CN109867334A - The method and application of catalysed particulate electrode activation persulfate under electric field driven - Google Patents
The method and application of catalysed particulate electrode activation persulfate under electric field driven Download PDFInfo
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Abstract
The present invention relates to stain disease process fields, and in particular, to a kind of methods and applications of the catalysed particulate electrode activation persulfate under electric field driven.Activation persulfate method of the present invention is added to persulfate in untreated organic wastewater with difficult degradation thereby, waste water is passed into a manner of continuously is formed by three-dimensional electrochemical system filled with catalysed particulate electrode, activate persulfate, to realize the efficient degradation and removal of organic pollutant.This activation method is easy to operate, low energy consumption, reaction rate is fast, degradation efficiency is high, can efficient process organic wastewater with difficult degradation thereby.
Description
Technical field
The present invention relates to stain disease process fields, in particular it relates to the catalysed particulate electricity under a kind of electric field driven
The method that pole activates persulfate, for handling organic stain disease difficult to degrade.
Background technique
Based on potentiometric titrations (SO4) high-level oxidation technology be that one to grow up in recent years effectively goes
Except the emerging technology of persistent organic pollutants.It is applied widely due to having many advantages, such as oxidation-reduction potential height, pH, and
It can be with H2O or OH-Reaction generates hydroxyl radical free radical (OH), and receives significant attention.
SO4·-It can be generated by the method for activating persulfate.Persulfate ionize in water the over cure acid group of generation from
Sub- S2O8 2-, standard oxidationreduction potential E0=+2.01V (relative to standard hydrogen electrode) ,-O-O- key contained in molecule exist
It can be broken and (activate) under certain condition, generate the stronger SO of oxidability4 -·(E0=2.6~3.2V).Currently, common
Activation method has ultrasound, ultraviolet light, heat, alkali, active carbon and transition metal etc..However it is difficult to degrade to utilize these activation methods to remove
Organic pollutant, persulfate dosage are usually several times to more than ten times of organic pollutant, to pass through excessive SO4·-Come real
Existing organic pollutant effectively removes.The use of a large amount of persulfates leads in water outlet that sulfate concentration is excessively high, brings secondary dirt
Dye problem, to limit the utilization of these activation methods.Therefore, for reduce persulfate medicament dosage and possess more
It is necessary to find a kind of new activation method for efficient removal efficiency.
In recent years, electrochemical advanced oxidation technique is because the features such as easy to operate, degradation efficiency is high, is by Successful utilization to respectively
In kind organic stain disease processing difficult to degrade.It is a kind of novel electrochemical treatments technology, and wherein the application of mosaic electrode system is wide
It is general.It refers to the granular electrode between being filled in cathode-anode plate, since each particle becomes independent microelectrode, considerably increases
The active site of electrochemical reaction can be such that polluter is more effectively removed.
In view of the above problems, the present invention is the work of the electrochemical oxidation system that is constituted using mosaic electrode as persulfate
Change condition generates SO using the mosaic electrode activation persulfate of electric field driven supported catalyst4 -, and cooperate with electrocatalytic oxidation
The efficient degradation and removal of the OH of generation, Lai Shixian organic pollutant.
Summary of the invention
Therefore, the purpose of the present invention is to provide under a kind of electric field driven persulfate activation method and its application.
According to the present invention, the method and its application of persulfate activation are realized by following steps:
(1) between mosaic electrode material being filled in cathode-anode plate, three-dimensional electrode reactor system is formed；
(2) persulfate is added in untreated stain disease；
(3) stain disease in step (2) is passed through in 3 D electrode reactor with continuous stream mode；
(4) electric current is applied to anodic-cathodic, forms granule electrode and react electric field, carries out stain disease processing.
Further, anode described in above-mentioned steps (1) is ruthenium titanium electrode (RuO2/ Ti), cathode is Ti electrode (Ti), yin
The spacing of anode plate is 5~40cm.
Further, above-mentioned steps (1) mosaic electrode is cylindrical particle, and it is highly 2~7mm that diameter, which is 2~6mm,
Loading is 100~400kg/m3；Cobalt oxide, cobalt protoxide, one or more kinds of in zeroth order cobalt are loaded on mosaic electrode
Catalyst etc., the quality of load cobalt catalyst are 20~100mg/g active carbon.
Further, persulfate described in above-mentioned steps (2) is permonosulphuric acid potassium (KHSO5), permonosulphuric acid sodium
(NaHSO5), potassium persulfate (K2S2O8), sodium persulfate (Na2S2O8) one or more of mixture；Over cure
HSO in hydrochlorate5 -And S2O8 2-The total mol concentration of ion is 2~30mM.
