CN114314771B - Activated blue algae biochar cathode material and application thereof in degradation of antibiotics - Google Patents
Activated blue algae biochar cathode material and application thereof in degradation of antibiotics Download PDFInfo
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Abstract
The invention discloses an activated blue algae biochar cathode material and application thereof in degradation of antibiotics, and belongs to the technical field of preparation of electro-Fenton cathode materials. The electrode modification material is obtained after activated biochar is activated, and the activated biochar, polyvinylidene fluoride and N, N-dimethylformamide are mixed and coated on a substrate to obtain the activated blue algae biochar electrode material. The active blue algae biochar electrode material prepared by the invention has good capability of producing hydrogen peroxide by electrocatalytic oxygen reduction, can effectively treat various antibiotics at the same time, and has high practicability and good applicability. The electrode material has good stability, can keep the structural integrity and good treatment effect after being used in batches, and can be reused.
Description
Technical Field
The invention relates to an activated blue algae biochar cathode material and application thereof in degradation of antibiotics, belonging to the technical field of preparation of electro-Fenton cathode materials.
Background
With the rise of health consciousness and the development of pharmaceutical technology, more and more antibiotics are applied to the treatment of diseases, and at the same time, new global problems, namely misuse and abuse of antibiotics, are generated. A large number of antibiotics are used in livestock breeding and human medicine, with serious problems of antibiotic contamination. The most part of the overused antibiotics are discharged into the water body along with the domestic wastewater, and the other part of the overused antibiotics are diffused into the environment through the forms of excrement and chemical fertilizers.
Antibiotics are macromolecular organic compounds which can inhibit the growth of microorganisms or directly kill microorganisms, but can induce the generation of drug resistance genes, and misuse and abuse of the antibiotics greatly improve the probability of the generation of the genes, so that drug resistant bacteria (ARB) and drug resistant genes (ARGs) are rapidly appeared, and the difficulty of drug treatment is increased by the drug resistant bacteria.
At present, most of the processes used by domestic sewage treatment plants are physicochemical serial biochemical treatment, and antibiotics can inhibit the activity of microorganisms in biochemical stages such as anaerobic and aerobic processes, and even kill the microorganisms in the biochemical stages, so that the degradation effect of the biochemical processes on the antibiotics is limited; however, although the coagulating sedimentation which is commonly used in the physical and chemical means can separate the antibiotics from the water body, the antibiotics cannot be degraded, and the sludge treatment containing the antibiotics becomes a derivative problem.
Fenton technology belongs to Advanced Oxidation (AOP) technology, can be used for treating organic wastewater which is difficult to biodegrade, such as antibiotic wastewater, as an advanced treatment technology, but the traditional Fenton technology needs to add hydrogen peroxide and Fe 2+ The hydroxyl free radical (OH) is generated, the drug adding cost and the safety in the transportation process are problems of Fenton technology application, so that the electro-Fenton technology is generated, and the oxygen in the water can be reduced to generate hydrogen peroxide through 2 electrons by applying an electric field, so that the application cost and difficulty are reduced.
For example: patent (CN 110117046A) discloses a preparation method and application of a green electro-Fenton cathode, which comprises the steps of mixing biochar, carbon black, polytetrafluoroethylene dispersion liquid and ethanol to form paste, pressing the paste on foam nickel, and heating and stabilizing to obtain the green electro-Fenton cathode. However, this method uses nickel foam as a substrate and has poor practicality; patent (CN 113023835A) discloses a preparation method of an electro-Fenton cathode material based on sludge-based biomass charcoal, a product and application thereof, wherein biomass powder obtained after municipal sludge treatment is subjected to hydrothermal reaction with urea, and then pyrolysis is carried out at 750-850 ℃ to obtain nitrogen-doped sludge-based biomass charcoal; and then uniformly mixing the material with polytetrafluoroethylene dispersion and ethanol, and pressing the obtained material on foam nickel to prepare the cathode. However, this method requires additional doping of urea as the N source and high temperature heating to stabilize the polytetrafluoroethylene coating.
