CN105293487A - Method for preparing modified activated carbon and capacitive deionization electrode - Google Patents
Method for preparing modified activated carbon and capacitive deionization electrode Download PDFInfo
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- CN105293487A CN105293487A CN201510617670.2A CN201510617670A CN105293487A CN 105293487 A CN105293487 A CN 105293487A CN 201510617670 A CN201510617670 A CN 201510617670A CN 105293487 A CN105293487 A CN 105293487A
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Abstract
The invention provides a method for preparing modified activated carbon. The method comprises the steps of mixing activated carbon with water, and obtaining a mixed material; carrying out ultrasonic treatment on the mixed material; carrying out ozone oxidation treatment; freezing under -18 to -20 DEG C; carrying out freezing and drying under -18 to -20 DEG C. According to the method for preparing the modified activated carbon and the capacitive deionization electrode, provided by the invention, the used raw material is the activated carbon, the cost is low, and the activated carbon can be conveniently and easily obtained; the prepared modified activated carbon has good hydrophilia and capacitive performance through simple ozonation treatment, and the modified activated carbon is suitable for a capacitive deionization technology; the modified activated carbon is used for an electrode material of the capacitive deionization technology, the desalting quantity and the desalting speed can be effectively increased, and a good application prospect is obtained.
Description
Technical field
The invention belongs to carbon material technical field of modification, particularly the preparation method of a kind of modified activated carbon and capacitive deionization electrode.
Background technology
In recent years, due to the water resources crisis grown with each passing day, capacitive deionization causes scientific circles and pays close attention to widely, and this technology also has application prospect very widely in technical fields such as biology, medical science.
Capacitive deionization (CDI) utilizes electrochemical method, uses porous carbon materials to realize the desalination of seawater for electrode.Desalination amount is an important parameter of capacitive deionization technique, is also the important indicator investigating commercial promise.Desalination amount, the i.e. quality of unit mass electrode materials absorption salinity.Current, the desalination energy of CDI is mainly improved by improving the wetting ability of electrode materials and capacitive property etc.When electrode surface contains hydrophilic functional groups, can improve the wetting ability of electrode, solution fully contacts with electrode surface, is conducive to the raising of electrode desalting efficiency; If but too high levels, the electroconductibility of electrode can be reduced, the generation that simultaneously electrode electro Chemical also may be caused to react, these all can be able to have a negative impact to the desalting efficiency of electrode, and the kind and the capacitive deionization performance of content to electrode that therefore control material surface functional group also have a significant impact.
Electrode materials is the key components of CDI, and the performance of electrode materials directly decides the desalination amount of battery, desalination speed and stability.At present, what be widely used in CDI electrode most is carbon material, because they have remarkable chemistry, machinery and thermostability, and adjustable electrical property.Carbon material because of raw material different with preparation method, surface can containing different functional group, and the kind of these functional groups and content all can have an impact to the wetting property of solution and electrode stability.
The study hotspot of capacitance present deionization desalination electrode material focuses mostly in the novel charcoal material of charcoal-aero gel, carbon nanotube and these excellent propertys of Graphene, though oneself obtains encouraging progress, but because these type materials are also in phase of basic research, preparation technology is not perfect, be difficult to preparation in enormous quantities, the shortcomings such as therefore to there is preparation cost high for the Carbon Materials of these novelties, underproduce, constrain the application of capacitive deionization technology commercialization.
Summary of the invention
The invention provides a kind of preparation method of modified activated carbon.The method preparation technology is simple, and the modified activated carbon prepared by ozonation treatment has good hydrophilicity and capacitive property, enhances the wettability of electrode material surface, can effectively raise desalination amount and the desalination speed of capacitive deionization technique.Realize especially by following technical scheme: a kind of preparation method of modified activated carbon, comprises the following steps:
(1) gac is mixed with water, obtain mixture;
(2) by described mixture supersound process;
(3) mixture after step (2) being processed carries out ozone Oxidation Treatment;
(4) mixture after step (3) being processed is freezing at-18 DEG C ~-20 DEG C;
(5) the mixture lyophilize at-18 DEG C ~-20 DEG C after step (4) being processed.
As preferred technical scheme, total pore volume of described gac is 0.95-1.05cm
3/ g.
As preferred technical scheme, the specific surface area of described gac is: 1800-2200m
2/ g.
As preferred technical scheme, described ozone oxidation take oxygen as source of the gas.
