CN110220963B - Determination method of electron transfer process and application of electron transfer process in degradation process of organic pollutants - Google Patents
Determination method of electron transfer process and application of electron transfer process in degradation process of organic pollutants Download PDFInfo
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Abstract
The invention relates to a determination method of an electron transfer process and application thereof in a degradation process of organic pollutants. The method for measuring the electron transfer comprises the following steps: fixing a carbon material on a glassy carbon electrode to form a three-electrode system, immersing the electrode in a buffer solution, detecting the open-circuit potential of the carbon material after persulfate is added, taking the open-circuit potential as an initial potential, recording the current increment before and after the electron donor compound is added, and judging the difficulty degree of electron transfer according to the current increment condition. According to the invention, the non-free radical electron transfer process of the carbon material activated persulfate is disclosed more accurately by an open-circuit potential and timing current coupling method, and the method is applied to the organic pollutant degradation process of a carbon material activated persulfate system, so that the degradation condition of the organic pollutant is directly judged, and a new thought is provided for the research and development of an organic pollutant control technology.
Description
Technical Field
The invention relates to a method for measuring an electron transfer process, in particular to a method for measuring an electron transfer process of a carbon material activated persulfate system and application thereof in an organic pollutant degradation process.
Background
In recent years, the activated persulfate advanced oxidation technology is attracting more and more attention, and the activation modes commonly used at present are thermal, alkali, ultraviolet light, ultrasonic, electric, transition metal and nonmetal activation. In the activation modes, the non-metallic carbon material has the unique advantages of no toxicity, acid and alkali resistance, wide sources, rich pore structure, adjustable surface groups and the like, and can effectively avoid the problems of leaching of metal catalysts and secondary pollutants in the persulfate activation process, thereby causing wide attention of researchers. At present, traditional carbon materials such as activated carbon, granular activated carbon, activated carbon fiber and biochar, and nano-carbon materials such as graphene, nano-diamond, mesoporous carbon and carbon nano-tube are found to be capable of effectively activating persulfate to rapidly degrade organic pollutants. Initially, a number of studies reported that non-metallic carbon materials activate persulfate primarily as a radical process (i.e., a process that generates sulfate radicals). Subsequently, researchers found that methanol (radical quencher) was not effective in inhibiting the degradation of organics in the system, and the reaction mechanism was thought to be primarily related to non-radical processes. Therefore, the non-free radical oxidation of the non-metal carbon material activated persulfate to degrade the organic pollutants is gradually recognized by researchers, wherein the non-free radical process is mainly represented by an electron transfer process. However, the non-radical pathway of electron transfer, unlike the radical pathway or singlet oxygen non-radical pathway, can directly demonstrate the presence of active species with Electron Paramagnetic Resonance (EPR) technology.
Although some measurement methods for electron transfer processes, such as the linear free energy relationship method (Environmental science & technology,2017,51(18):10718-10728), the density functional theory calculation method (Environmental science & technology,2017,51(19):11288-11296) and the linear sweep voltammetry method (Chemical Engineering Journal,2015,266:28-33), have been established at home and abroad, the test period of some methods, such as the linear free energy relationship method and the density functional theory calculation method, is long. The linear sweep voltammetry is adopted by extensive researchers due to the advantages of simplicity, high efficiency and the like. However, the linear sweep voltammetry has certain limitations in researching the non-radical process of the carbon activated persulfate: first, the carbon material generally has a large adsorbability, and the surface electrochemical properties of the carbon material may be changed after the persulfate and the electron donor compound are added (Electrochimica Acta,2018,286:179-186), so that the background value is deviated and the result is affected. Secondly, the surface of the Carbon material is susceptible to oxidation reactions at high oxidation potentials (Carbon,2018,140:41-56) and does not show the results of the starting material in the actual reaction process. Finally, most electron donating compounds volatilize electrons at a lower oxidation potential to form intermediates (Journal of electrochemical Chemistry,2011,655(1):9-16), and it cannot be stated during the test whether the transferred electrons are supplied by the electron donating compound itself or by the intermediates.
At present, the non-free radical route of carbon activated persulfate is gradually known by researchers, but the lack of reasonable research methods leads to controversial research results on the mechanism. Therefore, accurate, simple and efficient practical detection methods are needed for more precise research and disclosure of electron transfer processes of non-radical pathways of carbon material activated persulfate.
