CN115286077A - Method for removing perfluorinated compounds in water by reversing electrocoagulation with different electrode materials - Google Patents

Method for removing perfluorinated compounds in water by reversing electrocoagulation with different electrode materials Download PDF

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Publication number
CN115286077A
CN115286077A CN202210929659.XA CN202210929659A CN115286077A CN 115286077 A CN115286077 A CN 115286077A CN 202210929659 A CN202210929659 A CN 202210929659A CN 115286077 A CN115286077 A CN 115286077A
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reversing
electrode materials
pfass
different
perfluorinated
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CN202210929659.XA
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Chinese (zh)
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刘洋
张晓丽
鲍佳
鲁桂林
张文凯
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Shenyang University of Technology
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Shenyang University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur

Abstract

The method for removing perfluorinated compounds in water by reversing electro-flocculation with different electrode materials comprises the following steps that perfluorinated compounds PFASs comprise perfluorinated sulfonic acid compounds PFSAs and perfluorinated carboxylic acid compounds PFCAs; completely and vertically immersing two metal electrodes which are arranged in parallel in PFASs solution of an electric flocculation reactor, and continuously stirring; a relay/clock relay and a digital direct current power supply are connected into a circuit to realize the reversing energization of the electrodes; adopting the mutual combination mode of three metal electrode materials of aluminum, iron and zinc, namely Fe-Fe, fe-Zn, fe-Al, al-Al, zn-Zn and Al-Zn combination; different electrode materials are alternately used as anodes in a reversing way to generate different metal cations, and nano-scale hydroxyl flocs with different properties and complex structures are formed in the solution; PFASs pollutants are removed by utilizing the synergistic adsorption of the flocs, and the three metal electrode materials are alternately used as cathodes to eliminate electrode passivation.

Description

Method for removing perfluorinated compounds in water by reversing electrocoagulation with different electrode materials
Technical Field
The invention belongs to the technical field of removing perfluorinated compounds in water, and particularly relates to a method for removing perfluorinated compounds (PFASs) in water by reversing electrocoagulation by adopting different electrode materials.
Background
Perfluorinated compounds (PFASs) consist of a carbon backbone completely surrounded by fluorine atoms, with terminal sulfonic or carboxylic acid groups, which have endocrine, reproductive, hepato, developmental and neurotoxic properties and are potentially carcinogenic. Because PFASs have C-F bonds with extremely strong bond energy in chemical structures, the PFASs have very strong physical and chemical stability and have the characteristics of high temperature resistance, hydrolysis resistance, photolysis resistance and biodegradation resistance. The electric flocculation treatment technology has the advantages of simple and convenient operation, high efficiency, low cost and the like and is highly advocated. However, in practical applications, long-term use of a single-material electrode can result in surface passivation, which causes problems of decreased efficiency of PFASs removal, long treatment time, and increased energy and material consumption.
Disclosure of Invention
The invention aims to: aiming at the technical defects of poor PFASs removing effect, long treatment time, high energy consumption and material consumption and the like in the prior art, the method for removing the perfluorinated compounds (PFASs) in water by reversing electrocoagulation by adopting different electrode materials is provided.
The technical scheme is as follows:
the method for removing perfluorinated compounds PFASs in water by reversing electro-flocculation of different electrode materials, wherein the PFASs comprise perfluorinated sulfonic acid compounds PFSAs and perfluorinated carboxylic acid compounds PFCAs;
completely and vertically immersing two metal electrodes which are arranged in parallel in a PFASs solution of an electric flocculation reactor, and continuously stirring; a relay/clock relay and a digital direct current power supply are connected into a circuit to realize the reversing energization of the electrodes;
adopting the mutual combination mode of three metal electrode materials of aluminum, iron and zinc, namely Fe-Fe, fe-Zn, fe-Al, al-Al, zn-Zn and Al-Zn combination; different electrode materials are alternately used as anodes in a reversing way to generate different metal cations, and nano-scale hydroxyl flocs with different properties and complex structures are formed in the solution; PFASs pollutants are removed by utilizing the synergistic adsorption of the flocs, and the three metal electrode materials are alternately used as cathodes to eliminate electrode passivation.
