CN109759116B - Method for promoting decomposition and purification of perfluorinated compounds by photoelectric coupling - Google Patents
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- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims abstract description 21
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
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Abstract
The invention provides a method for promoting decomposition and purification of a perfluorinated compound by photoelectric coupling, belonging to the technical field of perfluorinated compound treatment and energy conservation and recycling. Preparing carbon nano sheet/g-C3N4/BiWO6The catalytic electrode is prepared by a method of fixedly coating silica sol on a stainless steel mesh, a photocatalysis and electrocatalysis coupled system is constructed by a connecting circuit, and the degradation and purification of the perfluorooctanoic acid under the actions of photocatalysis, electrocatalysis, dark adsorption and photoelectrocatalysis, the effect influence of degrading the perfluorooctanoic acid under different pH conditions and the effect influence of degrading the perfluorooctanoic acid under aeration and non-aeration conditions are respectively realized. The synergistic effect of the photocatalysis technology and the electrocatalysis technology greatly improves the degradation performance of the photoelectrocatalysis.
Description
Technical Field
The invention belongs to the technical field of perfluorinated compound treatment and energy conservation and recycling, and relates to carbon nanosheet/g-C3N4/BiWO6The preparation of the nano composite catalyst and the photoelectrocatalysis synergistic effect of the nano composite catalyst decompose and purify pollutants and generate electric energy, and the degradation efficiency and the electricity generation capability of perfluorinated compounds are improved.
Background
Perfluorocompounds are widely used in the fields of industrial production and consumer goods. It can be detected in different environmental media worldwide due to direct or indirect emissions during manufacturing, use and disposal. The perfluoro compound has environmental pollutants with strong biological toxicity, and is mainly manifested by neurobehavioral toxicity, organ toxicity, reproductive toxicity, genetic toxicity and carcinogenicity. Especially, the representative compound of perfluorooctanoic acid can seriously pollute the environment and harm human beings and the global ecosystem if the perfluorooctanoic acid is not properly treated. Different purification methods (physical removal, chemical removal and biological removal) have their limitations while being able to perform their purification functions. It is therefore necessary to find an effective and efficient treatment.
The photoelectrocatalysis technology combines two processes of electrolysis and catalysis, can prolong the service life of photoproduction electrons and holes, reduce the recombination rate of the electrons and the holes, and greatly enhance the activity of photocatalysis, thereby thoroughly removing pollutants or decomposing the pollutants into useful substances. Among them, the photocatalyst is the key of the photoelectrocatalysis technology. Bi2WO6As an excellent visible light driving photocatalyst, the photocatalyst has a narrow band gap and a proper energy band position (Eg ═ 0.58-3.30 eV). Due to double halogen interlayer [ Bi ]2O2]2+And WO6The octahedral nanosheets are overlapped to form an alternate layered structure, so that the octahedral nanosheets have a large internal electric field and an asymmetric polarization effect, and show excellent visible light catalytic activity, thereby facilitating electron-hole separation. Graphitic carbon nitride (g-C)3N4) Is a metal-free polymer semiconductor, and has great application in the field of photocatalysis due to good thermochemical stability, electronic and optical properties, low price and no toxicity. Due to g-C3N4The potential of the CB of (1.12 eV) is negative enough, and the strong reduction capability of electrons in the surface CB has great potential for the purification of pollutants.
In recent years, carbon nanomaterials have been extensively studied due to their excellent power density, fast charge/discharge rates and excellent cycle stability. The two-dimensional carbon material has a large aspect ratio and a porous structure, so that the ion transmission distance of a nano scale can be shortened, the pore structure and the conductivity of the material can be improved, the transfer process of electrons and electrolyte ions is improved, the electron transmission is facilitated, and the conductivity is improved.
The application uses carbon nano sheet/g-C3N4/BiWO6As experimental catalysts, enhanced photoelectrocatalysisThe degradation performance and the electricity generation performance of the technology effectively treat the perfluorooctanoic acid.