As preferred technical scheme, in described ozone oxidation process, gas flow is 0.15 ~ 0.2Nm
2/ h, ozone concn is 100 ~ 130mg/L, and yield of ozone is 9 ~ 10g/h, and temperature is set to 25 DEG C; The time of oxygen oxidation is 50min.
As preferred technical scheme, described supersound process 10 ~ 20min, freezing time is 2 ~ 4h, and sublimation drying is 72 ~ 96h.
As preferred technical scheme, described gac and water ratio are 3 ~ 4:200-300g/ml.
The present invention also provides above-mentioned any preparation method the modified activated carbon obtained.
The present invention also provides capacitive deionization technology electrode, comprises any one modified activated carbon above-mentioned.
The present invention also provides the complete processing of above-mentioned capacitive deionization technology electrode, described modified activated carbon is prepared into electrode slice and rubber sheet gasket, lucite spacer and non-woven fabrics are assembled into capacitive deionization modular unit.The capacitive deionization modular unit obtained and peristaltic pump, D.C. regulated power supply, conductivity measurement composition capacitive deionization system are used for brackish water desalination, on-line monitoring conductivity variations.
Further, in technique scheme, described capacitive deionization systemic circulation more than 30 times, in each circulation, the adsorption and desorption time is 1200s.
Invention beneficial effect is: the present invention is raw materials used for gac, cheap, is easyly easy to get; The present invention is by simple ozonation treatment, and the modified activated carbon prepared has good wetting ability and capacitive property, is well suited for for capacitive deionization technology; Modified activated carbon is used for the electrode materials of capacitive deionization technology, effectively can improve desalination amount and desalination speed, have a good application prospect.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the modified activated carbon (ACO) prepared of the present invention and initial activity charcoal (AC);
Fig. 2 is the infrared absorpting light spectra of the modified activated carbon (ACO) prepared of the present invention and initial activity charcoal (AC);
Fig. 3 is the graph of pore diameter distribution that the modified activated carbon (ACO) prepared of the present invention and initial activity charcoal (AC) are measured by physical adsorption appearance;
Fig. 4 is the CV figure of the modified activated carbon (ACO) prepared of the present invention and initial activity charcoal (AC);
Fig. 5 is capacitive deionization modular unit;
Fig. 6 is capacitive deionization test macro;
Fig. 7 be the embodiment of the present invention 1,2,3,4 prepare modified activated carbon (ACO) and initial gac (AC) for capacitive deionization technology, concentration curve figure under voltage is 1.2V;
Fig. 8 be the embodiment of the present invention 1,2,3,4 prepare modified activated carbon (ACO) and initial gac (AC) for capacitive deionization technology, concentration curve figure under voltage is 1.0V;
Fig. 9 be the embodiment of the present invention 1,2,3,4 prepare modified activated carbon (ACO) and initial gac (AC) for capacitive deionization technology, concentration curve figure under voltage is 0.8V;
Figure 10 be the embodiment of the present invention 1,2,3,4 prepare modified activated carbon (ACO) and initial gac (AC) for capacitive deionization technology, concentration curve figure under voltage is 0.6V;
Figure 11 be the embodiment of the present invention 1,2,3,4 prepare modified activated carbon (ACO) and initial gac (AC) for desalination discharge curve figure under the different voltages of capacitive deionization technology.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but the present invention is not limited to this.
Embodiment 1
With gac be raw material by the simple and quick preparation realizing modified activated carbon of ozone Oxidation Treatment, and use it for capacitive deionization effect, comprise the steps:
(1) be 2000m by 3.5g specific surface area
2/ g, total pore volume is 1cm
3the gac of/g mixes with 250mL water, is prepared into black and is suspended mixture, described mixture is placed in supersound process 15min at 300w Ultrasonic Cleaners 25 DEG C ~ 30 DEG C;
(2) mixture that step (1) obtains is carried out ozone Oxidation Treatment, be source of the gas with oxygen in ozone oxidation process, gas flow is 0.2Nm
2/ h, ozone concn is 100-130mg/L, and yield of ozone is 10g/h, and temperature is set to 25 DEG C, and the time of ozone oxidation is 50min;
(3) mixture step (2) obtained is freezing at-18 ~-20 DEG C, puts into the dry 84h of freeze drier of-19 DEG C, obtain black powder after freezing;
(4) black powder that step (3) obtains is mixed with the ratio of 8:1:1 with carbon black, binding agent in N-N-dimethyl-ethylenediamine, be stirred to evenly;
(5) the mixture coating device that step (4) obtains stirring is coated on collector graphite flake, at room temperature dry 2h, puts into the dry 24h of loft drier of 80 DEG C;
(6) the electrode slice rubber sheet gasket of drying, lucite spacer and non-woven fabrics barrier film are forced together in order, be screwed, be prepared into complete capacitive deionization modular unit deionized water and wash 24h under the flow velocity of 9mL/min.