Further, the PFSAs and PFCAs are formulated at a concentration of 10. Mu.g/L to 100mg/L.
Further, the working range of the digital direct current power supply is current intensity: 0 to 3A, voltage: 0-30V;
further, the different electrode materials have a commutating alternative working voltage range of 6-14V (or a current density of 17.5-40 mA/cm) 2 ) The stirring speed is 200-1200rpm, the electrode spacing is 1-3cm, the reversing time is 5-30s, the pH range is 3-10, and NaCl electrolyte is 1-2g/L.
Compared with the prior art, the invention has the following advantages and effects:
the invention adopts the electric flocculation method that different electrode materials are used as the anode alternately in a reversing way, different metal cations can be generated, hydroxyl flocs with nanometer grade, different properties and complex structures are formed in the solution, and the synergistic adsorption effect of the flocs and the alternate cathode are utilized to eliminate the electrode passivation, thereby achieving the effects of high speed and efficiency of PFASs removal, convenient operation, low energy consumption and the like.
Drawings
FIG. 1 is a schematic diagram of the principles of the present invention;
FIG. 2 (a) is a diagram showing the effect of the different electrode materials of the invention on the removal of PFOA in water by reversing electroflocculation;
FIG. 2 (b) is a graph of energy consumption for removing PFOA in water by reversing electro-flocculation with different electrode materials according to the present invention;
FIG. 3 is a diagram showing the effect of the present invention on the electric flocculation treatment of PFOA at different voltage ranges;
FIG. 4 is a diagram showing the effect of the present invention on the electric flocculation treatment of PFOA at different rotation speed ranges;
FIG. 5 is a graph showing the effect of the present invention on PFOS treatment by electroflocculation at different current density ranges;
FIG. 6 is a diagram showing the effect of the present invention on PFOS treatment by electroflocculation at different reversing time ranges;
FIG. 7 is a diagram showing the effect of the present invention on the electric flocculation treatment of PFOS at different electrode spacing ranges;
FIG. 8 is a graph showing the effect of electrocoagulation on perfluorosulfonic acid contaminants in different pH ranges;
FIG. 9 is a graph showing the effect of electroflocculation treatment according to the present invention on different PFASs concentration ranges;
FIG. 10 (a) is a non-commutating Al electrode energy spectrum of the present invention;
FIG. 10 (b) is a scanning electron micrograph of a non-commutating Al electrode according to the present invention;
FIG. 10 (c) is a commutating Al electrode energy spectrum of the present invention;
FIG. 10 (d) is a scanning electron micrograph of a commutating Al electrode of the present invention;
fig. 10 (e) is a non-commutating Zn electrode energy spectrum of the present invention;
FIG. 10 (f) is a scanning electron micrograph of a non-commutating Zn electrode of the present invention;
FIG. 10 (g) is a commutating Zn electrode energy spectrum of the present invention;
FIG. 10 (h) is a scanning electron micrograph of a commutating Zn electrode of the present invention.
Detailed Description
The invention will be described in further detail with reference to the following drawings and specific examples, which are intended to be illustrative rather than limiting.
Referring to the attached figure 1, the method for removing perfluorinated compounds PFASs in water by reversing electro-flocculation with different electrode materials comprises perfluorosulfonic acid compounds PFSAs and perfluorocarboxylic acid compounds PFCAs; PFSAs and PFCAs are formulated at a concentration of 10. Mu.g/L to 100mg/L.