As can be seen, there is currently no cathode modification material available for the electro-reduction hydrogen peroxide production reaction to generate sufficient hydroxyl radicals to remove antibiotics from water.
Disclosure of Invention
[ technical problem ]
The cathode material for the electro-Fenton reaction has poor practicability, and needs to be additionally doped with an external nitrogen source and needs high-temperature heating operation conditions; the preparation process is complex.
Technical scheme
In order to solve the problems, the invention obtains the electrode modification material after the activated biochar is activated, then the activated biochar, polyvinylidene fluoride and N, N-dimethylformamide are further mixed and coated on a substrate to obtain the activated blue algae biochar cathode material, and after the activated blue algae biochar cathode material is applied to an electro-Fenton system, various antibiotics can be degraded.
The first object of the invention is to provide a method for preparing activated blue algae biochar cathode material, comprising the following steps:
(1) Carrying out primary pyrolysis on blue algae powder to obtain pre-carbonized biochar; then combining the pre-carbonized biochar with a pore-forming agent for secondary pyrolysis; grinding, sieving and cleaning to obtain activated blue algae biochar;
(2) The activated blue algae biochar obtained in the step (1) is prepared from polyvinylidene fluoride (PVDF) and N, N-dimethylformamide according to the proportion (0.5-2.5 g): (0.5-2 g): (5-10 mL) and uniformly mixing to obtain electrode slurry;
(3) And (3) coating the electrode slurry obtained in the step (2) on an electrode substrate, and drying to obtain the activated blue algae biochar cathode material.
In one embodiment of the invention, the cyanobacteria of step (1) is taken from Jiangsu Taihu lake; the blue algae powder is obtained by drying blue algae at 105-120 ℃ for 6-12 h, grinding and sieving with a 80-100 mesh sieve.
In one embodiment of the invention, the primary pyrolysis in the step (1) is pyrolysis for 90-120 min at 300-500 ℃, and meanwhile, inert gas is introduced, and the flow rate is 150-200 mL/min; the inert gas includes nitrogen.
In one embodiment of the invention, the pore-forming agent in the step (1) is potassium hydroxide, and the mass ratio of the pore-forming agent to the pre-carbonized biochar is (1-2): 1.
in one embodiment of the invention, the secondary pyrolysis in the step (1) is pyrolysis for 90-120 min at 600-800 ℃, and meanwhile, inert gas is introduced, and the flow rate is 150-200 mL/min; the inert gas includes nitrogen.
In one embodiment of the present invention, the sieving in step (1) is a 80-100 mesh sieve.
In one embodiment of the present invention, the washing in step (1) is performed with ultrapure water until the pH is near neutral.
In one embodiment of the present invention, the electrode substrate in step (3) is a stainless steel substrate.
In one embodiment of the present invention, the drying in step (3) is performed at 60 to 105℃for 12 to 24 hours.
In one embodiment of the present invention, the amount of coating in step (3) is 2 to 8mg/cm 2 。
The second purpose of the invention is to prepare the activated blue algae biochar cathode material by the method.
The third object of the invention is to provide a method for degrading antibiotics based on the activated blue algae biochar cathode material, which comprises the following steps:
the antibiotic wastewater is taken as a treatment object, a stainless steel plate is taken as an anode, and the activated blue algae biochar cathode material is taken as a cathode, so that the antibiotic wastewater is degraded by electrifying, and the wastewater after degrading the antibiotic is obtained.
In one embodiment of the invention, the antibiotic wastewater contains one or more of sulfadiazine, chlortetracycline hydrochloride and ciprofloxacin; the concentration of the antibiotics is 12.5-50 mg/L.
In one embodiment of the present invention, the stainless steel plate is a 430 stainless steel plate.
In one embodiment of the invention, the aeration rate in the process is 100150mL/min, and the applied current density is 5-50 mA/cm 2 。
In one embodiment of the invention, the electrolyte used in the method is sodium sulfate at a concentration of 5 to 60mM.
In one embodiment of the invention, the pH value in the method is 3-7, and the medicament used for regulating the pH value is 1mol/L dilute sulfuric acid and sodium hydroxide.
