CN106277221B - A kind of high load carbon content active electrode preparation method - Google Patents
A kind of high load carbon content active electrode preparation method Download PDFInfo
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- CN106277221B CN106277221B CN201610727608.3A CN201610727608A CN106277221B CN 106277221 B CN106277221 B CN 106277221B CN 201610727608 A CN201610727608 A CN 201610727608A CN 106277221 B CN106277221 B CN 106277221B
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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
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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
- C02F2001/46133—Electrodes characterised by the material
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Abstract
The invention discloses a kind of high load carbon content active electrode preparation methods, take active carbon, crystal aluminum chloride, calcium carbonate by weight and uniformly mix；It takes by weight and adds sodium silicate and be uniformly mixed with deionized water, obtain active material slurry；Resulting active material slurry is coated uniformly on electrode base material, is placed at 50 DEG C -130 DEG C 2 hours dry；By after coating and dry electrode is placed in the atmosphere furnace of nitrogen protection, calcined 3 hours at 600 DEG C -900 DEG C；It impregnates 3 hours in hydrochloric acid solution, is rinsed with water later, it is dry, obtain high load carbon content active electrode.Active carbon is coated on electrode base material by electrode coating method of the present invention using inorganic binder；This method not only makes active carbon and electrode base material is stable is combined together, but also the too small problem of active carbon coated weight can be applied in actual production so that the chemical property of electrode significantly improves in very good solution electrode preparation.
Description
Technical field
The invention belongs to electrochemical field more particularly to a kind of high load carbon content active electrode preparation methods.
Background technique
As the important component of electrochemical appliance, stability and the chemical property of electrode determine that it is actually being answered
Value in.Wherein, activated carbon electrodes are widely used in the devices such as battery, capacitor, electrochemical desalting.Absorbent charcoal material
The chemical property of electrode is determined in the amount of electrode surface coating.So how to improve coating processes, increase absorbent charcoal material
Coated weight, obtain that chemical property is good, the high activated carbon electrodes of stability have highly important research significance and apply valence
Value.
For obtain can stable activated carbon electrodes used in practical applications, generally require using Carbon Materials as active matter
Matter bonding is coated in conductive substrate surface, it is desirable that obtained electrode firm stable can be used for a long time.Currently, being usually with poly-
Tetrafluoroethene gathers the organic binders such as inclined tetrafluoroethene, by certain technique by active carbon be coated to copper foil, aluminium foil, carbon paper,
Carbon cloth etc. is led on basal electrode surface.But the use of organic binder will increase the internal resistance of electrode, to reduce prepared electricity
The chemical property of pole；On the other hand, organic binder high temperature resistance is poor, is unable to satisfy the subsequent high temperature processing of carbon electrode；
It is of particular importance that the amount of active carbon coating is typically only several milligrams, and carrying capacity is lower, in practical application using organic binder
In can not play the maximal efficiencies of activated carbon electrodes, can not meet such as capacitor desalination practical application.
Existing activated carbon electrodes are typically all using organic binder by covering method, spraying hair preparation, but due to
The problems such as activated carbon supported amount for the electrode prepared using organic binder is small, poor water resistance, poor conductivity, so that active carbon
Electrode cannot be applied always in real life.
Summary of the invention
The purpose of the present invention is to provide a kind of high load carbon content active electrode preparation methods, it is intended to solve existing electrode system
Electrode material coated weight is small in standby technology, and carrying capacity is lower, can not play the maximal efficiency of activated carbon electrodes in practical applications, full
Foot not such as capacitor desalination practical application the problem of.
The invention is realized in this way a kind of high load carbon content active electrode, the high load carbon content active electrode is by weight
Amount part include: 60 parts -90 parts of active carbon, 5 parts -30 parts of sodium silicate, 5 parts -15 parts of crystal aluminum chloride, 1 part -10 parts of calcium carbonate,
1 part -5 parts of deionized water.
Further, the active carbon is -300 mesh of 20 mesh.