(7) battery washed is used for desalinating process, voltage is 1.2V, and circulation fluid is 50mL, and flow velocity is 5mL/min, and circulate more than 30 times at 25 DEG C, each circulation absorption and desorption time are 1200s.
The data of the conductivity variations of electrochemical workstation on-line monitoring in step (7) are processed, obtains concentration and desalination amount.
The present embodiment modified activated carbon (ACO) and initial activity charcoal (AC) carry out the concentration curve of capacitive deionization effect as Fig. 7 for electrode.
Embodiment 2
With gac be raw material by the simple and quick preparation realizing modified activated carbon of ozone Oxidation Treatment, and use it for capacitive deionization effect, comprise the steps:
(1) be 2000m by 3.5g specific surface area
2/ g, total pore volume is 1cm
3the gac of/g mixes with 250mL water, is prepared into black and is suspended mixture, described mixture is placed in supersound process 15min at 300w Ultrasonic Cleaners 25 DEG C ~ 30 DEG C;
(2) mixture that step (1) obtains is carried out ozone Oxidation Treatment, be source of the gas with oxygen in ozone oxidation process, gas flow is 0.2Nm
2/ h, ozone concn is 100-130mg/L, and yield of ozone is 10g/h, and temperature is set to 25 DEG C, and the time of ozone oxidation is 50min;
(3) mixture step (2) obtained is freezing at-18--20 DEG C, puts into the dry 84h of freeze drier of-19 DEG C, obtain black powder after freezing;
(4) black powder that step (3) obtains is mixed with the ratio of 8:1:1 with carbon black, binding agent in N-N-dimethyl-ethylenediamine, be stirred to evenly;
(5) the mixture coating device that step (4) obtains stirring is coated on collector graphite flake, at room temperature dry 2h, puts into the dry 24h of loft drier of 80 DEG C;
(6) the electrode slice rubber sheet gasket of drying, lucite spacer and non-woven fabrics barrier film are forced together in order, be screwed, be prepared into complete capacitive deionization modular unit deionized water and wash 24h under the flow velocity of 9mL/min.
(7) battery washed is used for desalinating process, voltage is 1.0V, and circulation fluid is 50mL, and flow velocity is 5mL/min, and circulate more than 30 times at 25 DEG C, each circulation absorption and desorption time are 1200s.
The data of the conductivity variations of electrochemical workstation on-line monitoring in step (7) are processed, obtains concentration and desalination amount.
The present embodiment modified activated carbon (ACO) and initial activity charcoal (AC) carry out the concentration curve of capacitive deionization effect as Fig. 8 for electrode.
Embodiment 3
With gac be raw material by the simple and quick preparation realizing modified activated carbon of ozone Oxidation Treatment, and use it for capacitive deionization effect, comprise the steps:
(1) be 2000m by 3.5g specific surface area
2the total pore volume of/g is 1cm
3the gac of/g mixes with 250mL water, is prepared into black mixture material, described mixture is placed in supersound process 15min at 300w Ultrasonic Cleaners 25 DEG C ~ 30 DEG C;
(2) mixture that step (1) obtains is carried out ozone Oxidation Treatment, be source of the gas with oxygen in ozone oxidation process, gas flow is 0.2Nm
2/ h, ozone concn is 100-130mg/L, and yield of ozone is 10g/h, and temperature is set to 25 DEG C, and the time of ozone oxidation is 50min;
(3) mixture step (2) obtained is freezing at-18--20 DEG C, puts into the dry 84h of freeze drier of-19 DEG C, obtain black powder after freezing;
(4) black powder that step (3) obtains is mixed with the ratio of 8:1:1 with carbon black, binding agent in N-N-dimethyl-ethylenediamine, be stirred to evenly;
(5) the mixture coating device that step (4) obtains stirring is coated on collector graphite flake, at room temperature dry 2h, puts into the dry 24h of loft drier of 80 DEG C;
(6) the electrode slice rubber sheet gasket of drying, lucite spacer and non-woven fabrics barrier film are forced together in order, be screwed, be prepared into complete capacitive deionization modular unit deionized water and wash 24h under the flow velocity of 9mL/min.
