CN106277231A - A kind of electrochemistry removes the method for heavy metal in liquid - Google Patents
A kind of electrochemistry removes the method for heavy metal in liquid Download PDFInfo
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- CN106277231A CN106277231A CN201610604718.0A CN201610604718A CN106277231A CN 106277231 A CN106277231 A CN 106277231A CN 201610604718 A CN201610604718 A CN 201610604718A CN 106277231 A CN106277231 A CN 106277231A
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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
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/006—Electrochemical treatment, e.g. electro-oxidation or electro-osmosis
-
- 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
- C02F2001/46138—Electrodes comprising a substrate and a coating
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/203—Iron or iron compound
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
Abstract
The invention discloses a kind of electrochemistry and remove the method for heavy metal in liquid, it comprises the following steps: 1) electrode active material, conductive agent, binding agent are mixed by the mass ratio of 50～100: 10～30: 5～20, ultrasonic 5～60min make slurry, coating on carbon paper, 60～90 DEG C of vacuum dryings make working electrode；2) being placed in the liquid containing heavy metal by above-mentioned working electrode, with bare carbon paper for electrode, saturated calomel electrode is that reference electrode forms three-electrode system, or with working electrode and bare carbon paper, electrode is formed two electrode systems, makes ultracapacitor；3) ultracapacitor is carried out discharge and recharge.The present invention can remove each heavy metal species in liquid efficiently, has removal capacity high, and speed is fast, and low cost is easy and simple to handle, advantages of environment protection.
Description
Technical field
The present invention relates to the minimizing technology of heavy metal ion in liquid, utilize ultracapacitor former more particularly to one
Reason electrochemistry removes heavy metal ion method in liquid.
Background technology
Heavy metal as one of major pollutants in water body and soil, derive from mineral mining, metallurgy, the use of coating,
Core and other commercial production etc. (Chem.Soc.Rev., 2013,42,3792-3807).Remove heavy metal mainly side in water at present
Method has chemical precipitation, ion exchange, membrane filtration, absorption, electrodialysis etc..Heavy metal in soil is mainly fixing by chemistry.But
These methods are restricted in the application owing to cost is high, complicated and adsorbance is low mostly.
Ultracapacitor is a kind of energy storage device between traditional capacitor and battery, with its power density height, fills
The electricity time is short and the feature such as has extended cycle life and receive much concern (Chem.Int.Ed., 2013,52,1882-1889).According to energy storage
Mechanism, can be divided into two classes: one is the electrochemical capacitor in double electrode layer that electrode and solution interface form electric double layer by ultracapacitor；
Two is redox fake capacitance between electroactive material in electrode and solution.It is a kind of based on electric double layer electricity that electric capacity removes (CDI)
Hold principle and remove salt (NaCl, MgCl in water2Deng) technology, electrode material is material with carbon element, and its advantage is that energy efficiency is high and become
This is low.It is preferable that electric capacity removes the removal effect to salt, and N doped graphene initially contains at NaCl for electric double layer capacitance electrode material
When amount is for 500mg/L, to Na+Removal amount is up to 21.0mg/g.Comparatively speaking, during fake capacitance discharge and recharge, electrode material aoxidizes
Also along with solion embedding in electrode material and abjection (Nature, 2008,7,845-854) while reduction.Cause
This, utilize fake capacitance to remove salt effect in water more notable.Be currently based on capacitor principle remove metal ion technology many should
For Na+、Mg2+、Ca2+Deng salt ion, and there is not been reported for the removal of heavy metal.
Fake capacitance electrode material is generally transition metal oxide, and modal have RuO2、MnO2、NiO、Co3O4Deng.MnO2
High with its theoretical specific capacity, abundance, production cost be low and environmental friendliness and be widely used in ultracapacitor.Additionally MnO2
Point-of-zero charge is relatively low, neutrallty condition heavy metal ion have stronger absorbability (Environ.Sci.Technol.,
2008,42,779-785), therefore the present invention selects MnO2Or the MnO of carbon nano-tube modification2As electrode material, for heavy metal
Removal.
Summary of the invention
It is an object of the invention to provide a kind of capacity height of removing, simple to operate, the electrochemistry of cleanliness without any pollution removes liquid
The method of middle heavy metal.