Disclosure of Invention
The invention designs a carbon nano sheet/g-C3N4/BiWO6The photoelectrocatalysis component successfully constructs a photoelectrocatalysis purification system. The system not only can be used as an electrode, but also has the photocatalysis function and the electric conduction, the whole treatment and purification efficiency is greatly improved, the energy consumption is lower, and the concentration of pollutants is greatly reduced. The degradation efficiency and the power generation capability of the photoelectrocatalysis technology are greatly improved under the condition of low energy consumption. The system can theoretically treat perfluorooctanoic acid, expands the application of a photoelectrocatalysis technology, and provides a new idea for photoelectrocatalysis and treatment of perfluorocompounds.
The technical scheme of the invention is as follows:
the method for promoting decomposition and purification of the perfluorinated compounds by photoelectric coupling comprises the following steps:
(1) preparation of carbon Nanosheet/g-C3N4/BiWO6The compound is as follows:
preparing GO according to an improved Hummers method for later use; adding the overdue flour and KOH into deionized water at the temperature of 80 ℃, stirring and mixing for 10 minutes, controlling the mass ratio of the overdue flour to the KOH to be 1: 1-2, and controlling the concentration of the overdue flour in a mixing system to be 10-15 mg/ml; adding GO, continuously stirring for 1.5-3 hours at the same temperature, controlling the mass ratio of KOH to GO to be 65-70: 1, adding urea when the mixed solution is cooled to 20-30 ℃, controlling the mass ratio of KOH to urea to be 1-3: 1, and continuously stirring for 0.5-2 hours; obtaining a mixture by freeze-drying; activating the freeze-dried mixture at 550-700 ℃ for 3-5 hours; treating the obtained product with dilute hydrochloric acid, neutralizing with deionized water, and freeze-drying overnight to obtain carbon nanosheets; heating melamine in a vacuum tube furnace at 500-600 ℃ for 3-5 hours, and heating the heated product at 480-550 ℃ for 1.5-3 hours to obtain g-C3N4；
(2) Cetyl trimethyl ammonium bromide and Na2WO4·2H2O and Bi (NO)3)·5H2Adding O into deionized water, cetyl trimethyl ammonium bromide and Na2WO4·2H2O and Bi (NO)3)·5H2The mass ratio of the oxygen to the sulfur to the oxygen is 1: 6-7: 19-20, the concentration of cetyl trimethyl ammonium bromide in the mixed solution is 0.6-0.7 mg/ml, after the mixture is uniformly stirred, the prepared carbon nanosheet and g-C are added3N4Continuously stirring for 0.5-1 hour, reacting for 20-26 hours at the temperature of 100-130 ℃, and cooling to obtain a mixture; washing, centrifuging, drying and grinding to obtain the carbon nano sheet/g-C3N4/BiWO6(ii) a Wherein g-C3N4And BiWO6The mass ratio of (1): 3-5 carbon nanosheet and g-C3N4/BiWO6The mass ratio of (1): 180-220 parts by weight;
(3) preparing a photoelectrocatalysis electrode: firstly, cutting a stainless steel net into proper sizes, washing with deionized water, ultrasonically washing with absolute ethyl alcohol, and drying in a blast furnace for later use; mixing carbon nanosheets with g-C3N4/BiWO6The ratio of the total mass of the silica sol to the silica sol in terms of mass-volume ratio g/mL is 1:1, then uniformly brushing the mixture on a stainless steel net to obtain the carbon nano sheet/g-C3N4/BiWO6An electrode;
(4) constructing a photoelectrocatalysis treatment system: with carbon nanosheet/g-C3N4/BiWO6The electrode is used as a cathode, the iron rod is used as an anode, and the electrodes are connected by a lead to form a circuit and are arranged in the long tubular single-chamber reactor; the light source vertically irradiates on the carbon nano-sheet/g-C3N4/BiWO6On the electrode.
The invention has the beneficial effects that: the system integrates photocatalytic purification, electro-catalytic purification and photoelectric cooperative operation, degrades and removes perfluorinated compounds, especially perfluorooctanoic acid, is favorable for degrading organic pollutants more thoroughly and rapidly, and enhances the power generation capacity and level. The catalytic electrode of the system has good stability, and can continuously degrade pollutants and generate electricity.
Drawings
Fig. 1 is a graph comparing the removal effect of degraded perfluorooctanoic acid by four systems of Photocatalysis (PC), Electrocatalysis (EC), Dark adsorption (Dark) and Photoelectrocatalysis (PEC). In the figure, the abscissa is time (min) and the ordinate is the ratio of the current concentration to the initial concentration.