Further, stain disease described in above-mentioned steps (2) is coking wastewater, dyeing waste water or landfill leachate raw water warp
Water outlet after crossing biochemical treatment, pH value are 4.0~10.0；COD (COD) concentration is≤500mg/L.
Further, the current density of above-mentioned steps (4) described pole plate is 0.5~15mA/cm2。
Further, in above-mentioned steps (4), hydraulic detention time of the stain disease in mosaic electrode bed be 10~
200min。
Further, active powdered carbon during the preparation process, is pressed mass body first by above-mentioned steps (1) described mosaic electrode
Product is immersed in the cobalt salt solution of 0.3~0.7mol/L of cobalt ions than 1:5~1:8 (g:L), and cobalt salt solution is by cobalt nitrate or sulfuric acid
Cobalt salt is formulated, and is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is pressed into quality with polyvinyl alcohol bonding agent
Volume ratio 1:1~1:2 (g:L) is uniformly mixed, and is prepared into particle, in N2In 450~800 DEG C of 1~6h of roasting under protection, obtain
Mosaic electrode；Or by the active powdered carbon after dipping first in N2In 450~800 DEG C of 1~6h of roasting under protection, then with polyvinyl alcohol
Bonding agent is uniformly mixed by mass volume ratio 1:1~1:2 (g:L), and is prepared into particle, and mosaic electrode is obtained after drying.
Persulfate activation method of the invention is to utilize the catalysed particulate electrode activation persulfate under electric field driven
Method, compared with original activation method, solve causes sulfate concentration in water outlet excessively high by the use of a large amount of persulfates
Brought secondary pollution problem.In the formation of catalysed particulate electrode reaction electric field, the particle of filling is all charged, and becomes independent
Microelectrode, accelerates mass transfer rate, on the one hand generates the hydroxyl radical free radical of many strong oxidizing properties；On the other hand, in persulfate
Contained-O-O- key can be broken under the driving of electric field, while cobalt is as work needed for the fracture of catalyst degradation-O-O- key
Change energy, to generate a large amount of potentiometric titrations；Two kinds of free radicals realize the Synergistic degradations of persistent organic pollutants with
Removal.Wherein, involved some reaction equations are as follows:
Activation persulfate method of the invention, has the following advantages that and technical effect outstanding:
(1) persulfate is adding less, and avoiding leads to sulfate concentration mistake in water outlet by the use of a large amount of persulfates
Secondary pollution problem brought by height；
(2) organic pollutant is high-efficient in degrading waste water, activates persulfuric acid using electric field and the driving of mosaic electrode joint
Salt increases the free radical generated in reaction system, can be with the persistent organic pollutants of efficient degradation waste water, chemical oxygen demand
The removal rate of amount (COD) all reaches 90% or more；
(3) activation method is easy to operate, and the material used is cheap and easy to get, so that the activation method has practical implementation
Feasibility；
(4) low energy consumption, runs under lower current condition, can activate persulfate and generate more free radical.
Specific embodiment
Embodiment 1
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.3mol/L by mass volume ratio 1:5 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is Nian Jie with polyvinyl alcohol
Agent is uniformly mixed by mass volume ratio 1:1.5 (g:L), and is prepared into particle, in N2In 600 DEG C of roasting 4h under protection, obtain
Grain electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 5cm, and 30g mosaic electrode material is filled out
It fills between pole plate, forms three-dimensional electrode reactor system；The potassium persulfate of 7mM is added to COD=300mg/L, pH=6.3's
In coking wastewater, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, forms grain
Sub-electrode reacts electric field, is 2mA/cm in current density2, hydraulic detention time be 40min under conditions of handled, 20min
Water outlet reaches stable afterwards, reaches 97.5% to the removal rate of COD.
Embodiment 2
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:6 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is Nian Jie with polyvinyl alcohol
Agent is uniformly mixed by mass volume ratio 1:1 (g:L), and is prepared into particle, in N2In 700 DEG C of roasting 3h under protection, particle is obtained
Electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 10cm, by 60g mosaic electrode material
It is filled between pole plate, forms three-dimensional electrode reactor system；The permonosulphuric acid sodium of 5mM is added to COD=200mg/L, pH=7.8
Coking wastewater in, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, is formed
Granule electrode reacts electric field, is 1.5mA/cm in current density2, hydraulic detention time be 20min under conditions of handled,
Water outlet reaches stable after 20min, reaches 98.4% to the removal rate of COD.
Embodiment 3
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.3mol/L by mass volume ratio 1:5 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；By the active powdered carbon after dipping first in N2In 700 DEG C under protection
1h is roasted, then is uniformly mixed with polyvinyl alcohol bonding agent by mass volume ratio 1:1 (g:L), and be prepared into particle, is obtained after drying
Mosaic electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 15cm, by 90g mosaic electrode material
It is filled between pole plate, forms three-dimensional electrode reactor system；The potassium persulfate of 10mM is added to COD=350mg/L, pH=
In 8.3 coking wastewater, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic,
It forms granule electrode and reacts electric field, be 3mA/cm in current density2, hydraulic detention time be 25min under conditions of handled,
Water outlet reaches stable after 20min, reaches 95.5% to the removal rate of COD.
