CN106395814A - Preparation method of special activated-carbon electrode block for capacitive deionizing equipment - Google Patents
Preparation method of special activated-carbon electrode block for capacitive deionizing equipment Download PDFInfo
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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
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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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Abstract
The invention provides a preparation method of a special activated-carbon electrode block for capacitive deionizing equipment. Activated carbon powder, a binding agent, a carbon fiber, expanded graphite powder and conducting carbon black are loaded in a material box to be mixed; an obtained first mixture is agitated and mixed uniformly; the agitated and mixed first mixture is kneaded to be paste with plasticity; the well mixed paste is molded into a green compact in a fixed shape in molding equipment. The green compact is loaded in a heating furnace to be subjected to high-temperature calcination under the protection of a filling material; a primary product of the electric block is obtained. The primary product is made into an electrode according to the size, the shape and the precision needed by the electrode by adopting cutting machining. Finally, the activation treatment is carried out on the electrode; the electrode is made into a final product of the electrode. The method is low in preparation cost, and is easy for large-scale production. No binding agent resides in the electrode; the conductivity is good; the electrode is good in integrality and high in mechanical strength; the electrode can be cut to be in various needed shapes. The electrode can be used for preparing a capacitive deionizing device, and is used for the desalting treatment of water or the removal of harmful ions such as heavy metal ions, hardness, fluorine ions and the like in the water.
Description
Technical field
The present invention relates to field of waste water treatment, particularly to the preparation side of capacitive deionization device-specific activated carbon electrodes block
Method.
Background technology：
Also known as Electro Sorb technology (EST), its general principle is based on the electric double layer reason in electrochemistry to capacitive deionization (CDI)
By using the electrochemical properties on charged electrode surface, realizing the absorption of charged particle and removal, the decomposition of organic matter etc. in water
Purpose.CDI has that operating cost is low, need not add medicine, non-secondary pollution, to entering, water quality requirement is low, operation and maintenance is simple, de-
The advantages of salt rate is adjustable, Water Sproading rate high and equipment life is long.
Activated carbon (AC) has larger specific surface area and extraordinary chemical stability, is the most widely used at present
CDI electrode material, usual CDI electrode typically passes through molding by activated carbon, conductive agent (Graphon) and adhesive or is coated with
Make.Activated carbon, as carbon-based electrode material the most cheap, is the electrode material being hopeful to carry out large-scale industrial application most.But
Activated carbon electrodes resistance itself is excessive and there is the defects such as resistance to mass tranfer and limits its application.Additionally, carbon electrode generally existing
A fatal problem is to be unable to self-supporting to use as absolute electrode.Inevitably to bonding in making electrode process
The use of the materials such as agent, conductive agent and collector, these materials will block most of aperture of traditional material with carbon element, reduces
Current efficiency, the electrical conductivity of electrode is also affected, thus reducing desalting efficiency and adsorbance.
United States Patent (USP) (US 6787235B2) reports a kind of preparation method of unformed activated carbon agglomerated materials and its use
On the way, the activated carbon block being obtained through high temperature high pressure process can cut into the shape of needs, have high ratio electric capacity, can be used for electricity
Hold deionization technical field.But this kind of method is due to without conductive agent and binding agent, thus the electric conductivity of material and blockiness
It is not fine.
Chinese patent (CN101369492A) reports a kind of manufacture method of high-energy ratio super capacitance electrode material, will be many
Hole carbon, conductive agent and polytetrafluoroethylene (PTFE) are ground mixing, and then carry out high energy with roller and roll prepared combination electrode material.
The volume preparation method of this electrode material is simple, but the polytetrafluoroethylene (PTFE) binding agent mixing will block porous carbon duct, and drops
The electric conductivity of low electrode.
Chinese patent (CN105185599A) reports a kind of layer structure of porous carbon layer/graphene layer/porous carbon layer
Super capacitor carbon composite.Phenolic resin or biomass material are mixed with water, adds graphene oxide and inorganic or have
Machine amine, then obtain presoma through hydro-thermal method, finally again precursor heating is carried out high-temperature activation.The carbon composite of gained can use
In super capacitance electrode material, the capacity of super capacitor can be effectively improved.But the Graphene raw material that this kind of method uses is non-
Chang Anggui, and the mechanical strength of electrode composite material is not fine.
