred at low speed for 48 h; after the reaction is finished, centrifuging at the rotating speed of 3000rpm and washing with deionized water, and repeating for multiple times until the pH value of the upper layer solution is 6; performing ultrasonic treatment, taking supernatant, and freeze-drying for 12h to obtain MXene nanosheets;
(2) weighing 0.110g of MXene nanosheet, 1.083g of lanthanum nitrate hexahydrate, 0.532g of strontium nitrate hexahydrate, 1.455g of cobalt nitrate hexahydrate and 3.92g of KOH, pouring into a three-necked round bottom flask, adding 80mL of deionized water, and ultrasonically stirring for 2 hours; then, transferring the mixed solution to a hydrothermal reaction kettle (100mL), and putting the hydrothermal reaction kettle into an oven to perform solvothermal reaction for 48 hours at 180 ℃; subsequently, the solution was centrifuged at 8000rpm and deionized with 75% ethanolWashing with water, repeating the operation for 3 times, freeze drying the precipitate to obtain La0.5Sr0.5CoO3-MXene complex (denoted LM-20);
(3) weighing 10g of polyvinyl alcohol (PVA), pouring the PVA into a beaker, adding 90mL of hot deionized water, heating the PVA in a water bath at 100 ℃, and stirring the PVA at a high speed until the PVA is completely dissolved to obtain a 10 wt% polyvinyl alcohol solution;
(4) adding 2mL of acetic acid into 98mL of deionized water to form an acetic acid solution; weighing 5g of Chitosan (CS), pouring the Chitosan (CS) into a beaker, adding 95mL of acetic acid solution, and stirring at a high speed to dissolve the Chitosan (CS) to obtain 5 wt% of chitosan solution;
(5) mixing 4g of polyvinyl alcohol solution with 1.4g of chitosan solution to form a precursor solution;
(6) in N2Adding 18mg of LM-20 into the precursor solution under the protection of atmosphere, and stirring at low speed to uniformly mix the precursor solution; then, slowly dripping glutaraldehyde (195 mu L, 4 wt%) and HCl (400 mu L, 0.1 wt%) into the precursor solution in sequence, mixing and stirring to generate a gel reaction, and completely gelatinizing the sample within 6 h; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid; finally, the water on the gel surface was blotted with filter paper, frozen in a refrigerator (-24 ℃ C.), thawed in warm water (40 ℃ C.), and the freeze-thaw operation was repeated 10 times to obtain a hydrogel material (designated as MLH-3) (FIG. 1).
As is evident from the transmission electron microscope image (FIG. 2a) and the X-ray diffraction pattern (FIG. 2c) of LM-20, La in LM-200.5Sr0.5CoO3Nanoparticles were successfully grown on MXene nanoplates.
MLH-2 exhibits better hydrophilicity by saturation of water content (FIG. 3 a).
The ultraviolet visible near-infrared absorption spectrum analysis shows that MLH-1 has good absorption capacity to the spectrum with the wavelength of 250-2500nm, and the absorption rate is 94.55% (FIG. 4 a). Under the irradiation of standard sunlight, the photothermal evaporation system consisting of MLH-3 shows good photothermal evaporation characteristics, and the evaporation rate can reach 2.59kg m-2h-1(fig. 4b), the photothermal conversion efficiency was 88.9% (fig. 4 c).
And (3) carrying out a photocatalytic degradation test on the tetracycline by using an XPA system photochemical reactor. 40mg of LM-20 photocatalyst was added to a tetracycline solution (TC, 10mg/L, 40mL), stirred under dark field conditions for 60min to reach adsorption equilibrium, and then the reaction vessel was placed in a water tank surrounded by circulating water. Under the two conditions of circulating water and non-circulating water, the TC concentration is measured by using an ultraviolet-visible spectrophotometer every 30min, and the obtained photodegradation performance is shown in figure 6. Under the condition of non-circulating water, the temperature of the photodegradation environment is raised by heat generated by photo-heat, the photodegradation performance of LM-20 is obviously improved, the LM-20 presents better photodegradation performance, and the photodegradation rate can reach 96%.