Method provided by the present invention comprises the following steps:
1) electrode active material, conductive agent, binding agent are mixed by the mass ratio of 50～100: 10～30: 5～20, ultrasonic
Processing 5～60min and make slurry, coat on carbon paper, 60～90 DEG C of vacuum dryings make working electrode；
2) by step 1) working electrode be placed in the liquid containing heavy metal, with bare carbon paper for electrode, saturated sweet
Mercury electrode is that reference electrode forms three-electrode system, or electrode is formed two electrode systems by working electrode and bare carbon paper,
Ultracapacitor is made with three-electrode system or two electrode systems；
3) ultracapacitor is carried out discharge and recharge.
Described electrode active material is Mn oxide or carbon nano tube modified Mn oxide, and described Mn oxide can be
Birnessite, Bu Saier ore deposit, lithiophorite, cryptomelane, todorokite, pyrolusite and draw any one of manganese ore etc..
Described conductive agent one in acetylene black, Super P, Super S；
Described binding agent is selected from Kynoar (PVDF), politef (PTFE), polyvinyl alcohol (PVA)
Kind；
Described discharge and recharge is constant current charge-discharge or constant voltage discharge and recharge or constant-resistance discharge and recharge.
Preferably, described electrode active material is carbon nano tube modified birnessite, and described conductive agent is acetylene black, institute
Stating binding agent is Kynoar.It is further preferred that described carbon nano tube modified birnessite, acetylene black, polyvinylidene fluoride
The mass ratio of alkene is 75: 15: 10.
Preferably, described discharge and recharge is constant current charge-discharge, and the electric current density of described constant current charge-discharge is 0.1～5A/g, phase
Potential window for reference electrode is-0.6～1.0V, and circulating cycle number is 30～60 times.
It is further preferred that the electric current density of described constant current charge-discharge is 0.1A/g, relative to the electrochemical window of reference electrode
Mouth is 0～0.9V, and circulating cycle number is 50 times.
The invention has the beneficial effects as follows: the Pb that the present invention can remove in water efficiently2+、Zn2+、Cd2+、Fe2+、Cu2+、Cr
(III,VI)、As(III,V)、Sr2+And Cs+Etc. each heavy metal species, it is also possible to remove the heavy metal in the environmental pollutions such as mud, tool
Having removal capacity high, speed is fast, and low cost is easy and simple to handle, advantages of environment protection.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 is to Pb in water2+Removal Capacity Plan.
Fig. 2 is that embodiment 2 is to Zn in water2+Removal Capacity Plan.
Fig. 3 is that embodiment 3 is to Cd in water2+Removal Capacity Plan.
Fig. 4 is that embodiment 4 is to Pb in water2+Removal Capacity Plan.
Fig. 5 is that embodiment 5 is to Pb in water2+Removal Capacity Plan.
Detailed description of the invention
Below by embodiment, the present invention is described in detail.
Embodiment 1
A kind of electrochemistry removes the method for heavy metal ion in liquid, comprises the following steps:
1) by carbon nano tube modified birnessite, acetylene black, Kynoar by the mass ratio mixing of 75: 15: 10, surpass
Slurry is made in sound 30min dispersion, coats on carbon paper, and 75 DEG C of vacuum dryings make working electrode；
2) above-mentioned working electrode is placed in containing Pb2+Water in, with bare carbon paper for electrode, saturated calomel electrode is ginseng
Form three-electrode system than electrode, make ultracapacitor；
3) (electric current density is 0.1A/g, relative to the electrochemical window of reference electrode ultracapacitor to carry out constant current charge-discharge
Mouth is 0～0.9V, and circulating cycle number is 50 times).Discharge and recharge detects Pb in solution after terminating2+Content, calculates removal amount.
The most carbon nano tube modified birnessite is the most homemade: 0.158gKMnO4With 0.05g carbon nanometer
Pipe adds 80mL reaction tube, adds 50mL water.Then reaction tube is placed in microwave synthesizer, power setting 250W, reaction temperature
Control is 120 DEG C, response time 10min, and reaction is centrifugal after terminating, washing of precipitate, dried prepared carbon nano tube modified water
Sodium manganese ore.
From fig. 1, it can be seen that Pb in solution2+When content is 200mg/L, unit mass birnessite is to Pb2+Removal amount is
280mg/g, along with Pb2+Content increases, and removal amount is also gradually increased, and works as Pb2+After content reaches 1800mg/L, removal amount base
This is stable, and maximum removal amount is 1520mg/g.