In one embodiment of the invention, the method comprises the step of activating the blue algae biochar cathode material for recycling for not less than 4 times.
The fourth object of the invention is to provide a method for producing hydrogen peroxide by electrocatalytic catalysis based on the activated blue algae biochar cathode material, which comprises the following steps:
the sodium sulfate is used as electrolyte, the 430 stainless steel plate is used as anode, the activated blue algae biochar cathode material is used as cathode, and the cathode is electrified to generate two-electron transfer, and oxygen is reduced to generate hydrogen peroxide.
In one embodiment of the invention, the aeration rate in the method is 100-150 mL/min, and the applied current density is 5-50 mA/cm 2 。
In one embodiment of the invention, the pH value in the method is 3-7, and the medicament used for regulating the pH value is 1mol/L dilute sulfuric acid and sodium hydroxide.
In one embodiment of the invention, the method comprises the step of activating the blue algae biochar cathode material for recycling for not less than 4 times.
[ advantageous effects ]
(1) The activated blue algae biochar adopted by the invention has a relatively good surface pore structure, can be used as a cathode modification material, can be prepared into an activated blue algae biochar cathode material, and can be used for treating wastewater.
(2) The invention takes blue algae as a water pollutant as a raw material to prepare the activated blue algae biochar cathode material so as to realize resource utilization.
(3) The invention uses the polyvinylidene fluoride to prepare the electrode slurry, avoids the plastic deformation (creep deformation) of the conventional polytetrafluoroethylene electrode under the action of long-time continuous load, also avoids the problems of the increase of the electrode preparation difficulty and the falling of the coating caused by the non-tackiness of the polytetrafluoroethylene material, and simultaneously ensures that the pore structure of the surface of the biochar material is not damaged by using the polyvinylidene fluoride to prepare the electrode slurry.
(4) According to the invention, an electro-Fenton system is constructed by using activated blue algae biochar cathode materials to treat antibiotic wastewater, and various antibiotics with different types can be efficiently degraded through parameter adjustment, such as: the removal rate of sulfadiazine, chlortetracycline hydrochloride and ciprofloxacin reaches over 96 percent, and meanwhile, the electrode can be repeatedly used for 4 times, and the removal effect can still be maintained to be over 96 percent.
(5) The activated blue algae biochar cathode material is used for electrocatalytically producing hydrogen peroxide, and the accumulation amount of the hydrogen peroxide for 4 hours reaches more than 14.0261 mg/L.
Drawings
FIG. 1 is a pore distribution diagram of activated cyanobacteria biochar of example 1.
FIG. 2 is a surface Scanning Electron Microscope (SEM) image of the activated cyanobacteria biochar cathode material of example 2.
FIG. 3 is a graph showing the degradation effect of activated cyanobacteria biochar cathode material as cathode treatment antibiotics of the electro-Fenton system in example 3, (a) shows the concentration change of each antibiotic, and (b) shows the removal rate.
FIG. 4 is a graph showing the recycling effect of the electrode in example 5.
FIG. 5 is a graph showing the effect of electrocatalytic hydrogen peroxide production in example 6.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for better illustration of the invention, and should not be construed as limiting the invention.
The testing method comprises the following steps:
hydrogen peroxide testing: the cumulative concentration of hydrogen peroxide in water was determined from the visible absorption of the colored complex of Ti (IV) at a wavelength of 400nm, and the water sample was tested after filtration through a 0.22 μm organic-based filter membrane, and was combined with 0.05mol/L potassium titanium oxalate, 3mol/L sulfuric acid at a ratio of 2:1:1, and the instrument used is an ultraviolet-visible spectrophotometer (UV-1600, AOELAB) at a wavelength of 400 nm.
The method for detecting the content of antibiotics in water comprises the following steps: the concentration of antibiotics in water is measured by liquid chromatography, the water sample is filtered by a 0.22 mu m organic filter membrane and then tested, the used instrument is high performance liquid chromatography (Thermo Ultra 3000), and the instrument accurately obtains the concentration of antibiotics in the water sample according to a set standard curve.