(7) battery washed is used for desalinating process, voltage is 0.8V, and circulation fluid is 50mL, and flow velocity is 5mL/min, and circulate more than 30 times at 25 DEG C, each circulation absorption and desorption time are 1200s.
The data of the conductivity variations of electrochemical workstation on-line monitoring in step (7) are processed, obtains concentration and desalination amount.
The present embodiment modified activated carbon (ACO) and initial activity charcoal (AC) carry out the concentration curve of capacitive deionization effect as Fig. 9 for electrode.
Embodiment 4
With gac be raw material by the simple and quick preparation realizing modified activated carbon of ozone Oxidation Treatment, and use it for capacitive deionization effect, comprise the steps:
(1) be 2000m by 3.5g specific surface area
2/ g, total pore volume is 1cm
3the gac of/g mixes with 250mL water, is prepared into black mixture material, described mixture is placed in supersound process 15min at 300w Ultrasonic Cleaners 25 DEG C ~ 30 DEG C;
(2) mixture that step (1) obtains is carried out ozone Oxidation Treatment, be source of the gas with oxygen in ozone oxidation process, gas flow is 0.2Nm
2/ h, ozone concn is 100-130mg/L, and yield of ozone is 10g/h, and temperature is set to 25 DEG C, and the time of ozone oxidation is 50min;
(3) mixture step (2) obtained is freezing at-18--20 DEG C, puts into the dry 84h of freeze drier of-19 DEG C, obtain black powder after freezing;
(4) black powder that step (3) obtains is mixed with the ratio of 8:1:1 with carbon black, binding agent in N-N-dimethyl-ethylenediamine, be stirred to evenly;
(5) the mixture coating device that step (4) obtains stirring is coated on collector graphite flake, at room temperature dry 2h, puts into the dry 24h of loft drier of 80 DEG C;
(6) the electrode slice rubber sheet gasket of drying, lucite spacer and non-woven fabrics barrier film are forced together in order, be screwed, be prepared into complete capacitive deionization modular unit deionized water and wash 24h under the flow velocity of 9mL/min.
(7) battery washed is used for desalinating process, voltage is 0.6V, and circulation fluid is 50mL, and flow velocity is 5mL/min, and circulate more than 30 times at 25 DEG C, each circulation absorption and desorption time are 1200s.
The data of the conductivity variations of electrochemical workstation on-line monitoring in step (7) are processed, obtains concentration and desalination amount.
The present embodiment modified activated carbon (ACO) and initial activity charcoal (AC) carry out the concentration curve of capacitive deionization effect as Figure 10 for electrode.
Embodiment 1-4 is characterized:
Scanning electron microscope is utilized to investigate the structural changes situation of the modified activated carbon prepared by embodiment 1,2,3,4, as shown in Figure 1, structurally significantly do not distinguished with raw material gac (a) by the modified activated carbon (b) of ozonize, the structure not changing material through ozonize is described.
Physical adsorption appearance is utilized to investigate pore size distribution and the specific surface area situation of the modified activated carbon prepared by embodiment 1,2,3,4, as shown in Figure 2, significantly do not distinguished on pore size distribution and accumulation specific surface area by the modified activated carbon of ozonize and initial gac, illustrate after ozonize, do not change pore structure and the specific surface area of material.
Infrared visible spectrophotometer is utilized to investigate the surface functional group situation of the modified activated carbon prepared by embodiment 1,2,3,4, as shown in Figure 3, a characteristic peak has been there is at 1716 places by the modified activated carbon of ozonize, this is the characteristic peak of the C=O key of carboxyl, illustrate after ozonize, the oxygen-containing functional group on absorbent charcoal material surface increases, wetting ability improves, enhancing due to surface wettability adds electrode transmission performance, reduce the diffusion resistance that ion transmits in the electrodes, improve desalination speed.
Utilize three-electrode system to the chemical property of modified activated carbon prepared by embodiment 1,2,3,4, mainly capacitive property is studied, as shown in Figure 4, can find out, the electrical capacity of the absorbent charcoal material after ozonize increases, and illustrates that modified activated carbon has good capacitive property.