Figure 2 is a graph comparing the removal of perfluorooctanoic acid by PEC system treatment at pH 3, 7, 11. In the figure, the abscissa is time (min) and the ordinate is the ratio of the current concentration to the initial concentration.
FIG. 3 is a graph comparing the effect of degrading perfluorooctanoic acid with and without aeration in a photoelectrocatalysis system. In the figure, the abscissa is time (min) and the ordinate is the ratio of the current concentration to the initial concentration.
Detailed Description
The following detailed description of the invention refers to the accompanying drawings.
The first embodiment is as follows: photoelectric coupling system for treating perfluorooctanoic acid
The catalytic electrode is placed in a long tubular quartz reactor, connected above the catalytic electrode by an alligator clip, connected by a lead to form a circuit and connected with a 1000 ohm resistor. Aeration is provided at the bottom of the reactor. The visible light source is a 50W tungsten halogen lamp. Before the reaction, 0.01mol/L sodium hydrogen sulfite was added to and dissolved in a 10mg/L perfluorooctanoic acid solution, and after the reaction, samples were taken every 30min and the concentration was measured by HPLC-MS. The reaction was carried out for a total of 2 hours, and the removal rate of perfluorooctanoic acid was calculated.
In fig. 1, the different degradation effects of four systems, Photocatalytic (PC), Electrocatalytic (EC), Dark adsorption (Dark) and Photoelectrocatalytic (PEC), were measured and compared to the electrogenic performance. Wherein, the PFC photoelectrocatalysis degradation rate is the highest, and can reach 90% in 1 hour.
In fig. 2, the removal of perfluorooctanoic acid by PEC at different initial pH conditions was determined. When the pH is not adjusted (pH 7), the degradation rate is the highest, which can reach 90% in 1 hour, while when the pH is 3 and 11, the degradation rate at 1 hour is lower than when the pH is not adjusted (pH 4.6), but the degradation tendency is the same, and finally the perfluorooctanoic acid can be degraded. Demonstrating that the PEC system's degradation of perfluorooctanoic acid can be applied to a wider range of pH.
Example two: treatment of perfluorooctanoic acid with and without aeration system
The catalytic electrode is placed in a long tubular quartz reactor, connected above the catalytic electrode by an alligator clip, connected by a lead to form a circuit and connected with a 1000 ohm resistor. Aeration is provided at the bottom of the reactor. The visible light source is a 50W tungsten halogen lamp. Before the reaction, 0.01mol/L sodium hydrogen sulfite was added to and dissolved in a 10mg/L perfluorooctanoic acid solution, and after the reaction, samples were taken every 30min and the concentration was measured by HPLC-MS. The reaction was carried out for a total of 2 hours, and the removal rate of perfluorooctanoic acid was calculated.
In fig. 3, the degradation effect and the electricity generation performance of the system aeration (aeration) and the system non-aeration (no aeration) are compared. Wherein, the photoelectrocatalysis degradation rate is the highest in aeration, and can reach 90 percent in 1 hour, which is far higher than that in non-aeration.