The calculation formula of the antibiotic concentration is shown as formula (1):
wherein, R: removal rate (%); c (C) 0 : initial concentration (mg/L); c: concentration (mg/L) after completion of the treatment.
Example 1
A method for preparing activated blue algae biochar, comprising the following steps:
(1) Drying Taihu blue algae in a 105 ℃ oven for 24 hours, grinding and sieving with a 80-mesh sieve after drying, then taking a sieved sample, heating to 300 ℃ at 10 ℃/min under a nitrogen atmosphere with a gas flow rate of 150mL/min, and pyrolyzing for 90min at 300 ℃ to obtain pre-carbonized biochar;
(2) The pre-carbonized biochar and potassium hydroxide are mixed according to the mass ratio of 1:2, mixing, heating the mixture to 700 ℃ at a speed of 10 ℃/min under a nitrogen atmosphere with a gas flow rate of 150mL/min, and preserving heat at 700 ℃ for 120min;
(3) Grinding the product of the step (2), sieving with a 80-mesh sieve, washing with ultrapure water until the pH value is close to neutral, and drying at 105 ℃ to obtain the activated blue algae biochar.
The obtained activated blue algae biochar is tested, and the test result is shown in figure 1:
as can be seen from fig. 1: the activated blue algae biochar has better carbonization degree, the pore size distribution is mainly concentrated at 5nm or below, and a small amount of pore size distribution exists in the range of 10-30 nm, which indicates that the activated blue algae biochar has a micropore and mesoporous structure and can be used for catalyzing 2-electron oxygen reduction to produce hydrogen peroxide.
Example 2PVDF electrode
A method for preparing activated blue algae biochar cathode material comprises the following steps:
(1) The activated cyanobacteria charcoal of example 1, polyvinylidene fluoride, N-dimethylformamide were mixed according to 2.5g:2g: uniformly mixing 10mL to prepare electrode slurry;
(2) The electrode slurry was coated on a stainless steel substrate in an amount of 2.2mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And (5) placing the blue algae activated biochar cathode material in a baking oven at 105 ℃ for drying for 12 hours to obtain the activated blue algae activated biochar cathode material (PVDF electrode).
The obtained activated blue algae biochar cathode material is tested, and the test result is shown in figure 2:
as can be seen from fig. 2: the pore structure of the activated blue algae biochar cathode material is well reserved.
Example 3
A method for degrading antibiotics based on the activated blue algae biochar cathode material of the embodiment 2, comprising the following steps:
taking antibiotic wastewater (the antibiotic concentration is shown in table 1) as a treatment object, adding 20mM sodium sulfate; taking a 430 stainless steel plate as an anode and taking the activated blue algae biochar cathode material of the embodiment 2 as a cathode; the DC power supply is used as a power supply, and the current density is 30mA/cm 2 Aeration rate is 150mL/min, stirring (60 rpm) is kept in the whole process, and pH is 3; the experimental time is 4 hours; carrying out degradation reaction;
TABLE 1 index of antibiotic wastewater
| Antibiotics | Sulfadiazine | Aureomycin hydrochloride | Ciprofloxacin |
| Actual concentration (mg/L) | 22.35633 | 25.33612 | 24.97669 |
After the reaction is finished, filtering the supernatant by a 0.22 mu m filter head, measuring the concentration of antibiotics by a liquid chromatography, and washing and recycling the activated blue algae biochar cathode material.
Degradation results are shown in fig. 3: as can be seen from fig. 3: final removal rates of sulfadiazine, chlortetracycline hydrochloride, and ciprofloxacin were 96.10%, 98.46%, and 98.04%, respectively, illustrating: the electro-Fenton system formed by activating the blue algae biochar cathode material has better removal effect on various antibiotics and higher removal efficiency.