Another object of the present invention is to provide a kind of preparation method of high load carbon content active electrode, the preparations
Method the following steps are included:
Step 1: taking active carbon, crystal aluminum chloride, calcium carbonate by weight and uniformly mixing；It takes and adds by weight
Sodium silicate is uniformly mixed with deionized water, obtains active material slurry；
Step 2: the resulting active material slurry of step 1 is coated uniformly on electrode base material, it is placed in 50 DEG C -130 DEG C
Lower drying -4 hours 1 hour, the electrode after must coating；
Step 3: after step 2 is coated and dry electrode is placed in the atmosphere furnace of nitrogen protection, at 600 DEG C -900 DEG C
Calcining -4 hours 2 hours, obtains coated electrode plate；
Step 4: being impregnated -3 hours 0.5 hour in the hydrochloric acid solution of 0.5mol/L-2mol/L concentration, rushed later with water
It washes, dries at room temperature, obtain high load carbon content active electrode.
Further, the electrode base material are as follows: carbon paper or carbon cloth.
Another object of the present invention is to provide a kind of method for desalting seawater using the high load carbon content active electrode.
Another object of the present invention is to provide a kind of processing industrial wastewaters using the high load carbon content active electrode
Method.
Another object of the present invention is to provide a kind of purification domestic waters using the high load carbon content active electrode
Method.
Active carbon is coated on electrode base material by electrode coating method of the present invention using inorganic binder.It should
Method not only makes active carbon and electrode base material is stable is combined together, but also active carbon in very good solution electrode preparation
The too small problem of coated weight can be applied in actual production so that the chemical property of electrode significantly improves；Add in filler
Calcium carbonate is entered, with that can generate bubble after salt acid soak, to generate hole on active carbon layer surface, this is conducive to the infiltration of liquid
Enter, improve absorbent charcoal material because stacking too closely difficult the phenomenon that being contacted with liquid, allow more materials in electricity
It plays a role in chemical process, further improves the chemical property of electrode.Method of the invention is simple, easy to operate, institute
There is process that can realize automation, time and the efficiency of electrode preparation can be improved；Utilize method active carbon of the invention
Coated weight can achieve 40mg/cm2.The present invention utilizes inorganic binder, and activated carbon supported amount is greatly improved, and utilizes knot
The problem of reacting between brilliant aluminium chloride and waterglass, very good solution poor water resistance.Due to inorganic bond can with high temperature resistant,
Active carbon is under inert gas protection after high-temperature calcination, so that the functional group of activated carbon surface largely reduces, to greatly mention
The high conductivity of activated carbon electrodes.Sea water desalination, processing industrial wastewater, purification domestic water etc. are main at present using anti-
Osmosis, electroosmose process and ion-exchange, but the drawback of these methods maximum is exactly higher cost, if prepared by the present invention
High load carbon content active application of electrode in these aspect, using CDI technology, the cost of water process will be substantially reduced.The present invention
The cyclic voltammetry curve for the electrode 1 that embodiment 1 is prepared illustrates that its internal resistance of the electrode material is relatively small close to rectangle, and
Charging current can be rapidly reached maximum value when applying backward voltage.And with the increase of sweep speed, the area of rectangle
It becomes larger, and can still keep rectangular shape in high sweep speed 0.2V/S.Illustrate when applying backward voltage, charging electricity
Stream can be rapidly reached maximum value, and ion still can be in electrode material quick adsorption and desorption under high scanning speed.
