CN113401976B - Preparation method of hybrid graphene magnetic catalytic particle electrode for three-dimensional electro-Fenton degradation of arbidol in water - Google Patents
Preparation method of hybrid graphene magnetic catalytic particle electrode for three-dimensional electro-Fenton degradation of arbidol in water Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a hybrid graphene magnetic catalytic particle electrode for three-dimensional electro-Fenton degradation of arbidol in water3O4The layered structure of the montmorillonite is further opened, and the adsorption sites and the specific surface area of the catalytic particle electrode are increased, so that the adsorption capacity and the catalytic capacity of the catalytic particle electrode and the degradation effect of the three-dimensional electro-Fenton technology are improved.
Description
Technical Field
The invention relates to a preparation method of a hybrid graphene magnetic catalytic particle electrode for three-dimensional electro-Fenton degradation of arbidol in water.
Background
Arbidol has good effect on treating virus infection, but has the main defects that the arbidol can be used in large dose to achieve the treatment effect and has low bioavailability, and nearly 40 percent of ARB is discharged with human excrement and enters into the environmental water body. The excessive amount and long-time exposure of the antiviral drugs in the water environment easily cause the mutation of aquatic animals, induce the viruses to generate drug resistance, and seriously threaten the water environment safety.
At present, no relevant literature report on degradation methods of ARB in water is found. The method for removing the medicines in the water mainly comprises a biological treatment method, a physical and chemical method and an advanced oxidation method. Since drugs are generally difficult to biodegrade, biological treatment is not ideal for drug removal. The main techniques for treating the drugs by the physical and chemical methods comprise adsorption and membrane separation techniques, which have good removal effect on the drugs, but waste adsorbents and wastewater generated in the treatment process bring secondary pollution to the environment and increase the treatment cost. The advanced oxidation method is an effective method for degrading the medicines in water, common technologies comprise Fenton, ozone, photocatalysis technology and the like, but the advanced oxidation method also has the problems of high chemical consumption, low removal rate of medicines with high stability, low catalyst recycling rate and the like. The three-dimensional electro-Fenton technology introduces the particle electrode into a traditional electro-Fenton reaction system, increases the reaction area and mass transfer, and thus improves the degradation efficiency. However, the particle electrodes in three-dimensional electro-fenton are insufficient in stability, recyclability, corrosion resistance, and the like, and the processing effect of the three-dimensional electro-fenton technique is affected.
Disclosure of Invention
The invention aims to provide a preparation method and application of a hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water.
The invention is realized by the following technical scheme:
a preparation method of a hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water comprises the following steps:
step S1, weighing montmorillonite (MMT) and sucrose, wherein the mass ratio of the montmorillonite to the sucrose is 3: (8-12), adding ethylene glycol, and performing ultrasonic treatment to form a white and uniform suspension;
step S2, FeCl is weighed3•6H2O, anhydrous sodium acetate, polyethylene glycol, FeCl3•6H2The mass ratio of the O, the anhydrous sodium acetate and the polyethylene glycol is 1: (3.5-4.0): (1.5-2.5), adding ethylene glycol for simple mixing, then adding into the suspension obtained in the step S1, stirring, putting the uniformly stirred solution into a polytetrafluoroethylene high-pressure reaction kettle for heating at the temperature of 180-220 ℃ for 7.5-8.5 hours, mixing the obtained black solid with ethanol, centrifugally removing the supernatant to obtain a black solid, washing the black solid with ethanol for multiple times, drying in a vacuum drying oven at the temperature of 45-55 ℃ for 2-4 hours, grinding by using a mortar, and sieving by using a sieve of 80-120 meshes to obtain black powder;
step S3, mixing the black powder with 4 wt% of polyvinyl alcohol aqueous solution, wherein the mass ratio of the black powder to the 4 wt% of polyvinyl alcohol aqueous solution is (2.5-3.5): 1, extruding a long strip with the diameter of 5-7 mm by using a strip extruder, placing the long strip on a pill rolling plate for granulation to obtain circular particles with the diameter of 5-7 mm, freeze-drying, and carrying out N2Calcining at 750-850 ℃ for 100-150 min under a protective atmosphere to finally obtain a hybrid graphene magnetic catalytic particle electrode MMT/GH/Fe with the diameter of 4-6 mm3O4。
In the step S1, the volume of the added glycol is 25-35 ml, and the ultrasonic time is 50-70 min.
In step S2, the volume of the added glycol is 15-25 ml, and the stirring time is 55-65 min.
In step S2, the black solid is mixed with 2 to 4 times by volume of ethanol, and the number of times of washing the black solid with ethanol after the supernatant is removed by centrifugation is 2 to 4.