Example 4
A method for degrading antibiotics based on the activated blue algae biochar cathode material of the embodiment 2, comprising the following steps:
taking 25mg/L sulfadiazine wastewater as a treatment object, and adding 60mM sodium sulfate; taking a 430 stainless steel plate as an anode and taking the activated blue algae biochar cathode material of the embodiment 2 as a cathode; the DC power supply is used as a power supply, the current density and the pH are shown in Table 2, the aeration rate is 150mL/min, the stirring (60 rpm) is kept in the whole process, and the pH is 3; the experimental time is 4 hours; carrying out degradation reaction;
degradation results are shown in table 2: as can be seen from table 2: different pH values and current density conditions have great influence on degradation effect, under the condition that the pH value is 3, the degradation effect is better than other acid-base environments, and when neutral, precipitation occurs in a large amount, so that the degradation effect is improved, but the generated sludge needs subsequent treatment. At a current density higher than 20mA/cm 2 After that, the degradation effect is kept stable, so that the blue algae biochar electrode is activated under different parameter conditionsThe use of the electro-Fenton system to degrade antibiotics has a great influence and proper parameter conditions need to be selected to achieve the best treatment effect.
Table 2 results of degradation rate test in example 4
Example 5
A method for degrading antibiotics based on the activated blue algae biochar cathode material of the embodiment 2, comprising the following steps:
taking 30mg/L sulfadiazine wastewater as a treatment object, and adding 20mM sodium sulfate; taking a 430 stainless steel plate as an anode and taking the activated blue algae biochar cathode material of the embodiment 2 as a cathode; the DC power supply is used as a power supply, and the current density is 30mA/cm 2 Aeration rate is 150mL/min, stirring (60 rpm) is kept in the whole process, and pH is 3; the experimental time is 4 hours; carrying out degradation reaction;
after the reaction is finished, the activated blue algae biochar cathode material is washed and then recycled;
the electrodes were subjected to a cycling experiment, the results of which are shown in fig. 4, as can be seen from fig. 4: after 4 times of use, the electrode treatment effect is still stable, and the removal effect can still be maintained to be more than 96%.
Comparative example 1 PTFE electrode
The polyvinylidene fluoride in example 2 was modified to be Polytetrafluoroethylene (PTFE); the specific operation is as follows:
(1) The activated cyanobacteria charcoal of example 1, polytetrafluoroethylene (PTFE), N-dimethylformamide were mixed according to 2.5g:2g: uniformly mixing 10mL to prepare electrode slurry;
(2) The electrode slurry was coated on a stainless steel substrate in an amount of 2.1mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And (3) after coating, stabilizing the cathode material in a muffle furnace at a high temperature of 360 ℃ for 2 hours.
Comparative example 2 SBR electrode
A method of preparing a cathode material comprising the steps of:
(1) The activated blue algae biochar, styrene-butadiene rubber emulsion and carboxymethyl cellulose of example 1 were mixed according to 2.5g:357mL: uniformly mixing the materials in a proportion of 0.35g to prepare electrode slurry;
(2) The electrode slurry was coated on a stainless steel substrate in an amount of 2.5mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And (5) placing the cathode material in a baking oven at 105 ℃ for drying for 12 hours to obtain the cathode material.
Comparative example 3 nafion electrode
A method of preparing a cathode material comprising the steps of:
(1) Activated blue algae biochar of example 1, perfluorosulfonic acid (nafion) and ethanol were mixed according to 2.5g:25mL: uniformly mixing 225mL to prepare electrode slurry;
(2) The electrode slurry was coated on a stainless steel substrate in an amount of 1.9mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And (5) placing the cathode material in a baking oven at 105 ℃ for drying for 12 hours to obtain the cathode material.