Claims (2)
1. A method for promoting decomposition and purification of perfluorinated compounds by photoelectric coupling is characterized by comprising the following steps:
(1) preparation of carbon nanoplatelets and g-C3N4：
Preparing GO according to an improved Hummers method for later use; adding the overdue flour and KOH into deionized water at the temperature of 80 ℃, stirring and mixing for 10 minutes, controlling the mass ratio of the overdue flour to the KOH to be 1: 1-2, and controlling the concentration of the overdue flour in a mixing system to be 10-15 mg/ml; adding GO, continuously stirring for 1.5-3 hours at the same temperature, controlling the mass ratio of KOH to GO to be 65-70: 1, adding urea when the mixed solution is cooled to 20-30 ℃, controlling the mass ratio of KOH to urea to be 1-3: 1, and continuously stirring for 0.5-2 hours; obtaining a mixture by freeze-drying; activating the freeze-dried mixture at 550-700 ℃ for 3-5 hours; treating the obtained product with dilute hydrochloric acid, neutralizing with deionized water, and freeze-drying overnight to obtain carbon nanosheets; heating melamine in a vacuum tube furnace at 500-600 ℃ for 3-5 hours, and heating the heated product at 480-550 ℃ for 1.5-3 hours to obtain g-C3N4；
(2) Cetyl trimethyl ammonium bromide and Na2WO4·2H2O and Bi (NO)3)3·5H2Adding O into deionized water, cetyl trimethyl ammonium bromide and Na2WO4·2H2O and Bi (NO)3)3·5H2The mass ratio of the oxygen to the sulfur to the oxygen is 1: 6-7: 19-20, the concentration of cetyl trimethyl ammonium bromide in the mixed solution is 0.6-0.7 mg/ml, after the mixture is uniformly stirred, the prepared carbon nanosheet and g-C are added3N4Continuously stirring for 0.5-1 hour, reacting for 20-26 hours at the temperature of 100-130 ℃, and cooling to obtain a mixture; washing, centrifuging, drying and grinding to obtain the carbon nano sheet/g-C3N4/Bi2WO6(ii) a Wherein g-C3N4And Bi2WO6The mass ratio of (1): 3-5 carbon nanosheet and g-C3N4/Bi2WO6The mass ratio of (1): 180-220 parts by weight;
(3) preparing a photoelectrocatalysis electrode: firstly, cutting a stainless steel net into proper sizes, washing with deionized water, ultrasonically washing with absolute ethyl alcohol, and drying in a blast furnace for later use; mixing carbon nano-sheets/g-C3N4/Bi2WO6The ratio of the total mass of the silica sol to the silica sol in terms of mass-volume ratio g/mL is 1:1, then uniformly brushing the mixture on a stainless steel net to obtain the carbon nano sheet/g-C3N4/Bi2WO6An electrode;
(4) constructing a photoelectrocatalysis treatment system: with carbon nanosheet/g-C3N4/Bi2WO6The electrode is used as a cathode, the iron rod is used as an anode, and the electrodes are connected by a lead to form a circuit and are arranged in the long tubular single-chamber reactor; the light source vertically irradiates on the carbon nano-sheet/g-C3N4/Bi2WO6On the electrode.
2. The method for promoting decomposition and purification of perfluoro-compounds by photoelectric coupling as claimed in claim 1, wherein the photo-catalytic technique is coupled with the electro-catalytic technique, and the perfluoro-compound is perfluoro-octanoic acid.
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| WO2011048128A3 (en) * | 2009-10-22 | 2012-04-12 | Basf Se | Photocatalyst having increased daylight activity |
| CN104628193A (en) * | 2014-12-30 | 2015-05-20 | 北京师范大学 | Method for performing combined catalytic degradation on perfluorooctane sulfonate in water by using visible light-electricity |
| CN105688970A (en) * | 2016-02-29 | 2016-06-22 | 湖南大学 | g-C3N4 modified self-doping Bi2WO6 composite photocatalyst and preparation method and application thereof |
| CN107020143A (en) * | 2017-03-24 | 2017-08-08 | 江苏大学 | A kind of preparation method and purposes of visible light-responded Three-element composite photocatalyst |
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| WO2011048128A3 (en) * | 2009-10-22 | 2012-04-12 | Basf Se | Photocatalyst having increased daylight activity |
| CN104628193A (en) * | 2014-12-30 | 2015-05-20 | 北京师范大学 | Method for performing combined catalytic degradation on perfluorooctane sulfonate in water by using visible light-electricity |
| CN105688970A (en) * | 2016-02-29 | 2016-06-22 | 湖南大学 | g-C3N4 modified self-doping Bi2WO6 composite photocatalyst and preparation method and application thereof |
| CN107020143A (en) * | 2017-03-24 | 2017-08-08 | 江苏大学 | A kind of preparation method and purposes of visible light-responded Three-element composite photocatalyst |
Non-Patent Citations (2)
| Title |
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| Bi2WO6/g-C3N4复合型催化剂的制备及其可见光光催化性能;桂明生 等;《无机化学学报》;20131031;第29卷(第10期);第2057-2064页 * |
| Enhanced photocatalytic activity of graphitic carbon nitride/carbon nanotube/Bi2WO6 ternary Z-scheme heterojunction with carbon nanotube as efficient electron mediator;Deli Jiang et al.;《Journal of Colloid and Interface Science》;20180215;第512卷;第1-23页 * |
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