Chinese patent (CN105261490A) reports a kind of preparation method of battery capacitor electrode slurry, conductive agent, super
Level capacitance electrode material is added in the glue of binding agent, capacitance electrode slurries is obtained by mechanical agitation, and slurries pass through coating
Method can be prepared by electrode material.The volume preparation method of this electrode material is simple, but the polytetrafluoroethylene (PTFE) binding agent mixing
Porous carbon duct will be blocked.
Chinese patent (CN103570107A) reports a kind of preparation method of electrode material for electrosorption desalination, by activity
Carbon fibe powder and graphite are added in phenol resin solution, and prepared slurries, then by slurries compression molding, are then placed in electric furnace
Middle activation.The electrode material electric conductivity and all very better than electric capacity that this method is obtained.But the cost of NACF is too high,
And electrode material intensity is not good.
Content of the invention
It is an object of the present invention to provide big and higher than the electric capacity active carbon electrode block of a kind of good conductivity, specific surface area
Preparation method, binder free residual in electrode, electrode good integrity, high mechanical strength, the various required shape of cleavable one-tenth.
The technical solution used in the present invention is：
A kind of preparation method of capacitive deionization device-specific activated carbon electrodes block, methods described is：
Take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black be raw material, through mixing, shaping, roasting,
Machining, activation, are obtained described capacitive deionization device-specific activated carbon electrodes block；
Described activated carbon, binding agent, carbon fiber, expanded graphite powder, the mass fraction of conductive carbon black are active carbon powder 60
～90%, binding agent 8～25%, carbon fiber 0.5～2.5%, expanded graphite 1～10%, conductive black 2～10%.
Described activated carbon can be Active Carbon Based on Coal-tar Pitch powder, wood-based activated carbon powder, bamboo fiber-based activated carbon
Powder or shell base super capacitor special active carbon powder, particle diameter is 5～100 μm, specific surface area 1500～2000m2/g.
Described binding agent is coal tar pitch, humic acid sodium salt, polyethylene adjoin pyrrolidone, sodium cellulose glycolate, phenolic aldehyde tree
One of fat or polyvinyl butyral resin or two or more.The molecular weight of binding agent is less, and the blocking to activated carbon capillary is got over
Seriously；
Described carbon fiber is 5～10 μm of diameter, and length is the chopped carbon fiber of 1mm～100mm, and fiber surface does not contain upper
Slurry agent；
Described expanded graphite powder is generally 50～100 mesh.
Further, the method for the invention comprises the following steps：
(1) take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black to be raw material, obtain through hybrid technique
Thickener, described hybrid technique is wet blending process after kneading technique or dissolving；
(2) through moulding process, the raw embryo of prepared solid shape, described moulding process can adopt and is molded, extrudes, shaking thickener
Dynamic shaping or isostatic pressing process；
(3) raw embryo of solid shape, through high-temperature roasting, makes the binding agent in green compact carbonize, obtains electrode block head product；
Described sintering temperature is 850～1250 DEG C；
(4) the electrode block head product after roasting carries out machining, and described being machined in stock-removing machine is carried out, and adopts
With machining, the size being needed according to electrode, shape, precision make electrode to be activated；
(5) electrode to be activated carries out activating process, and described capacitive deionization device-specific activated carbon electrodes block is obtained；
In described step (1), described hybrid technique is pressed different binding agents and is adopted different mixed methods, and binding agent drips for coal
When green grass or young crops, phenolic resin, polyvinylpyrrolidone or polyvinyl butyral resin, mixed using kneading technique；Described binding agent
During for humic acid sodium salt, sodium cellulose glycolate or phenolic resin, mixed using wet blending process after dissolving, that is, first will be described
Binding agent solvent dissolves, and is then mixed with mixer with the siccative particle in addition to binding agent.
Further, described kneading technique includes two processes of dry blend wet mixing, is wherein dry mixed and carries out at normal temperatures, duration
For 20～35min, a length of 40～55min during wet mixing, operation temperature is higher than 50～80 DEG C of binding agent softening point, and not can exceed that viscous
The carburizing temperature of knot agent.