Completely and vertically immersing two metal electrodes which are arranged in parallel in PFASs solution of an electric flocculation reactor, and continuously stirring; a relay/clock relay and a digital direct current power supply are connected into a circuit to realize the reversing energization of the electrodes; the working range of the digital direct current power supply is current intensity: 0 to 3A, voltage: 0-30V;
adopting the mutual combination mode of three metal electrode materials of aluminum, iron and zinc, namely Fe-Fe, fe-Zn, fe-Al, al-Al, zn-Zn and Al-Zn combination; different electrode materials are alternately used as anodes in a reversing way to generate different metal cations, and nano-scale hydroxyl flocs with different properties and complex structures are formed in the solution; the synergistic adsorption of the flocs is utilized to remove PFASs pollutants, and the three metal electrodes are utilizedThe material is alternated as a cathode to eliminate electrode passivation. The range of the different electrode materials for the commutating alternate working voltage is 6-14V (or the current density is 17.5-40 mA/cm) 2 ) The stirring speed is 200-1200rpm, the electrode spacing is 1-3cm, the reversing time is 5-30s, the pH range is 3-10, and NaCl electrolyte is 1-2g/L.
Example 1
With reference to the attached figure 1-2 and the table 1, the PFOA concentration is 1mg/L, the voltage is 10V, the electrode spacing is 2cm, the stirring speed is 1000rmp, the NaCl concentration is 2g/L, and the period is reversed to 10s; measuring the concentration of perfluorooctanoic acid (PFOA) before and after the electric flocculation by liquid chromatography-mass spectrometry (HPLC-MS/MS); by adopting an Al-Zn two parallel electrodes (the size is 6.0 x 4.0 x 0.2 cm) reversing electrocoagulation method, the PFOA removal rate is 100.0 percent at 20min, which is greater than the traditional electrocoagulation removal effect (10-50min 10.6-96.7 percent); the energy consumption is 43.9kWh/kg, which is less than that of single electrode combinations such as Al-Al and Zn-Zn; compared with the Al-Al and Zn-Zn single electrode combination, the electrode loss can be saved by 20-60%.
Table 1 shows the consumption of the different electrode materials according to the invention during the electroflocculation
Figure BDA0003780282990000051
Example 2
With reference to the attached drawings 1-2, by adopting the conditions of the example 1 and adopting a Zn-Zn two parallel electrodes reversing electrocoagulation method, the PFOA removal rate is 95.4 percent at 20min, and the energy consumption is 51.5kWh/kg.
Example 3
With reference to the attached figures 1-2, the conditions of the example 1 are adopted, a Fe-Al two-parallel-electrode reversing electrocoagulation method is adopted, the PFOA removal rate is 91.3% at 20min, and the energy consumption is 48.4kWh/kg.
Example 4
With reference to the attached drawings 1-2, by adopting the conditions of the example 1 and adopting a Fe-Zn two-parallel-electrode reversing electrocoagulation method, the PFOA removal rate is 69.9 percent at 20min, and the energy consumption is 61.4kWh/kg.
Example 5
With reference to the attached drawings 1-2, by adopting the conditions of the embodiment 1 and adopting an Al-Al two-parallel-electrode reversing electroflocculation method, the PFOA removal rate is 19.4 percent at 20min, and the energy consumption is 214.8kWh/kg.
Example 6
With reference to the attached drawings 1-2, by adopting the conditions of the example 1 and adopting a Fe-Fe two-parallel-electrode reversing electrocoagulation method, the PFOA removal rate is 16.4 percent at 20min, and the energy consumption is 315.0kWh/kg.
Example 7
With reference to figure 3, two parallel electrodes of Al-Zn (size of 6.0 x 4.0 x 0.2 cm), PFOA concentration of 1mg/L, electrode spacing of 2cm, stirring speed of 1000rmp, naCl concentration of 2g/L, cycle switching of 10s, PFOA removal rate of 92.7% at 10min at voltage of 6V.
Example 8
With reference to FIG. 3, under the conditions of example 7, the PFOA removal rate at 10min at 14V was 95.4%.