The cyclic voltammetry curve for the electrode 2 that the embodiment of the present invention 2 is prepared illustrates that its internal resistance of the electrode material is opposite close to rectangle
It is small, and charging current can be rapidly reached maximum value when applying backward voltage.And with the increase of sweep speed, rectangle
Area become larger, and can still keep rectangular shape in high sweep speed 0.2V/S.Illustrate when applying backward voltage,
Charging current can be rapidly reached maximum value, and under high scanning speed ion still can in electrode material quick adsorption and
Desorption.The ordinate of the cyclic voltammetry curve of electrode 1 is twice of the ordinate of the cyclic voltammetry curve of electrode 2, i.e. electrode 1
Rectangular area is greater than the rectangular area of electrode 2, illustrates that the capacitor of electrode 1 is bigger.Coating processes are applied slurry with coating machine
Carbon paper surface is overlayed on, hydrone is reset and plays catalytic action to the condensation between adjacent silanol group when the temperature increases.Further
Heating, remaining hydrone promote the condensation of silanol group, and mutually dehydration association between Si-OH key, form Si-O-Si
Key.This is the curing system of the fabulous three-dimensional structure of water resistance.Na+And H+In closed state in three-dimensional structure film, water is met not
It is molten.Al3+Into being conducive to increase its cementing strength and water resistance in silicate sturcture so that electrode have better water resistance with
Mechanical strength.The process being sintered using activated carbon electrodes prepared by organic binder without this step.Technical effect: in indifferent gas
The lower calcining active carbon of body protection, to reduce the resistance of electrode, increases so that the functional group of activated carbon surface greatly reduces
Conductivity.The further bonding for promoting inorganic binder, enhances the mechanical strength of electrode；Another aspect and calcium carbonate reaction,
Activated carbon electrodes surface manufactures hole, so that electrolyte is easier to penetrate into electrode interior, increases active carbon and electrolyte
Contact area, so that chemical property improves.
Detailed description of the invention
Fig. 1 is high load carbon content active electrode preparation method flow chart provided in an embodiment of the present invention.
Fig. 2 is the desalination performance map of embodiment 1,2 provided in an embodiment of the present invention.
Fig. 3 is 1 cyclic voltammetry curve schematic diagram of embodiment provided in an embodiment of the present invention.
Fig. 4 is 2 cyclic voltammetry curve schematic diagram of embodiment provided in an embodiment of the present invention.
Fig. 5 is the electrode of embodiment 1 and embodiment 2 provided in an embodiment of the present invention in 0.5M Na Cl solution 0.05V s-1
Sweep the cyclic voltammetry curve schematic diagram under speed.
Fig. 6 is 40mg cm provided in an embodiment of the present invention-2Scanning electron microscope image (SEM) schematic diagram of electrode side.
Fig. 7 is 40mg cm provided in an embodiment of the present invention-2Scanning electron microscope image (SEM) schematic diagram of electrode side.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention uses inorganic binder, and active carbon carrying capacity is made to reach 100mg cm-2, do not fall off, good mechanical stability, electricity
Pole can high temperature resistant, be substantially reduced by the resistance of high-temperature process activated carbon electrodes, this method preparation activated carbon electrodes removing
Salt application advantage is obvious.
The present invention is in the proportion of active carbon different meshes；Sodium silicate binder, crystal aluminum chloride, the calcium carbonate used
In the proportion of deionized water；On the temperature and time of preliminarily dried；It is optimized on the temperature and time of high-temperature calcination.
Application principle of the invention is explained in detail with reference to the accompanying drawing.
The high load carbon content active electrode of the embodiment of the present invention, the raw material according to parts by weight include: the work of 20-300 mesh number
Property 60-90 parts of charcoal, 5-30 parts of sodium silicate, 5-15 parts of crystal aluminum chloride, 1-10 parts of calcium carbonate, 1-5 parts of deionized water.
The preparation method of high load carbon content active electrode provided in an embodiment of the present invention as shown in Figure 1:, including following step
It is rapid:
S101, active carbon, crystal aluminum chloride, calcium carbonate are uniformly mixed；Sodium silicate is added to mix with deionized water
Uniformly, active material slurry is obtained.
S102, active material slurry is coated uniformly on electrode base material, is placed at 50 DEG C -130 DEG C 1-4 hours dry.
S103, the electrode of preliminarily dried is placed in the atmosphere furnace of nitrogen protection, is calcined 2-4 hours at 600 DEG C -900 DEG C.
Obtain coated electrode plate.
S104, it impregnates 0.5-3 hours in the hydrochloric acid solution of 0.5mol/L-2mol/L concentration, is rinsed with water later, do
It is dry, obtain high load carbon content active electrode.