Embodiment 2
A kind of electrochemistry removes the method for liquid heavy metal ion, comprises the following steps:
1) birnessite, acetylene black, politef being mixed by the mass ratio of 80: 10: 10, ultrasonic 15min makes slurry
Material, coats on carbon paper, and 80 DEG C of vacuum dryings make working electrode；
2) above-mentioned working electrode is placed in containing Zn2+Water in, with bare carbon paper for electrode, saturated calomel electrode is ginseng
Form three-electrode system than electrode, make ultracapacitor；
3) (electric current density is 5A/g, relative to the potential window of reference electrode ultracapacitor to carry out constant current charge-discharge
For-0.6～1.0V, circulating cycle number is 50 times).Discharge and recharge detects Zn in solution after terminating2+Content, calculates removal amount.
As can be seen from Figure 2, Zn in solution2+When content is 350mg/L, unit mass birnessite is to Zn2+Removal amount is
320mg/g, along with Zn2+Content increases, and removal amount is also gradually increased, and works as Zn2+After content reaches 1400mg/L, removal amount base
This is stable, and maximum removal amount is 530mg/g.
Embodiment 3
A kind of electrochemistry removes the method for liquid heavy metal ion, comprises the following steps:
1) by carbon nano tube modified birnessite, Super P, polyvinyl alcohol by the mass ratio mixing of 70: 10: 20, surpass
Sound 15min makes slurry, coats on carbon paper, and 60 DEG C of vacuum dryings make working electrode；
2) above-mentioned working electrode is placed in containing Cd2+Water in, with bare carbon paper for electrode, saturated calomel electrode is ginseng
Form three-electrode system than electrode, make ultracapacitor；
3) (electric current density is 2A/g, relative to the potential window of reference electrode ultracapacitor to carry out constant current charge-discharge
Being 0～1.0V, circulating cycle number is 40 times).Discharge and recharge detects Cd in solution after terminating2+Content, calculates removal amount.
As can be seen from Figure 3, Cd in solution2+When content is 200mg/L, unit mass birnessite is to Cd2+Removal amount is
150mg/g, along with Cd2+Content increases, and removal amount is also gradually increased, and works as Cd2+After content reaches 1400mg/L, removal amount base
This is stable, and maximum removal amount is 900mg/g.
Embodiment 4
A kind of electrochemistry removes the method for liquid heavy metal ion, comprises the following steps:
1) carbon nano tube modified birnessite, Super S, Kynoar are mixed by the mass ratio of 50: 30: 20,
Slurry is made in ultrasonic 30min dispersion, coats on carbon paper, and 75 DEG C of vacuum dryings make working electrode；
2) above-mentioned working electrode is placed in containing Pb2+Water in, with bare carbon paper for electrode, saturated calomel electrode is ginseng
Form three-electrode system than electrode, make ultracapacitor；
3) (electric current density is 1A/g, relative to the potential window of reference electrode ultracapacitor to carry out constant current charge-discharge
For-0.6～0V, circulating cycle number is 30 times).Discharge and recharge detects Pb in solution after terminating2+Content, calculates removal amount.
As can be seen from Figure 4, Pb in solution2+When content is 200mg/L, unit mass birnessite is to Pb2+Removal amount is
190mg/g, along with Pb2+Content increases, and removal amount is also gradually increased, and works as Pb2+After content reaches 1850mg/L, removal amount base
This is stable, and maximum removal amount is 1100mg/g.
Embodiment 5
A kind of electrochemistry removes the method for liquid heavy metal ion, comprises the following steps:
1) carbon nano tube modified birnessite, Super S, Kynoar are mixed by the mass ratio of 60: 20: 20,
Slurry is made in ultrasonic 20min dispersion, coats on carbon paper, and 75 DEG C of vacuum dryings make working electrode；
2) above-mentioned working electrode is placed in containing Pb2+Water in, with bare carbon paper for electrode being formed two electrode systems, system
Become ultracapacitor；
3) (electric current density is 2A/g, relative to the potential window of reference electrode ultracapacitor to carry out constant current charge-discharge
Being 0～0.6V, circulating cycle number is 40 times).Discharge and recharge detects Pb in solution after terminating2+Content, calculates removal amount.
As can be seen from Figure 5, Pb in solution2+When content is 200mg/L, unit mass birnessite is to Pb2+Removal amount is
200mg/g, along with Pb2+Content increases, and removal amount is also gradually increased, and works as Pb2+After content reaches 1740mg/L, removal amount base
This is stable, and maximum removal amount is 1140mg/g.