Example 9
With reference to FIG. 4, two Al-Zn parallel electrodes (6.0 x 4.0 x 0.2cm in size), PFOA concentration of 1mg/L, voltage of 9V, electrode spacing of 2cm, naCl concentration of 2g/L, cycle reversal of 10s, stirring speed of 200, and PFOA removal rate of 78.2% at 10 min.
Example 10
With reference to FIG. 4, under the conditions of example 9, the PFOA removal rate at 10min was 94.4% at a stirring speed of 1200 rpm.
Example 11
With reference to FIG. 5, two parallel electrodes of Al-Zn (size of 6.0 x 4.0 x 0.2 cm), PFOS concentration of 2mg/L, electrode spacing of 2cm, stirring speed of 600rmp, naCl concentration of 2g/L, cycle reversal of 10s, and current density of 17.5mA/cm 2 In this case, the PFOS removal rate at 5min was 88.1%, and at 10min was 100.0%.
Example 12
With reference to FIG. 5, the current density was 40mA/cm under the conditions of example 11 2 In time, the PFOS removal rate can reach 100.0 percent at 5 min.
Example 13
With reference to figure 6, two parallel electrodes of Al-Zn (size 6.0 x 4.0 x 0.2 cm), PFOS concentration 2mg/L, electrode spacing 2cm, stirring speed600rmp, naCl concentration 2g/L, current density 25mA/cm 2 When the period is reversed to 5s, the PFOS removal rate at 10min is 90.8%.
Example 14
With reference to the attached figure 6, under the conditions of the embodiment 13, when the period is reversed to 10s, the PFOS removal rate at 10min is 100.0%.
Example 15
With reference to the attached figure 6, under the conditions of the example 13, when the period is reversed to be 30s, the PFOS removal rate at 10min is 99.2%.
Example 16
With reference to FIG. 7, two parallel electrodes of Al-Zn (size: 6.0 x 4.0 x 0.2 cm), PFOS concentration of 2mg/L, stirring speed of 600rmp, naCl concentration of 2g/L, cycle switching of 10s, current density of 25mA/cm 2 When the electrode spacing is 1 or 2 or 3cm, the PFOS removal rate can reach 100.0% at 10 min.
Example 17
With reference to FIG. 8, the removal rates of perfluorooctane sulfonic acid (PFOS), perfluorohexane sulfonic acid (PFHxS) and perfluorobutane sulfonic acid (PFBS) treated at 10min were 100.0%, 90.5% and 85.3%, respectively, at PFASs concentration of 1mg/L, voltage of 9V, electrode spacing of 2cm, stirring speed of 600rmp, naCl concentration of 1g/L, cycle switching of 10s and pH of 3.
Example 18
With reference to FIG. 8, under the conditions of example 17, the removal rates of PFOS, PFHxS and PFBS at 10min were 97.0%, 59.4% and 49.3%, respectively, at pH 10.
Example 19
With reference to FIG. 9, the removal rates of perfluorobutyric acid (PFBA), perfluorobutanesulfonic acid (PFBS), perfluorovaleric acid (PFPEA) and perfluorohexanoic acid (PFHxA) at 10min were 53.6%, 56.1%, 63.0% and 59.7%, respectively, for two parallel Al-Zn electrodes (6.0 x 4.0 x 0.2cm in size), 9V in voltage, 2cm in electrode spacing, a stirring speed of 600rmp, a NaCl concentration of 2g/L, a cycle reversal of 10s, a pH of 5, and a PFASs concentration of 10. Mu.g/L.
Example 20
With reference to FIG. 9, under the conditions of example 19, at a PFASs concentration of 100mg/L, the removal rates of PFBA, PFBS, PFPEA, PFHxA at 10min were 91.0%, 97.0%, 96.3% and 97.6%, respectively.