Further, described kneading technique preferably operates in accordance with the following methods：First the siccative particle in addition to binding agent is added
Enter kneading machine, under normal temperature in be dry mixed, be dry mixed the time be 20～35min, so that various raw materials is mixed, make different grains simultaneously
The solid carbonaceous material of degree size equably mixes and fills, and improves the packing of compound；Then add toward in kneading machine again
Binding agent, carries out wet mixing, and described binding agent is in coal tar pitch, phenolic resin, polyvinylpyrrolidone or polyvinyl butyral resin
One or more, wet mixing time 40～55min, temperature is higher than 50～80 DEG C of binding agent softening point, and not can exceed that viscous
The carburizing temperature of knot agent；During wet mixing, liquid adhesive even spread and infiltration particle surface, formed one layer of tack coat,
All materials are bonded to each other, and then form the plasticity thickener of homogeneous, are conducive to being molded.Meanwhile, portion of binder leaching
Thoroughly arrive carbonaceous material internal voids, further increase density and the caking property of thickener.Thickener after kneading carries out next step one-tenth
Type technique.
When described binding agent is humic acid sodium salt or sodium cellulose glycolate, using the hybrid technique of wet mixing after dissolving, institute
Stating technique is：Binding agent is added in the water of 10 times of quality, and adds the ethanol of the mass fraction 5～20% that quality is water,
Stir and dissolve to abundant, obtain binder solution, then the siccative particle in addition to binding agent is mixed with binder solution, adopt
Electric blender mixes.
When described binding agent is phenolic resin, can be mixed using kneading technique, also can be by phenolic resin solvent
After dissolving, mixed using wet blending process, described technique is specially：The phenolic resin ethanol of 10 times of quality is dissolved, so
Mix 1h with the siccative particle electric blender in addition to binding agent afterwards, adding quality is binding agent quality 6～10%
Curing agent, continues mixing 30～40min.Described curing agent can be methenamine.
In described step (2), described moulding process can be using molding, extruding, vibration moulding or isostatic pressing method, system
Become the raw embryo product of fixing proterties.Molding uses vertical hydraulic press, is generally used for preparing low-grade pellet electrode.Extrusion molding is adopted
With Horizontal hydraulic extruder or screw extruder.Vibration moulding adopts vibrating forming machine, can prepare that packing is good, and mechanical performance is excellent
Electrode block.Isostatic pressing adopts iso-static pressure shaping machine, and it is homogeneous to prepare Density Distribution, uniform texture, and density is high, burns
Knot shrinkage factor is little, complex-shaped, the good electrode of machining property.
Further, preferably moulding process is from extruding or isostatic pressing mode.Described extruding is preferably squeezed in carbon pole
Carry out in press, technique is：The thickener that step (1) is obtained is cooled to 90～120 DEG C) after, carry out successively feeding, precompressed and squeezing
Three processes of pressure.
Further, described charging process is point 2～3 blankings, then 4～10MPa compacting；Described pre-pressing process is：Pressure
Power 20～25MPa, time 3～5min, vacuumize simultaneously, are de-gassed；Described extrusion process is：Pressure is 5～15MPa, system
Obtaining isostatic pressing process described in bar-shaped or block shaping raw embryo is：The thickener that step (1) is obtained, after being cooled to 90～120 DEG C, fills out
It is charged in rubber mold, is vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, vacuumized after sealing, discharge powder
The air of intergranular.Then rubber mold is put in the high-pressure bottle equipped with liquid mediums such as water or oil, it is pressurized to 100～
200MPa, dwell time 10～20min, are pressed into cylinder or the shaping raw embryo of cuboid.
In described step (3), described high-temperature roasting one of inert atmosphere, ammonia atmosphere, vapor or both
Carry out under above mixed atmosphere, concrete technology is：Shaping raw embryo is carried out pre- carbonization treatment, with 2 DEG C/min's in electric furnace
Programming rate, is warmed up to 800～900 DEG C, and is incubated 1～2 hour；Then carry out high-temperature roasting, during roasting, a length of 1～2 is little
When, temperature is 850～1250 DEG C.High-temperature roasting makes the binding agent in green compact carbonize, and obtains electrode block head product.
After high-temperature roasting, binding agent is also burnt till activated carbon, but after shaping compacting before, binding agent defines jail
Solid skeleton structure, thus there being certain intensity, will not be loose after roasting.