In the three-dimensional electro-Fenton degradation, the method for degrading arbidol in water by using the hybridized graphene magnetic catalytic particle electrode comprises the following steps:
adding an aqueous solution containing arbidol into a three-dimensional electro-Fenton reactor based on a hybrid graphene magnetic catalytic particle electrode, starting aeration and applying voltage,carrying out electrocatalytic advanced oxidation reaction. The concentration of arbidol is 15-25 mg/L, the adding amount of a hybridized graphene magnetic catalytic particle electrode is 5-45 g/L, the electrode plate distance of the three-dimensional electro-Fenton reactor is 2-6 cm, the initial pH value of the three-dimensional electro-Fenton electrolytic cell is 3-11, and the electrolyte of the three-dimensional electro-Fenton reaction cell is 0.005-0.08 mol/L Na2SO4The applied voltage of the solution is 5-30V, and the aeration intensity is 0.4-12L/min.
The invention has the following beneficial effects:
1. the invention is simple and easy to implement; montmorillonite is used as a carrier, sucrose is used as a carbon source, the method is economic and environment-friendly, and the catalytic particle electrode is hybridized with graphene and Fe by loading3O4The layered structure of the montmorillonite is further opened, and the adsorption sites and the specific surface area of the catalytic particle electrode are increased, so that the adsorption capacity and the catalytic capacity of the catalytic particle electrode and the degradation effect of the three-dimensional electro-Fenton technology are improved.
2. The hybrid graphene magnetic catalytic particle electrode is easy to recover due to magnetism, high in stability and reusable. After 10 times of recycling, the degradation rate of the three-dimensional electro-Fenton technology to arbidol can still reach more than 95%.
3. In the three-dimensional electro-Fenton degradation, the hybrid graphene magnetic catalytic particle electrode degrades arbidol in water, the reaction is rapid, the degradation efficiency is high, the removal rate of arbidol in 2 min reaches 87%, the arbidol is completely removed in 10 min, and the arbidol is preferably completely removed by degradation for 10-20 min.
4. Use of the hybrid graphene magnetic catalytic particle electrodes in comparison to GACs and Al in three-dimensional electro-fenton degradation2O3The particle electrode has better effect of removing arbidol in water: the hybrid graphene magnetic catalytic particle electrode can be used for completely removing target pollutants, the removal rate of the GACs particle electrode is 98%, and Al is used2O3The particle electrode removal rate was 92%.
Drawings
FIG. 1 shows the magnetic MMT/GH/Fe obtained in example 13O4Particle electrodeScanning Electron Microscope (SEM) images;
FIG. 2 shows the effect of hybrid graphene magnetic catalytic particle electrode on arbidol degradation in three-dimensional electro-Fenton as in example 1;
FIG. 3 shows the effect of three-dimensional electro-Fenton on arbidol degradation under different particle electrodes.
Detailed Description
The following is a further description of the invention and is not intended to be limiting.
Example 1:
the method comprises the steps of taking montmorillonite as a hard template and sucrose as a precursor, and preparing the hybrid graphene magnetic catalytic particle electrode through hydrothermal and high-temperature calcination.
0.3 g of montmorillonite and 1.0 g of sucrose are weighed in a beaker, 30 ml of ethylene glycol is added, and ultrasonic treatment is carried out for 60 min to form white uniform suspension. 1.0 g FeCl was weighed3•6H2O, 3.6 g of anhydrous sodium acetate and 2.0 g of polyethylene glycol are put into a beaker, 20 ml of ethylene glycol is added for simple mixing, then the mixture is added into the suspension, magnetons are added, and the mixture is stirred for 60 min on a magnetic stirrer. And (3) putting the uniformly stirred solution into a polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 8h, mixing the obtained black substance with ethanol with the volume being three times that of the black substance, washing the black solid obtained after centrifuging to remove the supernatant with ethanol for 3 times, drying in a vacuum drying oven at 50 ℃ for about 3 hours, grinding by using a mortar, and sieving by using a 100-mesh sieve to obtain black powder. Mixing black powder and 4 wt% of polyvinyl alcohol aqueous solution according to a mass ratio of 3:1, extruding a long strip with the diameter of 6 mm by using a strip extruder, and placing the long strip on a pill rolling plate for granulation to obtain round granules with the diameter of about 6 mm; freeze drying round particles and adding N2Calcining at 800 ℃ for 120 min under the protective atmosphere to finally obtain the MMT/GH/Fe with the diameter of about 5 mm3O4Magnetic particle electrodes.
100 mL of 20 mg/L arbidol solution is added into a reaction vessel, the distance between electrode plates is 6 cm, and electrolyte Na is added2SO4The adding amount is 0.02 mol/L, the aeration intensity is 2L/min, the applied voltage is 10V, the original pH value of the reaction tank is kept at 6.3, the normal illumination is realized, and the hybridized grapheneThe dosage of the magnetic catalytic particle electrode is 10 g/L, and the degradation time is 15 min. After the reaction is finished, the degradation rate of the arbidol is 97 percent by adopting high performance liquid chromatography for detection.