Example 21
With reference to fig. 10 (a) - (d), compared with the non-reversed energization, the oxygen content of the Al electrode material after reversal is reduced from 4.73% to 2.05%, and the electrical corrosion of the surface structure is lighter; with reference to fig. 10 (e) - (h), compared with the non-reversal energization, the reversal of the Zn electrode material reduces the oxygen content of the electrode from 18.9% to 6.66% after the reversal, and the galvanic corrosion of the surface structure is lighter. Namely, the periodic reversing electrocoagulation technology of different electrode materials can effectively slow down the passivation phenomenon.
The foregoing description shows and describes the preferred embodiments of the present invention, but as aforementioned, it is to be understood that the invention is not limited to the forms disclosed herein, and is not to be construed as excluding other embodiments, and that the invention is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (4)

1. The method for removing the perfluorinated compounds in the water by reversing electro-flocculation of different electrode materials is characterized by comprising the following steps: the perfluorinated compounds PFASs comprise perfluorinated sulfonic acid compounds PFSAs and perfluorinated carboxylic acid compounds PFCAs; completely and vertically immersing two metal electrodes which are arranged in parallel in PFASs solution of an electric flocculation reactor, and continuously stirring; a relay/clock relay and a digital direct current power supply are connected into a circuit to realize the reversing energization of the electrodes;
adopting the mutual combination mode of three metal electrode materials of aluminum, iron and zinc, namely Fe-Fe, fe-Zn, fe-Al, al-Al, zn-Zn and Al-Zn combination; different electrode materials are alternately used as anodes in a reversing way to generate different metal cations, and nano-scale hydroxyl flocs with different properties and complex structures are formed in the solution; PFASs pollutants are removed by utilizing the synergistic adsorption of the flocs, and the three metal electrode materials are alternately used as cathodes to eliminate electrode passivation.
2. The method for removing perfluorinated compounds in water by reverse electrocoagulation according to claim 1, wherein the method comprises the following steps: the preparation concentration of the PFSAs and the PFCAs is 10 mug/L-100 mg/L.
3. The method for removing perfluorinated compounds in water by reverse electrocoagulation according to claim 1, wherein the method comprises the following steps: the working range of the digital direct current power supply is current intensity: 0 to 3A, voltage: 0 to 30V.
4. The method for removing perfluorinated compounds in water by reverse electrocoagulation according to claim 1, wherein the method comprises the following steps: the different electrode materials have the reversing alternate working voltage range of 6-14V or the current density of 17.5-40mA/cm 2 The stirring speed is 200-1200rpm, the electrode spacing is 1-3cm, the reversing time is 5-30s, the pH range is 3-10, and NaCl electrolyte is adopted at a concentration of 1-2g/L.
CN202210929659.XA 2022-08-03 2022-08-03 Method for removing perfluorinated compounds in water by reversing electrocoagulation with different electrode materials Pending CN115286077A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN212832974U (en) * 2020-07-03 2021-03-30 沈阳工业大学 Double-chamber electric flocculation wastewater in-situ defluorination device
US20210395112A1 (en) * 2018-11-28 2021-12-23 The Texas A&M University System Reusable functionalized hydrogel sorbents for removing perfluoroalkyl and polyfluoroalkyl substances from aqueous solution
CN114180684A (en) * 2021-12-15 2022-03-15 南京工业大学 Device and method for treating perfluorinated compound wastewater through electrocatalysis-electrocoagulation cooperation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104944533A (en) * 2014-03-26 2015-09-30 北京师范大学 Concentration separation removal method of perfluorinated compounds
US20210395112A1 (en) * 2018-11-28 2021-12-23 The Texas A&M University System Reusable functionalized hydrogel sorbents for removing perfluoroalkyl and polyfluoroalkyl substances from aqueous solution
CN212832974U (en) * 2020-07-03 2021-03-30 沈阳工业大学 Double-chamber electric flocculation wastewater in-situ defluorination device
CN114180684A (en) * 2021-12-15 2022-03-15 南京工业大学 Device and method for treating perfluorinated compound wastewater through electrocatalysis-electrocoagulation cooperation

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Title
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