Example 4
A preparation method of hydrogel adopting photo-thermal-photochemical cooperative conversion comprises the following steps:
(1) weighing 0.5g Ti3AlC2(MAX) powder, soaking it in NH4F (2.96g) and HCl (20mL) mixed solution, heated to 60 ℃ in water bath, and stirred at low speed for 48 h; after the reaction is finished, centrifuging at the rotating speed of 3000rpm and washing with deionized water, and repeating for multiple times until the pH value of the upper layer solution is 6; performing ultrasonic treatment, taking supernatant, and freeze-drying for 12h to obtain MXene nanosheets;
(2) weighing 10g of polyvinyl alcohol (PVA), pouring the PVA into a beaker, adding 90mL of hot deionized water, heating the PVA in a water bath at 100 ℃, and stirring the PVA at a high speed until the PVA is completely dissolved to obtain a 10 wt% polyvinyl alcohol solution;
(3) adding 2mL of acetic acid into 98mL of deionized water to form an acetic acid solution; weighing 5g of Chitosan (CS), pouring the Chitosan (CS) into a beaker, adding 95mL of glacial acetic acid solution, and stirring at a high speed to dissolve the Chitosan (CS) to obtain 5 wt% of chitosan solution;
(4) mixing 4g of polyvinyl alcohol solution with 1.4g of chitosan solution to form a precursor solution;
(5) in N2Under the protection of atmosphere, adding 18mg of MXene into the precursor solution, and stirring at a low speed to uniformly mix the MXene and the precursor solution; then, slowly dripping glutaraldehyde (195 mu L, 4 wt%) and HCl (400 mu L, 0.1 wt%) into the precursor solution in sequence, mixing and stirring to generate a gel reaction, and completely gelatinizing the sample within 6 h; removing the obtained gelRepeatedly soaking in ionized water to remove hydrochloric acid; finally, the water on the gel surface was blotted dry with filter paper, frozen in a refrigerator (-24 ℃) and thawed in warm water (40 ℃), and the freeze-thaw operation was repeated 10 times to obtain a hydrogel material (designated as MH-MXene) (FIG. 1).
MH-MXene exhibited better hydrophilicity by saturated water content (FIG. 3 a).
The ultraviolet visible near-infrared absorption spectrum analysis shows that MH-MXene has better absorption capacity to the spectrum with the wavelength of 250-2500nm, and the absorption rate is 93.54 percent (figure 4 a). Under the irradiation of standard sunlight, a photothermal evaporation system consisting of MH-MXene shows good photothermal evaporation characteristics, and the evaporation rate can reach 2.26kg m-2h-1(fig. 4b), the photothermal conversion efficiency was 81.9% (fig. 4 c).
And (3) carrying out a photocatalytic degradation test on the tetracycline by using an XPA system photochemical reactor. 40mg of MXene photocatalyst was added to a tetracycline solution (TC, 10mg/L, 40mL), stirred under dark field conditions for 60min to reach adsorption equilibrium, and then the reaction vessel was placed in a water tank surrounded by circulating water. Under the two conditions of circulating water and non-circulating water, the TC concentration is measured by using an ultraviolet-visible spectrophotometer every 30min, and the obtained photodegradation performance is shown in figure 6. Under the condition of non-circulating water, the temperature of a photodegradation environment is raised by heat generated by photo-heat, the MXene photodegradation performance is obviously improved, the LM-20 presents poorer photodegradation performance, and the photodegradation rate can only reach 64%.
Example 5
A preparation method of hydrogel adopting photo-thermal-photochemical cooperative conversion comprises the following steps:
(1) weighing 1.083g of lanthanum nitrate hexahydrate, 0.532g of strontium nitrate hexahydrate, 1.455g of cobalt nitrate hexahydrate and 3.92g of KOH, pouring the weighed materials into a three-neck round-bottom flask, adding 80mL of deionized water, and ultrasonically stirring for 2 hours; then, transferring the mixed solution to a hydrothermal reaction kettle (100mL), and putting the hydrothermal reaction kettle into an oven to perform solvothermal reaction for 48 hours at 180 ℃; subsequently, the solution was centrifuged at 8000rpm and washed with 75% ethanol and deionized water, and after repeating the operation 3 times, the precipitate was freeze-dried to obtain La0.5Sr0.5CoO3Nanoparticles;
(2) weighing 10g of polyvinyl alcohol (PVA), pouring the PVA into a beaker, adding 90mL of hot deionized water, heating the PVA in a water bath at 100 ℃, and stirring the PVA at a high speed until the PVA is completely dissolved to obtain a 10 wt% polyvinyl alcohol solution;
(3) adding 2mL of acetic acid into 98mL of deionized water to form an acetic acid solution; weighing 5g of Chitosan (CS), pouring the Chitosan (CS) into a beaker, adding 95mL of glacial acetic acid solution, and stirring at a high speed to dissolve the Chitosan (CS) to obtain 5 wt% of chitosan solution;
(4) mixing 4g of polyvinyl alcohol solution with 1.4g of chitosan solution to form a precursor solution; in N2Under the protection of atmosphere, 18mg of La is added0.5Sr0.5CoO3Adding the mixture into the precursor solution, and stirring at a low speed to uniformly mix the mixture; then, glutaraldehyde (195. mu.L, 4 wt%) and HCl (400. mu.L, 0.1 wt%) were slowly dropped into the above solution in this order, mixed and stirred to cause a gel reaction, and the sample was completely gelled within 6 hours; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid; finally, the water on the gel surface was blotted with filter paper, frozen in a refrigerator (-24 ℃) and thawed in warm water (40 ℃), and the freeze-thaw operation was repeated 10 times to obtain a hydrogel material (designated as LH-LSC) (FIG. 1).