Comparative example 1:
the method comprises the steps of taking montmorillonite as a hard template and sucrose as a precursor, and preparing the hybrid graphene magnetic catalytic particle electrode through hydrothermal and high-temperature calcination. 0.3 g of montmorillonite and 1.0 g of sucrose are weighed in a beaker, 30 ml of ethylene glycol is added, and ultrasonic treatment is carried out for 60 min to form white uniform suspension. 1.0 g FeCl was weighed3•6H2O, 3.6 g of anhydrous sodium acetate and 2.0 g of polyethylene glycol are put into a beaker, 20 ml of ethylene glycol is added for simple mixing, then the mixture is added into the suspension, magnetons are added, and the mixture is stirred for 60 min on a magnetic stirrer. And (3) putting the uniformly stirred solution into a polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 8h, mixing the obtained black substance with ethanol with the volume being three times that of the black substance, washing the black solid obtained after centrifuging to remove the supernatant with ethanol for 3 times, drying in a vacuum drying oven at 50 ℃ for about 3 hours, grinding by using a mortar, and sieving by using a 100-mesh sieve to obtain black powder. Mixing black powder and 4 wt% of polyvinyl alcohol aqueous solution according to a mass ratio of 3:1, extruding a long strip with the diameter of 6 mm by using a strip extruder, and placing the long strip on a pill rolling plate for granulation to obtain round granules with the diameter of about 6 mm; freeze drying round particles and adding N2Calcining at 600 ℃ for 120 min under the protective atmosphere to finally obtain the MMT/GH/Fe with the diameter of about 5 mm3O4Magnetic particle electrodes, but the resulting particle electrodes are not strong enough after the reaction is complete, about half of the particle electrodes are broken.
100 mL of 20 mg/L arbidol solution is added into a reaction vessel, the distance between electrode plates is 6 cm, and electrolyte Na is added2SO4The adding amount is 0.02 mol/L, the aeration intensity is 2L/min, the applied voltage is 10V, the original pH of the reaction tank is kept at 6.3 and normal illumination is kept, the adding amount of the hybrid graphene magnetic catalytic particle electrode is 10 g/L, and the degradation time is 15 min. After the reaction is finished, high performance liquid chromatography is adopted for detection, and the degradation rate of arbidol is 94%.
Comparative example 2
The method comprises the steps of taking montmorillonite as a hard template and sucrose as a precursor, and preparing the hybrid graphene magnetic catalytic particle electrode through hydrothermal and high-temperature calcination. 0.3 g of montmorillonite and 1.0 g of sucrose are weighed in a beaker, 30 ml of high-purity water is added, and ultrasonic treatment is carried out for 60 min to form white uniform suspension. 1.0 g FeCl was weighed3•6H2O, 3.6 g of anhydrous sodium acetate and 2.0 g of polyethylene glycol are put into a beaker, 20 ml of high-purity water is added for simple mixing, then the mixture is added into the suspension, magnetons are added, and the mixture is stirred for 60 min on a magnetic stirrer. And (3) putting the uniformly stirred solution into a polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 8h, mixing the obtained black substance with ethanol with the volume being three times that of the black substance, washing the black solid obtained after centrifuging to remove the supernatant with ethanol for 3 times, drying in a vacuum drying oven at 50 ℃ for about 3 hours, grinding by using a mortar, and sieving by using a 100-mesh sieve to obtain black powder. Mixing black powder and 4 wt% of polyvinyl alcohol aqueous solution according to a mass ratio of 3:1, extruding a long strip with the diameter of 6 mm by using a strip extruder, and placing the long strip on a pill rolling plate for granulation to obtain round granules with the diameter of about 6 mm; freeze drying round particles and adding N2Calcining at 800 ℃ for 120 min under the protective atmosphere to finally obtain the MMT/GH/Fe with the diameter of about 5 mm3O4Magnetic particle electrodes, but the resulting particle electrodes are not strong enough after the reaction is complete, about half of the particle electrodes are broken.
100 mL of 20 mg/L arbidol solution is added into a reaction vessel, the distance between electrode plates is 6 cm, and electrolyte Na is added2SO4The adding amount is 0.02 mol/L, the aeration intensity is 2L/min, the applied voltage is 10V, the original pH and normal illumination of the reaction tank are kept, the adding amount of the hybrid graphene magnetic catalytic particle electrode is 10 g/L, and the degradation time is 15 min. After the reaction is finished, the degradation rate of the arbidol is 64 percent by adopting high performance liquid chromatography for detection.
Example 2
Referring to example 1, other parameters are unchanged, the dosage of the electrode of the hybrid graphene magnetic catalytic particle is 40 g/L, and after the reaction is finished, the degradation rate of arbidol is 100% by adopting high performance liquid chromatography for detection.