Embodiment 4
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:7 (g:L), cobalt salt is molten
Liquid is formulated by sulfuric acid cobalt salt, is dried after active powdered carbon centrifugation；By the active powdered carbon after dipping first in N2In 700 DEG C under protection
1h is roasted, then is uniformly mixed with polyvinyl alcohol bonding agent by mass volume ratio 1:1.5 (g:L), and be prepared into particle, is obtained after drying
Obtain mosaic electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 20cm, by 120g mosaic electrode material
Between being filled in, three-dimensional electrode reactor system is formed；The permonosulphuric acid sodium of 7mM is added to COD=300mg/L, the coke of pH=6.3
Change in waste water, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, forms particle
Electrode reaction electric field is 2mA/cm in current density2, hydraulic detention time be 15min under conditions of handled, after 20min
Water outlet reaches stable, reaches 93.7% to the removal rate of COD.
Embodiment 5
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:7 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；By the active powdered carbon after dipping first in N2In 600 DEG C under protection
2h is roasted, then is uniformly mixed with polyvinyl alcohol bonding agent by mass volume ratio 1:1 (g:L), and be prepared into particle, is obtained after drying
Mosaic electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 30cm, by 180g mosaic electrode material
It is filled between pole plate, forms three-dimensional electrode reactor system；The permonosulphuric acid potassium of 7mM is added to COD=400mg/L, pH=7.3
Coking wastewater in, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, is formed
Granule electrode reacts electric field, is 2mA/cm in current density2, hydraulic detention time be 60min under conditions of handled,
Water outlet reaches stable after 20min, reaches 98.5% to the removal rate of COD.
Embodiment 6
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.7mol/L by mass volume ratio 1:8 (g:L), cobalt salt is molten
Liquid is formulated by sulfuric acid cobalt salt, is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is Nian Jie with polyvinyl alcohol
Agent is uniformly mixed by mass volume ratio 1:2 (g:L), and is prepared into particle, in N2In 700 DEG C of roasting 3h under protection, particle is obtained
Electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 25cm, by 150g mosaic electrode material
It is filled between pole plate, forms three-dimensional electrode reactor system；The sodium persulfate of 7mM is added to COD=250mg/L, pH=5.4
Coking wastewater in, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, is formed
Granule electrode reacts electric field, is 3mA/cm in current density2, hydraulic detention time be 20min under conditions of handled,
Water outlet reaches stable after 20min, reaches 97.5% to the removal rate of COD.
Embodiment 7
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:5 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；By the active powdered carbon after dipping first in N2In 600 DEG C under protection
2h is roasted, then is uniformly mixed with polyvinyl alcohol bonding agent by mass volume ratio 1:2 (g:L), and be prepared into particle, is obtained after drying
Mosaic electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 15cm, by 90g mosaic electrode material
It is filled between pole plate, forms three-dimensional electrode reactor system；The permonosulphuric acid potassium of 10mM is added to COD=100mg/L, pH=
In 9.3 coking wastewater, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic,
It forms granule electrode and reacts electric field, be 3mA/cm in current density2, hydraulic detention time be 10min under conditions of handled,
Water outlet reaches stable after 20min, reaches 96.1% to the removal rate of COD.
Embodiment 8
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:6 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is Nian Jie with polyvinyl alcohol
Agent is uniformly mixed by mass volume ratio 1:2 (g:L), and is prepared into particle, in N2In 600 DEG C of roasting 4h under protection, particle is obtained
Electrode.
It is anode by cathode, ruthenium titanium electrode of titanium net electrode, cathode-anode plate spacing is 5cm, and 30g mosaic electrode material is filled out
It fills between pole plate, forms three-dimensional electrode reactor system；The sodium persulfate of 9mM is added to COD=150mg/L, pH=7.1's
In coking wastewater, waste water is passed through in 3 D electrode reactor in a manner of continuously；Voltage is applied to anodic-cathodic, forms grain
Sub-electrode reacts electric field, is 2mA/cm in current density2, hydraulic detention time be 20min under conditions of handled, 20min
Water outlet reaches stable afterwards, reaches 98.5% to the removal rate of COD.
Comparative example
Active powdered carbon is immersed in the cobalt salt solution of cobalt ions 0.5mol/L by mass volume ratio 1:5 (g:L), cobalt salt is molten
Liquid is formulated by nitric acid cobalt salt, is dried after active powdered carbon centrifugation；Then the active powdered carbon after dipping is Nian Jie with polyvinyl alcohol
Agent is uniformly mixed by mass volume ratio 1:2 (g:L), and is prepared into particle, in N2In 600 DEG C of roasting 4h under protection, particle is obtained
Electrode.