Disclosure of Invention
The invention aims to provide a method for measuring an electron transfer process, which can more accurately disclose the electron transfer process of a non-free radical path of a carbon material activated persulfate system by an open-circuit potential and timing current coupling method, and can be applied to the degradation process of organic pollutants in the carbon material activated persulfate system to directly judge the degradation condition of the organic pollutants.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for measuring an electron transfer process in a carbon material activated persulfate system comprises the following steps:
(1) fixing a carbon material on a glassy carbon electrode to form a three-electrode system and immersing the three-electrode system in a buffer solution;
(2) detecting the change of the open circuit potential on the surface of the carbon material when persulfate is added into the solution in the step (1), and recording the potential in a stable state as U;
(3) taking U obtained in the step (2) as an initial potential, recording the current passing through the carbon material before and after the electron-donating compound is added into the solution in the step (1), and respectively recording the average current as I1And I2；
(4) The current change value Δ I in step (3) is I2-I1When Δ I>When Δ I is 0, electron transfer occurs, and when Δ I is larger, electron transfer is easier, and when Δ I is 0, electron transfer does not occur in the system.
According to the scheme, the carbon material in the step (1) is carbon nano tube, graphene, graphite powder, biochar or activated carbon.
According to the scheme, the three electrode systems in the step (1) are as follows: the carbon material is fixed on a glassy carbon electrode to serve as a working electrode, a platinum electrode serves as a counter electrode, and a saturated calomel electrode serves as a reference electrode.
According to the scheme, the buffer solution in the step (1) is a phosphate buffer solution, and the pH range is 3-11.
According to the scheme, the persulfate is peroxydisulfate or peroxymonosulfate.
According to the above scheme, the peroxydisulfate is potassium peroxydisulfate, sodium peroxydisulfate or ammonium peroxydisulfate.
According to the scheme, the electron donor compound is a phenolic compound or an organic dye.
According to the scheme, the organic dye is azo dye, anthraquinone dye or triphenylmethane dye.
According to the scheme, the phenolic compound is a compound which takes phenol as a basic structure and is substituted by 1-5 same or different substituent groups R at the ortho-position, the meta-position or the para-position, wherein the R group is methoxy, hydroxyl, phenyl, a halogen group, nitro, carboxyl, ester group, alkyl, amide or amino.
A method for judging an electron transfer process in an organic pollutant degradation process comprises the following specific steps: when the electron donor organic pollutants are degraded by the carbon material activated persulfate system, the electron transfer difficulty is judged by the measurement method of the electron transfer process.
The persulfate is brought into contact with the non-metallic carbon material to form a carbon/persulfate complex, whereby the potential of the surface of the carbon layer can be increased. In the invention, firstly, the open-circuit potential of the carbon material after adding the persulfate is measured by an open-circuit potential method, and the potential of the surface of the carbon layer after adding the persulfate is determined. In a three-electrode system formed by taking a carbon material as a working electrode, the open-circuit potential of the carbon material after persulfate is added is used as an initial potential to simulate the interaction process of the carbon material and the persulfate, the current change condition (delta I) of the surface of the carbon material before and after the electron donor compound is added is detected by a chronoamperometry, and the process of capturing electrons of the electron donor compound after the interaction of the carbon material and the persulfate is simulated. The difficulty degree of electron transfer is judged according to the current change condition. In the actual situation that the carbon material activated persulfate degrades electron-donating organic pollutants, the more easily the organic pollutants give electrons, and the larger the delta I is, the faster the degradation rate is; if the electron-donating ability of the organic pollutants is extremely weak, and the delta I is 0, the organic pollutants cannot be degraded.
The invention has the beneficial effects that:
1. the method for measuring the electron transfer process provided by the invention can monitor the change condition of the electrochemical property of the non-metallic carbon material in situ in the process of activating persulfate to degrade the electron-donating organic pollutants from the electrochemical angle, thereby disclosing the electron transfer reaction process and providing a new technology for researching the electron transfer mechanism.
2. According to the method for determining the electron transfer process, the degradation condition of the organic pollutants is judged only by simple electrochemical tests, and the result is not judged by the traditional complex degradation experiment, so that a new thought is provided for the research and development of the organic pollutant control technology.
Drawings
FIG. 1 is a graph showing the open circuit potential change before and after adding potassium peroxodisulfate to a carbon nanotube electrode.
FIG. 2 is a graph of the timing current before and after the addition of phenol to the carbon nanotube electrode at a potential of 0.636V.
FIG. 3 is a graph showing the timing current of the carbon nanotube electrode before and after the addition of 4-nitrophenol at a potential of 0.636V.
FIG. 4 is a graph showing the timing current curve before and after adding dimethyl phthalate to the carbon nanotube electrode at a potential of 0.636V.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Comparative example 1
(1) Mixing carbon nanotube powder and a Nafion adhesive, fixing the mixture on a glassy carbon electrode to prepare a working electrode, forming a three-electrode system by using a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and immersing the electrodes in a proper amount of 20 mmol/L phosphoric acid buffer solution with the pH value of 7.3;
(2) detecting the open-circuit potential of the carbon nano tube in the solution in the step (1), wherein the plateau value is 0.397V;
(3) the surface current of the carbon nano tube electrode before and after adding the organic pollutant (phenol, 4-nitrophenol or dimethyl phthalate) is detected by taking 0.397V (simulating the potential of the carbon nano tube when the potassium persulfate is not added) as an initial potential, and the result shows that the current is not obviously changed.