Example 6
A method for electrocatalytic hydrogen peroxide production based on cathode material, comprising the steps of:
ultrapure water as a medium, 20mM sodium sulfate was added; the cathode materials of example 2, comparative example 1, comparative example 2, comparative example 3 were used as cathodes with 430 stainless steel plates as anodes; the DC power supply is used as a power supply, and the current density is 30mA/cm 2 Aeration rate is 150mL/min, stirring (60 rpm) is kept in the whole process, and pH is 3; the experimental time is 4 hours; performing electrocatalytic hydrogen peroxide production reaction;
after the reaction was completed, the supernatant was filtered through a 0.22 μm filter head, and then subjected to a hydrogen peroxide concentration test, the test results being shown in table 3 below:
as can be seen from table 3: the PVDF electrode of example 2 had a hydrogen peroxide production accumulation of 14.0261mg/L and the PTFE electrode of comparative example 1 had a hydrogen peroxide production accumulation of 8.3547mg/L; the accumulation amount of hydrogen peroxide produced by the SBR electrode of comparative example 2 is 8.4735mg/L; the accumulation amount of hydrogen peroxide produced by the nafion electrode of comparative example 3 was 11.0876mg/L.
TABLE 3 test results of Hydrogen peroxide concentration (mg/L) for example 6
Fig. 5 is a graph showing the effect of electrocatalytic hydrogen peroxide production for the PTFE electrode of comparative example 1 and the PVDF electrode of example 2. As can be seen from fig. 5: in the high-temperature stabilization process of the preparation, the pores of the biochar collapse to a certain extent due to high temperature, so that a certain pore structure is destroyed, and meanwhile, in the high-temperature stabilization process, PTFE covers the surface of the biochar, so that the hydrogen peroxide production capacity of the electrocatalytic system is further weakened. It can be seen that the choice of coating material affects the effect of the finishing material.
Claims (4)
1. The method for producing hydrogen peroxide by electrocatalytic catalysis based on activated blue algae biochar cathode material is characterized by comprising the following steps:
sodium sulfate is used as electrolyte, a 430 stainless steel plate is used as an anode, an activated blue algae biochar cathode material is used as a cathode, and the cathode is electrified to generate two-electron transfer, and oxygen is reduced to generate hydrogen peroxide;
wherein the aeration rate in the method is 100-150 mL/min, and the applied current density is 5-50 mA/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The pH value is 3-7;
the method for preparing the activated blue algae biochar cathode material comprises the following steps:
(1) Carrying out primary pyrolysis on blue algae powder to obtain pre-carbonized biochar; then combining the pre-carbonized biochar with a pore-forming agent for secondary pyrolysis; grinding, sieving and cleaning to obtain activated blue algae biochar; the secondary pyrolysis is pyrolysis for 90-120 min at 700-800 ℃; the obtained activated blue algae biochar has a micropore and mesoporous structure;
(2) The activated blue algae biochar obtained in the step (1) is prepared from polyvinylidene fluoride and N, N-dimethylformamide according to the proportion (0.5-2.5 g): (0.5-2 g): (5-10 mL) uniformly mixing to obtain electrode slurry;
(3) Coating the electrode slurry obtained in the step (2) on an electrode substrate, and drying at 105 ℃ to obtain the activated blue algae biochar cathode material; wherein the electrode substrate is stainless steel baseThe coating amount is 2-8 mg/cm 2 。
2. The method of claim 1, wherein the primary pyrolysis in the step (1) is pyrolysis at 300-500 ℃ for 90-120 min, and inert gas is introduced at the same time, and the flow rate is 150-200 mL/min; the inert gas comprises nitrogen; introducing inert gas into the furnace at the same time of secondary pyrolysis, wherein the flow rate is 150-200 mL/min; the inert gas includes nitrogen.
3. The method of claim 1, wherein the pore-forming agent of step (1) is potassium hydroxide, and the mass ratio of the pore-forming agent to the pre-carbonized biochar is (1-2): 1.
4. a method for degrading antibiotics based on the activated blue algae biochar cathode material prepared in claim 1, comprising the following steps:
taking antibiotic wastewater as a treatment object, taking a stainless steel plate as an anode, taking the activated blue algae biochar cathode material prepared in the method of claim 1 as a cathode, and carrying out power on degradation to obtain wastewater after degrading the antibiotic;
the aeration rate in the method is 100-150 mL/min, and the applied current density is 5-50 mA/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The pH value is 3-7;
the antibiotic wastewater contains one or more of sulfadiazine, chlortetracycline hydrochloride and ciprofloxacin; the concentration of the antibiotics is 12.5-50 mg/L.
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