Example 3
Referring to example 1, other parameters are unchanged, the dosage of the electrode of the hybrid graphene magnetic catalytic particle is 20 g/L, and after the reaction is finished, the degradation rate of arbidol is 97% by adopting high performance liquid chromatography for detection.
Comparative example 3
With reference to example 1, the other parameters were unchanged, except that Al was used2O3The dosage of the particle electrode is 40 g/L, and the degradation rate of the arbidol is 92 percent by adopting high performance liquid chromatography for detection after the reaction is finished.
Comparative example 4
Referring to example 1, other parameters were unchanged except that GACs were used as particle electrodes in an amount of 40 g/L, and after the reaction was completed, degradation rate of arbidol was 98% as measured by high performance liquid chromatography.
Example 4
Referring to example 1, the other parameters were unchanged except that the degradation time was 4 min, and after the reaction was completed, the degradation rate of arbidol was 90% as measured by high performance liquid chromatography.
The embodiment and the comparative example show that in three-dimensional electro-Fenton degradation, the hybrid graphene magnetic catalytic particle electrode has a good effect of removing arbidol in water, and is rapid in reaction and high in degradation efficiency.
Claims (5)
1. A preparation method of a hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water is characterized by comprising the following steps:
step S1, weighing montmorillonite and sucrose, wherein the mass ratio of montmorillonite to sucrose is 3: (8-12), adding ethylene glycol, and performing ultrasonic treatment to form a white and uniform suspension;
step S2, FeCl is weighed3•6H2O, anhydrous sodium acetate, polyethylene glycol, FeCl3•6H2The mass ratio of the O, the anhydrous sodium acetate and the polyethylene glycol is 1: (3.5-4.0): (1.5-2.5), adding ethylene glycol for simple mixing,adding the suspension obtained in the step S1, stirring, heating the uniformly stirred solution in a polytetrafluoroethylene high-pressure reaction kettle at the heating temperature of 180-220 ℃ for 7.5-8.5 h, mixing the obtained black solid with ethanol, centrifugally removing supernatant to obtain black solid, washing the black solid for multiple times with ethanol, drying the black solid in a vacuum drying oven at the temperature of 45-55 ℃ for 2-4 h, grinding the mixture by using a mortar, and sieving the mixture by using a sieve of 80-120 meshes to obtain black powder;
step S3, mixing the black powder with 4 wt% of polyvinyl alcohol aqueous solution, wherein the mass ratio of the black powder to the 4 wt% of polyvinyl alcohol aqueous solution is (2.5-3.5): 1, extruding a long strip with the diameter of 5-7 mm by using a strip extruder, placing the long strip on a pill rolling plate for granulation to obtain circular particles with the diameter of 5-7 mm, freeze-drying, and carrying out N2Calcining at 750-850 ℃ for 100-150 min under a protective atmosphere to finally obtain the hybridized graphene magnetic catalytic particle electrode with the diameter of 4-6 mm.
2. The preparation method of the hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water according to claim 1, wherein in step S1, the volume of the added glycol is 25-35 ml, and the ultrasonic time is 50-70 min.
3. The preparation method of the hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water according to claim 1, wherein in step S2, the volume of the added glycol is 15-25 ml, and the stirring time is 55-65 min.
4. The preparation method of the hybrid graphene magnetic catalytic particle electrode for arbidol in three-dimensional electro-Fenton degradation water according to claim 1, wherein in step S2, the black solid is mixed with 2-4 times of ethanol, and the number of times of washing the black solid with ethanol after the supernatant is removed by centrifugation is 2-4.
5. The application of the hybrid graphene magnetic catalytic particle electrode obtained by the preparation method of any one of claims 1 to 4, which is characterized in thatIn the three-dimensional electro-Fenton degradation, the hybrid graphene magnetic catalytic particle electrode is used for degrading arbidol in water, and the method comprises the following steps: adding an aqueous solution containing arbidol into a three-dimensional electro-Fenton reactor based on a hybrid graphene magnetic catalytic particle electrode, starting aeration and applying voltage to perform electro-catalytic advanced oxidation reaction, wherein the concentration of arbidol is 15-25 mg/L, the adding amount of the hybrid graphene magnetic catalytic particle electrode is 5-45 g/L, the electrode plate spacing of the three-dimensional electro-Fenton reactor is 2-6 cm, the initial pH value of a three-dimensional electro-Fenton electrolytic cell is 3-11, and the electrolyte of the three-dimensional electro-Fenton reaction cell is 0.005-0.08 mol/L Na2SO4The applied voltage of the solution is 5-30V, and the aeration intensity is 0.4-12L/min.
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| 核壳式磁性碳纳米吸附剂的制备及其对水环境中金霉素的吸附研究;王懿萱;《环境科学》;20120415;第33卷(第4期);第1234-1240页 * |
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