The active carbon particle electrode material of active carbon particle electrode material, Supported Co is filled in cathode-anode plate reaction respectively
In device, three-dimensional electrode reactor system is formed, is anode by cathode, ruthenium titanium electrode of titanium net electrode；By COD=200mg/L, pH=
7.1 humic acid simulated wastewater is passed through reactor, hydraulic detention time 10min, cold in a manner of continuum micromeehanics
Under the conditions of, operation absorption 200min makes activated carbon adsorption humic acid reach saturation, then applies electric current, compares reality by table 1
It tests, after reaction operation 20min, water outlet reaches stable, measures the COD concentration value of water outlet.
1 mosaic electrode material of table is at different conditions to the comparison treatment effect of humic acid simulated wastewater
It is filled into three-dimensional reactor using two kinds of particles material as mosaic electrode, does not also add persulfate in no power
Under conditions of, the active carbon particle electrode of the homemade active carbon particle electrode in laboratory and load cobalt catalyst does not almost have waste water
There is treatment effect.When only adding persulfate, but in cold situation, the treatment effect of waste water is also very poor, illustrates without electricity
In the presence of, mosaic electrode can not activate persulfate.When being only powered, persulfate, the active carbon particle of Supported Co are not added
Electrode has obvious rising to the treatment effect of waste water, and the removal rate of COD has reached 65%, is much higher than the homemade active carbon in laboratory
Mosaic electrode material (28%), illustrates in the presence of having electric field, and the mosaic electrode of Supported Co has preferable treatment effect to waste water.When
Under conditions of adding persulfate again while energization, the treatment effect of the active carbon particle electrode material of Supported Co to humic acid
It is further promoted, is promoted to 98% by 65%, the processing much larger than the homemade active carbon particle electrode in laboratory to humic acid
Effect (is promoted to 43% from 28%), illustrates that Co catalysts have played important function；The active carbon particle of Supported Co at the same time
Electrode material much higher than the summation for being individually powered with individually adding persulfate condition, illustrates in electric field the treatment effect of waste water
Catalysed particulate electrode activation persulfate produces a large amount of potentiometric titrations under conditions of driving, and cooperates with electrocatalytic oxidation
The OH of generation realizes the efficient degradation and removal of organic pollutant.
Claims (7)
1. a kind of method of the catalysed particulate electrode activation persulfate under electric field driven, which is characterized in that the method packet
Include following steps:
(1) between mosaic electrode material being filled in cathode-anode plate, three-dimensional electrode reactor system is formed；
(2) persulfate is added in untreated stain disease；
(3) stain disease in step (2) is passed through in 3 D electrode reactor with continuous stream mode；
(4) voltage is applied to anodic-cathodic, forms granule electrode and react electric field, carries out stain disease processing.
2. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
In load has catalysis one or more kinds of in cobalt oxide, cobalt protoxide or zeroth order cobalt on mosaic electrode described in step (1)
Agent, the quality of load cobalt catalyst are 20~100mg/g active carbon.
3. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
It is 5~40cm in, the pole plate spacing of cathode described in step (1) and anode, the loading of catalysed particulate electrode is 100~
400kg/m3。
4. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
In persulfate described in step (2) is permonosulphuric acid potassium (KHSO5), permonosulphuric acid sodium (NaHSO5), potassium persulfate
(K2S2O8), sodium persulfate (Na2S2O8) one or more of mixture, HSO5 -And S2O8 2-The total moles of ion
Concentration is 2~30mM.
5. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
In, waste water described in step (2) is the water outlet of coking wastewater, dyeing waste water or landfill leachate raw water after biochemical treatment,
PH value is 4.0~10.0, and COD (COD) concentration is≤500mg/L.
6. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
In current density described in step (4) is 0.5~15mA/cm2。
7. the method for the catalysed particulate electrode activation persulfate under electric field driven according to claim 1, feature exist
In hydraulic detention time of step (4) the described stain disease in mosaic electrode bed is 10~200min.
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| CN114573153B (en) * | 2022-01-19 | 2023-12-19 | 中国科学院山西煤炭化学研究所 | Method for degrading salt-containing organic wastewater by activating persulfate through carbon electrode under electric field driving/pH regulation |
| CN115092992A (en) * | 2022-07-01 | 2022-09-23 | 广东工业大学 | Method for synergistic electric activation of peroxymonosulfate by trace cobalt and application |
| CN115092992B (en) * | 2022-07-01 | 2023-01-24 | 广东工业大学 | Method for synergistic electric activation of peroxymonosulfate by trace cobalt and application |
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