LH-LSC exhibits better hydrophilicity by saturation with water content (FIG. 3 a).
The ultraviolet-visible near-infrared absorption spectrum analysis shows that the LH-LSC has excellent absorption capacity to the spectrum with the wavelength of 250-2500nm, and the absorption rate is 94.70% (FIG. 4 a). Under the irradiation of standard sunlight, a photothermal evaporation system consisting of LH-LSC shows good photothermal evaporation characteristics, and the evaporation rate can reach 2.24kg m-2h-1(fig. 4b), the photothermal conversion efficiency was 81.2% (fig. 4 c).
And (3) carrying out a photocatalytic degradation test on the tetracycline by using an XPA system photochemical reactor. 40mg of the LSC photocatalyst was added to a tetracycline solution (TC, 10mg/L, 40mL), stirred under dark field conditions for 60min to reach adsorption equilibrium, and then the reaction vessel was placed in a water tank surrounded by circulating water. Under the two conditions of circulating water and non-circulating water, the TC concentration is measured by using an ultraviolet-visible spectrophotometer every 30min, and the obtained photodegradation performance is shown in figure 6. Under the condition of non-circulating water, the temperature of the photodegradation environment is raised by heat generated by photo-heat, the photodegradation performance of the LSC is obviously improved, the LSC presents better photodegradation performance, and the photodegradation rate can reach 91%.
Claims (9)
1. A preparation method of hydrogel by photo-thermal-photochemical cooperative conversion is characterized in that a photo-thermal photocatalyst and interpenetrating network polymers of chitosan and polyvinyl alcohol are mutually combined to prepare a photo-thermal cooperative photocatalytic degradation hydrogel material; the photo-thermal photocatalyst is a two-dimensional MXene sheet and nano La0.5Sr0.5CoO3Particles and La0.5Sr0.5CoO3-MXene composite material.
2. The method for preparing photo-thermal-photochemical cooperative conversion hydrogel according to claim 1, comprising the steps of:
(1) respectively preparing a polyvinyl alcohol aqueous solution, a chitosan aqueous solution, a glutaraldehyde solution and a hydrochloric acid solution;
(2) mixing the polyvinyl alcohol solution obtained in the step (1) with a chitosan solution to form a precursor solution;
(3) in N2Adding the photo-thermal photocatalyst into the precursor solution under the protection of atmosphere, and stirring at low speed to uniformly mix the photo-thermal photocatalyst and the precursor solution; then, slowly dripping a glutaraldehyde solution and a hydrochloric acid solution into the precursor solution, mixing and stirring to generate a gel reaction; repeatedly soaking the obtained gel in deionized water to remove hydrochloric acid when the sample is completely gelatinized;
(4) and (3) sucking water on the surface of the gel by using filter paper, freezing in a refrigerator, unfreezing in warm water, and repeating freezing-temperature returning operation for several times to obtain the hydrogel material.
3. The method for preparing photo-thermal-photochemical cooperative conversion hydrogel according to claim 2, wherein the polyvinyl alcohol solution is: adding polyvinyl alcohol with alcoholysis degree of 87.0-89.0% into hot deionized water according to the mass concentration of 10 wt%, heating in water bath at 100 ℃, and stirring at high speed until the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol solution.
4. The method for preparing a photothermal-photochemical interconversion hydrogel according to claim 2, wherein polyvinyl alcohol is added to a 2 wt% acetic acid solution at a mass concentration of 5 wt%, and stirred at a high speed until completely dissolved, to obtain a chitosan solution.
5. The method for preparing a photothermal-photochemical cooperative conversion hydrogel according to claim 2, wherein the concentration of the hydrochloric acid solution is 1mol/L, and the mass concentration of the glutaraldehyde solution is 4%.
6. The method for preparing the photo-thermal-photochemical cooperative conversion hydrogel according to claim 2, wherein the polyvinyl alcohol solution, the chitosan solution and the photo-thermal photocatalytic powder are mixed in a weight ratio of 4:1.4:0.018, and then 3.25 wt% of glutaraldehyde solution and 6.5 wt% of hydrochloric acid solution are added.
7. The photo-thermal-photochemical cooperative conversion hydrogel material prepared by the method of any one of claims 1 to 6.
8. The photo-thermal-photochemical cooperative conversion hydrogel material as claimed in claim 7, which is used for photo-thermal evaporation purification of seawater, heavy metals, dyes and strongly acidic and alkaline wastewater.
9. Use of the photo-thermal-photochemical co-conversion hydrogel material of claim 7 for efficient photocatalytic degradation of tetracycline contaminants.
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