Claims (10)
1. a preparation method for modified activated carbon, is characterized in that comprising the following steps:
(1) gac is mixed with water, obtain mixture;
(2) by described mixture supersound process;
(3) mixture after step (2) being processed carries out ozone Oxidation Treatment;
(4) mixture after step (3) being processed is freezing at-18 DEG C ~-20 DEG C;
(5) the mixture lyophilize at-18 DEG C ~-20 DEG C after step (4) being processed.
2. preparation method according to claim 1, is characterized in that, total pore volume of described activated carbon is 0.95-1.05cm
3/ g.
3. preparation method according to claim 1, is characterized in that, the specific surface area of gac is: 1800-2200m
2/ g.
4. preparation method according to claim 1, is characterized in that, described ozone oxidation take oxygen as source of the gas.
5. preparation method according to claim 1, is characterized in that, in described ozone oxidation process, gas flow is 0.15 ~ 0.2Nm
2/ h, ozone concn is 100 ~ 130mg/L, and yield of ozone is 9 ~ 10g/h, and temperature is set to 25 DEG C; The time of oxidation is 50min.
6. preparation method according to claim 1, is characterized in that, described supersound process 10 ~ 20min, and freezing time is 2 ~ 4h, and sublimation drying is 72 ~ 96h.
7. preparation method according to claim 1, is characterized in that, described gac and water ratio are 3 ~ 4:200-300g/ml.
8. the modified activated carbon that obtains of claim 1-7 any one preparation method.
9. capacitive deionization technology electrode, is characterized in that, comprises modified activated carbon according to claim 7.
10. the complete processing of capacitive deionization technology electrode according to claim 8, is characterized in that, described modified activated carbon is prepared into electrode slice and rubber sheet gasket, lucite spacer and non-woven fabrics are assembled into capacitive deionization modular unit.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587052A (en) * | 2016-11-29 | 2017-04-26 | 东至县森茂炭业有限公司 | Preparation process of activated carbon special for water purification |
| CN111732165A (en) * | 2020-06-30 | 2020-10-02 | 东莞理工学院 | Asymmetric CDI desalination module and desalination method using same |
| CN113754021A (en) * | 2021-08-30 | 2021-12-07 | 南京公诚节能新材料研究院有限公司 | Method for preparing capacitive deionization electrode |
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| US20060223701A1 (en) * | 2001-02-26 | 2006-10-05 | Adrianov Michail N | Modified activated carbon for capacitor electrodes and method of fabrication thereof |
| CN102216213A (en) * | 2008-11-04 | 2011-10-12 | 唐纳森公司 | Custom water adsorption material |
| CN103739043A (en) * | 2013-09-06 | 2014-04-23 | 广西大学 | Particle electrode for photocatalytic three-dimensional electrode/electro-Fenton system and preparation method thereof |
| CN104817143A (en) * | 2015-04-05 | 2015-08-05 | 北京化工大学 | Ion exchange membrane composite multi-electrode capacitance adsorption desalting apparatus |
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2015
- 2015-09-23 CN CN201510617670.2A patent/CN105293487A/en active Pending
Patent Citations (4)
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| US20060223701A1 (en) * | 2001-02-26 | 2006-10-05 | Adrianov Michail N | Modified activated carbon for capacitor electrodes and method of fabrication thereof |
| CN102216213A (en) * | 2008-11-04 | 2011-10-12 | 唐纳森公司 | Custom water adsorption material |
| CN103739043A (en) * | 2013-09-06 | 2014-04-23 | 广西大学 | Particle electrode for photocatalytic three-dimensional electrode/electro-Fenton system and preparation method thereof |
| CN104817143A (en) * | 2015-04-05 | 2015-08-05 | 北京化工大学 | Ion exchange membrane composite multi-electrode capacitance adsorption desalting apparatus |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587052A (en) * | 2016-11-29 | 2017-04-26 | 东至县森茂炭业有限公司 | Preparation process of activated carbon special for water purification |
| CN111732165A (en) * | 2020-06-30 | 2020-10-02 | 东莞理工学院 | Asymmetric CDI desalination module and desalination method using same |
| CN111732165B (en) * | 2020-06-30 | 2022-04-08 | 东莞理工学院 | Asymmetric CDI desalination module and desalination method using same |
| CN113754021A (en) * | 2021-08-30 | 2021-12-07 | 南京公诚节能新材料研究院有限公司 | Method for preparing capacitive deionization electrode |
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