The electrode base material are as follows: carbon paper, carbon cloth.
Active carbon is coated on electrode base material by electrode coating method of the present invention using inorganic binder.It should
Method not only makes active carbon and electrode base material is stable is combined together, but also active carbon in very good solution electrode preparation
The too small problem of coated weight can be applied in actual production so that the chemical property of electrode significantly improves；
It joined calcium carbonate in filler, with bubble can be generated after salt acid soak, so that hole is generated on active carbon layer surface,
This is conducive to the infiltration of liquid, improve absorbent charcoal material because stacking too closely difficult the phenomenon that being contacted with liquid so that more
More materials can play a role in electrochemical process, further improve the chemical property of electrode.
This method equipment is simple, easy to operate, and all processes can realize automation, can be improved electrode preparation when
Between and efficiency.
It can achieve 40mg cm using the coated weight of method active carbon of the invention2。
Activated carbon electrodes surface；Surface uniform ground has hole appropriate, conducive to the infiltration of electrolyte.
40mg cm activated carbon electrodes: there is certain mechanical strength, buckling strength, water resistance and high temperature resistance.It can be with
It is prepared into arbitrary size.
40mg cm-1Activated carbon electrodes side: having certain thickness, and adjustable material different proportion adjusts electricity
The thickness of pole.
Application principle of the invention is explained in detail combined with specific embodiments below.
Embodiment 1:
A kind of high load carbon content active electrode, the raw material according to parts by weight include: 80 parts of active carbon, the sodium of 20-300 mesh number
10 parts of waterglass, 6 parts of crystal aluminum chloride, 3 parts of calcium carbonate, 1 part of deionized water.
A kind of preparation method of high load carbon content active electrode, comprising the following steps:
Active carbon, crystal aluminum chloride, calcium carbonate are uniformly mixed；Sodium silicate is added to be uniformly mixed with deionized water,
Obtain active material slurry.
Active material slurry is coated uniformly on electrode base material, is placed at 100 DEG C 2 hours dry.
The electrode of preliminarily dried is placed in the atmosphere furnace of nitrogen protection, is calcined 3 hours at 700 DEG C.
Obtain coated electrode plate.
It impregnates 3 hours in the hydrochloric acid solution of 0.5mol/L concentration, is rinsed with water later, it is dry, it is living to obtain high load amount
Property carbon resistance rod.
1 electrode difference of embodiment is swept under speed in cyclic voltammetry curve: the circulation for the electrode 1 prepared using the above method is lied prostrate
Peace curve illustrates that its internal resistance of the electrode material is relatively small close to rectangle, and charging current can be fast when applying backward voltage
Speed reaches maximum value.And with the increase of sweep speed, the area of rectangle is become larger, and in high sweep speed 0.2V
s-1When can still keep rectangular shape.Illustrate that charging current can be rapidly reached maximum value, Er Qie when applying backward voltage
Ion still can be in electrode material quick adsorption and desorption under high scanning speed.
Embodiment 2:
A kind of high load carbon content active electrode, the raw material according to parts by weight include: 60 parts of active carbon, the sodium of 20-300 mesh number
20 parts of waterglass, 5 parts of crystal aluminum chloride, 4 parts of calcium carbonate, 1 part of deionized water.
A kind of preparation method of high load carbon content active electrode, comprising the following steps:
Active carbon, crystal aluminum chloride, calcium carbonate are uniformly mixed；Sodium silicate is added to be uniformly mixed with deionized water,
Obtain active material slurry.
Active material slurry is coated uniformly on electrode base material, is placed at 130 DEG C 3 hours dry.
The electrode of preliminarily dried is placed in the atmosphere furnace of nitrogen protection, is calcined 4 hours at 800 DEG C.
Obtain coated electrode plate.
It impregnates 2 hours in the hydrochloric acid solution of 1mol/L concentration, is rinsed with water later, it is dry, obtain high load amount activity
Carbon resistance rod.