Claims (5)
1. an electrochemistry removes the method for heavy metal in liquid, it is characterised in that comprise the following steps:
1) electrode active material, conductive agent, binding agent are mixed by the mass ratio of 50～100: 10～30: 5～20, supersound process
5～60min make slurry, coat on carbon paper, and 60～90 DEG C of vacuum dryings make working electrode；
2) by step 1) working electrode be placed in the liquid containing heavy metal, with bare carbon paper for electrode, saturated calomel electricity
Extremely reference electrode composition three-electrode system, or working electrode and bare carbon paper are formed two electrode systems to electrode, with three
Electrode system or two electrode systems make ultracapacitor；
3) ultracapacitor is carried out discharge and recharge,
Described electrode active material is Mn oxide or carbon nano tube modified Mn oxide；
Described conductive agent one in acetylene black, Super P, Super S；
Described binding agent one in Kynoar, politef, polyvinyl alcohol；
Described discharge and recharge is constant current charge-discharge or constant voltage discharge and recharge or constant-resistance discharge and recharge.
The method of heavy metal during the most according to claim 1, electrochemistry removes liquid, it is characterised in that: described electrode activity material
Material is carbon nano tube modified birnessite, described conductive agent is acetylene black, described binding agent is Kynoar.
The method of heavy metal during the most according to claim 2, electrochemistry removes liquid, it is characterised in that: described electrode activity material
Material, conductive agent, the mass ratio of binding agent are 75: 15: 10.
The method of heavy metal during the most according to claim 1, electrochemistry removes liquid, it is characterised in that: described discharge and recharge is permanent
Stream discharge and recharge, the electric current density of described constant current charge-discharge is 0.1～5A/g, relative to the potential window of reference electrode be-0.6～
1.0V, circulating cycle number is 30～60 times.
The method of heavy metal during the most according to claim 4, electrochemistry removes liquid, it is characterised in that: described constant current charge-discharge
Electric current density be 0.1A/g, be 0～0.9V relative to the potential window of reference electrode, circulating cycle number is 50 times.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179589A (en) * | 2018-09-20 | 2019-01-11 | 同济大学 | The preparation method of carbon coating vanadium phosphate sodium electrode material and its application in hydridization capacitive deionization technology |
| CN109678227A (en) * | 2019-01-29 | 2019-04-26 | 华中农业大学 | A kind of method of electrochemical reduction ferriferous oxide removal Heavy Metals in Waters anion contamination |
| CN110010373A (en) * | 2019-03-27 | 2019-07-12 | 中国科学院福建物质结构研究所 | A kind of embedding zinc processing method of electrode and its application in the preparation of cell type supercapacitor |
| CN114507786A (en) * | 2021-12-30 | 2022-05-17 | 中国科学院广州能源研究所 | Method for assisting dissociation, concentration and in-situ monitoring of low-concentration rare and precious rare earth elements of supercapacitor by using quantum dots |
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| CN103736724A (en) * | 2013-12-30 | 2014-04-23 | 贵州大学 | Method for removing polluted ions in water body or porous medium |
| CN103936116A (en) * | 2014-04-22 | 2014-07-23 | 中国科学院生态环境研究中心 | Manganese dioxide/carbon combined electrode and electric adsorption method for electrically adsorbing heavy metal ions from water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103736724A (en) * | 2013-12-30 | 2014-04-23 | 贵州大学 | Method for removing polluted ions in water body or porous medium |
| CN103936116A (en) * | 2014-04-22 | 2014-07-23 | 中国科学院生态环境研究中心 | Manganese dioxide/carbon combined electrode and electric adsorption method for electrically adsorbing heavy metal ions from water |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179589A (en) * | 2018-09-20 | 2019-01-11 | 同济大学 | The preparation method of carbon coating vanadium phosphate sodium electrode material and its application in hydridization capacitive deionization technology |
| CN109678227A (en) * | 2019-01-29 | 2019-04-26 | 华中农业大学 | A kind of method of electrochemical reduction ferriferous oxide removal Heavy Metals in Waters anion contamination |
| CN110010373A (en) * | 2019-03-27 | 2019-07-12 | 中国科学院福建物质结构研究所 | A kind of embedding zinc processing method of electrode and its application in the preparation of cell type supercapacitor |
| CN114507786A (en) * | 2021-12-30 | 2022-05-17 | 中国科学院广州能源研究所 | Method for assisting dissociation, concentration and in-situ monitoring of low-concentration rare and precious rare earth elements of supercapacitor by using quantum dots |
| CN114507786B (en) * | 2021-12-30 | 2023-06-09 | 中国科学院广州能源研究所 | Method for utilizing quantum dots to assist dissociation, concentration and in-situ monitoring of low-concentration diluted noble elements of supercapacitor |
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| CN106277231B (en) | 2019-03-19 |
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