The comparative example shows that the original open circuit potential of the carbon nano tube is taken as the initial potential, the electron transfer of the organic pollutant (phenol, 4-nitrophenol or dimethyl phthalate) can not be caused, and the oxidation reaction of the organic pollutant is not caused.
Example 1
Carbon nanotube activated potassium peroxydisulfate determination of the Electron transfer Process to phenol
(1) Mixing carbon nanotube powder and a Nafion adhesive, fixing the mixture on a glassy carbon electrode to prepare a working electrode, forming a three-electrode system by using a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and immersing the electrodes in a proper amount of 20 mmol/L phosphoric acid buffer solution with the pH value of 7.3;
(2) detecting the open circuit potential of the carbon nano tube when potassium peroxodisulfate is added into the solution in the step (1), wherein the plateau value is 0.636V;
(3) detecting the current change before and after phenol is added into the solution in the step (1) by taking 0.636V as an initial potential, wherein the result shows that the current change value delta I is about 0.4 mu A;
in this example, the phenol concentration was 0.1 mmol/L, the carbon nanotube concentration was 0.1 g/L, and the potassium peroxodisulfate concentration was 1.0 mmol/L.
Fig. 1 is a graph showing the variation of open circuit potential before and after adding potassium peroxodisulfate to a carbon nanotube electrode, wherein the open circuit potential of the carbon nanotube is increased from 0.397V to 0.636V after adding potassium peroxodisulfate, so that electrons of electron-donating organic pollutants can be more easily captured to oxidize the organic pollutants.
FIG. 2 is a graph of the timing current before and after the addition of phenol to the carbon nanotube electrode at a potential of 0.636V; it is shown that when the potential is 0.636V (i.e., simulating the potential of the carbon nanotubes after the addition of potassium peroxodisulfate), the current increases significantly by about 0.4 muA after the addition of phenol, indicating that the electron transfer process has occurred.
Table 1 shows the phenol removal effect of the various systems, and from the results in Table 1, the phenol removal efficiency of the potassium peroxodisulfate/carbon nanotube system was about 80.81% in 60 minutes (wherein the adsorption removal effect was less than 0.1%). From the above results, it can be shown that the carbon nanotubes and potassium peroxodisulfate perform oxidation on phenol in the process of electron transfer.
TABLE 1 removal of phenol by different systems
Example 2
Determination of electron transfer process of carbon nanotube activated potassium peroxodisulfate to 4-nitrophenol
(1) Mixing carbon nanotube powder and a Nafion adhesive, fixing the mixture on a glassy carbon electrode as a working electrode, a platinum electrode as a counter electrode, and a saturated calomel electrode as a reference electrode to form a three-electrode system, and immersing the electrodes in a proper amount of 20 mmol/L phosphoric acid buffer solution with the pH value of 7.3;
(2) detecting the open circuit potential of the carbon nano tube after potassium peroxodisulfate is added into the solution in the step (1), wherein the plateau value is 0.636V;
(3) detecting the current change before and after the 4-nitrophenol is added into the solution in the step (1) by taking 0.636V as an initial potential, wherein the result shows that the change value delta I is about 0.025 mu A;
in this example, the concentration of 4-nitrophenol was 0.1 mmol/L, the concentration of carbon nanotubes was 0.1 g/L, and the concentration of potassium peroxodisulfate was 1.0 mmol/L.
FIG. 3 is a graph of the timing current before and after the addition of 4-nitrophenol to the carbon nanotube electrode at a potential of 0.636V; it is shown that when the potential is 0.636V (i.e., simulating the potential of the carbon nanotubes after the addition of potassium peroxodisulfate), the current increases significantly by about 0.025 μ A after the addition of 4-nitrophenol. The number of electrons transferred when the electron donating compound was phenol was about 16 times that when 4-nitrophenol, compared to the increased current in example 1. It is shown that phenol transfers electrons more readily than 4-nitrophenol in the potassium peroxodisulfate/carbon nanotube system, causing oxidation to occur.
Table 2 shows the effect of different systems on the removal of 4-nitrophenol; the results show that the removal efficiency of 4-nitrophenol is about 34.59% in 60 minutes for the potassium peroxodisulfate/carbon nanotube system (with an adsorption removal effect of about 4.11%). From the above results, it can be shown that the carbon nanotubes and potassium peroxodisulfate can undergo an electron transfer process to oxidize 4-nitrophenol, but the oxidation rate is not as high as that of phenol.