2 electrode difference of embodiment is swept under speed in cyclic voltammetry curve: the circulation for the electrode 1 prepared using the above method is lied prostrate
Peace curve illustrates that its internal resistance of the electrode material is relatively small close to rectangle, and charging current can be fast when applying backward voltage
Speed reaches maximum value.And with the increase of sweep speed, the area of rectangle is become larger, and in high sweep speed 0.2V
Rectangular shape can be still kept when s-1.Illustrate that, when applying backward voltage, charging current can be rapidly reached maximum value, and
Ion still can be in electrode material quick adsorption and desorption under high scanning speed.The vertical seat of the cyclic voltammetry curve of electrode 1
Mark is twice of the ordinate of the cyclic voltammetry curve of electrode 2, i.e. the rectangular area of electrode 1 is greater than the rectangular area of electrode 2,
Illustrate that the capacitor of electrode 1 is bigger.Fig. 2 is the desalination performance map of example 1,2 provided in an embodiment of the present invention.Fig. 3 is of the invention real
The 1 cyclic voltammetry curve schematic diagram of embodiment of example offer is provided.Fig. 4 is that 2 cyclic voltammetric of embodiment provided in an embodiment of the present invention is bent
Line schematic diagram.Fig. 5 is the electrode of embodiment 1 and embodiment 2 provided in an embodiment of the present invention in 0.5M Na Cl solution 0.05V
s-1Sweep the cyclic voltammetry curve schematic diagram under speed.Fig. 6 is 40mg cm provided in an embodiment of the present invention2The scanning electricity of electrode side
Mirror image (SEM) schematic diagram.Fig. 7 is 40mg cm provided in an embodiment of the present invention2The scanning electron microscope image (SEM) of electrode side
Schematic diagram.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of high load carbon content active electrode, which is characterized in that the high load carbon content active electrode includes: work by weight
Property 60 parts -90 parts of charcoal, 5 parts -30 parts of sodium silicate, 5 parts -15 parts of crystal aluminum chloride, 1 part -10 parts of calcium carbonate, 1 part of deionized water -
5 parts.
2. high load carbon content active electrode as described in claim 1, which is characterized in that the active carbon is -300 mesh of 20 mesh.
3. a kind of preparation method of high load carbon content active electrode as described in claim 1, which is characterized in that the preparation method
The following steps are included:
Step 1: taking active carbon, crystal aluminum chloride, calcium carbonate by weight and uniformly mixing；It takes by weight and adds sodium water
Glass is uniformly mixed with deionized water, obtains active material slurry；
Step 2: the resulting active material slurry of step 1 is coated uniformly on electrode base material, it is placed at 50 DEG C -130 DEG C and does
Dry -4 hours 1 hour, the electrode after must coating；
Step 3: being calcined at 600 DEG C -900 DEG C after step 2 is coated and dry electrode is placed in the atmosphere furnace of nitrogen protection
- 4 hours 2 hours, obtain coated electrode plate；
Step 4: being impregnated -3 hours 0.5 hour in the hydrochloric acid solution of 0.5mol/L-2mol/L concentration, it is rinsed with water later, room
The lower drying of temperature, obtains high load carbon content active electrode.
4. the preparation method of high load carbon content active electrode as claimed in claim 3, which is characterized in that the electrode base material
Are as follows: carbon paper or carbon cloth.
5. a kind of method for desalting seawater using high load carbon content active electrode as claimed in claim 1 or 2.
6. a kind of processing method for industrial waste water using high load carbon content active electrode as claimed in claim 1 or 2.
7. a kind of purification domestic water method using high load carbon content active electrode as claimed in claim 1 or 2.
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| JPS5376581A (en) * | 1976-12-20 | 1978-07-07 | Ibigawa Electric Ind Co Ltd | Method of producing arc carbon electrode bar |
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| KR102212322B1 (en) * | 2013-12-24 | 2021-02-03 | 삼성전자주식회사 | Electrode material for capacitive deionization, methods of producing the same and capacitive deionization apparatus including the same |
| CN103950917A (en) * | 2014-05-07 | 2014-07-30 | 北京理工大学 | Method for preparing porous carbon material |
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