TABLE 2 Effect of different systems on the removal of 4-nitrophenol
Example 3
Determination of electron transfer process of carbon nano tube activated potassium peroxodisulfate to dimethyl phthalate
(1) Mixing carbon nanotube powder and a Nafion adhesive, fixing the mixture on a glassy carbon electrode to prepare a working electrode, forming a three-electrode system by using a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and immersing the electrodes in a proper amount of 20 mmol/L phosphoric acid buffer solution with the pH value of 7.3;
(2) detecting the open circuit potential of the carbon nano tube after potassium peroxodisulfate is added into the solution in the step (1), wherein the plateau value is 0.636V;
(3) and (2) detecting the current change before and after adding dimethyl phthalate into the solution in the step (1) by taking 0.636V as an initial potential, wherein the result shows that the current has no obvious change, and the delta I is about 0.
In this example, the concentration of dimethyl phthalate was 0.1 mmol/L, the concentration of carbon nanotubes was 0.1 g/L, and the concentration of potassium peroxodisulfate was 1.0 mmol/L.
FIG. 4 is a graph of the timing current before and after adding dimethyl phthalate to the carbon nanotube electrode at a potential of 0.636V; the results show that when the potential is 0.636V (i.e., simulating the potential of the carbon nanotubes after potassium peroxodisulfate is added), the current does not change significantly after the addition of dimethyl phthalate, indicating that no electron transfer and no degradation reaction occurs.
Table 3 shows the effect of different systems on dimethyl phthalate removal; the results show that the removal efficiency of dimethyl phthalate in 60 minutes by the potassium peroxodisulfate/carbon nanotube system is about 15.92% (wherein the adsorption removal effect is about 15.83%), which indicates that the carbon nanotubes and potassium peroxodisulfate can not perform the electron transfer process to oxidize the dimethyl phthalate.
TABLE 3 dimethyl phthalate removal effectiveness of different systems
Claims (10)
1. A method for measuring an electron transfer process in a carbon material activated persulfate system is characterized by comprising the following steps:
(1) fixing a carbon material on a glassy carbon electrode to form a three-electrode system and immersing the three-electrode system in a buffer solution;
(2) detecting the change of the open circuit potential on the surface of the carbon material when persulfate is added into the solution in the step (1), and recording the potential in a stable state as U;
(3) taking U obtained in the step (2) as an initial potential, recording the current passing through the carbon material before and after the electron-donating compound is added into the solution in the step (1), and respectively recording the average current as I1And I2；
(4) The current change value Δ I in step (3) is I2-I1When Δ I>When 0, electron transfer occurs, and when Δ I is larger, electron transfer is easier, and when Δ I is 0No electron transfer occurs in the system.
2. The method for determining an electron transfer process according to claim 1, wherein the carbon material in the step (1) is carbon nanotube, graphene, graphite powder, biochar, or activated carbon.
3. The method for determining an electron transfer process according to claim 1, wherein the three-electrode system in the step (1) is: the carbon material is fixed on the glassy carbon electrode to serve as a working electrode, the platinum electrode serves as a counter electrode, and the saturated calomel electrode serves as a reference electrode.
4. The method for detecting an electron transfer process according to claim 1, wherein the buffer in step (1) is a phosphate buffer and has a pH of 3 to 11.
5. The method for measuring an electron transfer process according to claim 1, wherein the persulfate in the step (2) is a peroxodisulfate or a peroxomonosulfate.
6. The method for determining an electron transfer process according to claim 5, wherein the peroxodisulfate is potassium peroxodisulfate, sodium peroxodisulfate or ammonium peroxodisulfate.
7. The method for measuring an electron transfer process according to claim 1, wherein the electron donor compound in the step (3) is a phenolic compound or an organic dye.
8. The method for measuring an electron transfer process according to claim 7, wherein the organic dye is an azo dye, an anthraquinone dye, or a triphenylmethane dye.
9. The method for determining an electron transfer process according to claim 7, wherein the phenolic compound is a compound having phenol as a basic structure and substituted with 1 to 5 identical or different substituents R at the ortho, meta or para positions, wherein the substituents R are methoxy, hydroxy, phenyl, halogen, nitro, carboxyl, ester, alkyl, amide or amino groups.
10. A method for judging an electron transfer process in an organic pollutant degradation process is characterized by comprising the following specific steps: when degradation treatment of an electron donor organic contaminant is performed by the carbon material activated persulfate system, the electron transfer difficulty level is determined by the method for measuring an electron transfer process according to claim 1.
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| CN107298477A (en) * | 2017-06-22 | 2017-10-27 | 武汉纺织大学 | A kind of method for being catalyzed organic pollution in persulfate degrading waste water |
| CN109047320A (en) * | 2018-09-04 | 2018-12-21 | 中冶华天工程技术有限公司 | The restorative procedure of organic polluted soil |
| CN109174154A (en) * | 2018-09-13 | 2019-01-11 | 浙江大学 | The application of antibiotic in a kind of doping modification method and degrading waste water of nitrogen carbide |
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