For broken after roasting or crack unqualified roasting base, can reclaim and process further, be soaked with binding agent
Stain and after baking, concrete technology is：Underproof roasting base carries out removing surface first, then preheats 6 at 260～380 DEG C
～10 hours, be then charged into impregnating autoclave, vacuumize (8～9KPa, 40～50min), add binding agent, in 180～200 DEG C of temperature
Under degree, under 1.2～1.5MPa pressure, impregnating by pressure 3～4 hours and then the idiosome after further taking out dipping, at 700～800 DEG C
Roasting 1～2 hour.
In described step (5), described activating process is：First carry out physical activation method in activation furnace, using vapor
Or CO2Gas activation, 800～900 DEG C of activation temperature, activation duration 1～2 hour.Then, then carry out chemical activation, chemistry is lived
Change method is to immerse electrode in the activator aqueous solution, soaks 5～7 hours, then take out electrode, put into electric furnace at a temperature of 80 DEG C
In, in nitrogen or argon gas atmosphere, activate 1～2 hour at 450 DEG C, finally, deionized water is washed, until cleaning solution
PH is 6～7.Described activator solution can be the potassium hydroxide that the phosphoric acid solution of mass fraction 40%, mass fraction are 110%
One of nitric acid of solution, the liquor zinci chloridi of mass fraction 25% or mass fraction 8%.
The present invention also provides the capacitive deionization device-specific activated carbon electrodes block preparing according to the method described above.
Described capacitive deionization device-specific activated carbon electrodes block can be used for preparing capacitor deionizing instrument, further,
Can be used for water demineralizing process, or in water the harmful ion such as heavy metal ion, hardness, fluorine ion removal.
The beneficial effects of the present invention is
1. the method preparation cost cheap it is easy to large-scale production.Ripe graphite electrode or sintering activity charcoal may be selected
Preparation technology and equipment, as reference, are amplified metaplasia and produce.
2. the electrode good integrity that the method is obtained, high mechanical strength, it is less prone to disintegration and slag-off phenomenon, can be according to setting
Standby group reload request, cuts into various required shapes.
3. compare common cold spraying or mould pressing method, binder free residual in the electrode that the method is obtained, it is to avoid
The problem blocking duct and reducing electric conductivity because of binding agent.Thus electrode hole is flourishing, specific surface area is high.
4. compare common sintering activity charcoal preparation technology, the present invention selects super capacitor special-purpose activated charcoal as main one-tenth
Point, containing more mesoporous, thus the electric conductivity of electrode material being obtained and ratio constant volume function admirable, it is highly suitable for electric capacity and go
Application in ion device.
5. in the present invention, calcine technology can achieve that the crystallization to binding agent and activated carbon granule and graphitization control, both really
Protect unformed form and the voids content of activated carbon granule main body, achieve binding agent and the graphitization of amount of activated charcoal again,
Thus obtaining electric conductivity and all moderate electrode product of specific surface area.
6. the carbon fiber adding in the method and conductive black can improve the electric conductivity of electrode, and can improve electricity
The mechanical strength of pole block and blockiness.
Specific embodiment
Technical scheme is described further with specific embodiment below, but protection scope of the present invention is not
It is limited to this.
Embodiment 1：
Take cocoanut active charcoal 600g, medium temperature coal pitch 200g, carbon fiber 20g, expanded graphite powder 50g, conductive carbon black 50g.
The particle diameter of activated carbon is 6 μm, and specific surface area is 1550m2/g.Medium temperature coal pitch softening temperature is 80～86 DEG C.Carbon fiber diameter
For 5 μm, length is 1.5cm.Expanded graphite powder is 50 mesh, phosphorus content 93%.The resistivity of conductive black is 1.2 Ω m.
First the siccative particle in addition to coal tar pitch is added in kneading machine and is dry mixed under normal temperature, the time that is dry mixed is 20min,
Then add coal tar pitch toward in kneading machine again, carry out wet mixing, wet mixing 40min, temperature is 145 DEG C；
Thickener after kneading carries out next step moulding process, and moulding process selects isostatic pressing process：By the thickener after kneading,
After being cooled to 90 DEG C, it is filled in rubber mold, vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, taken out after sealing
Vacuum, discharges the air between powder particle, then puts in the high-pressure bottle equipped with liquid mediums such as water or oil by rubber mold,
Put in cold isostatic press, be pressurized to 100MPa, dwell time 10min, be pressed into the square that the length of side is 20cm.
Then shaping raw embryo is carried out roasting, roasting technique：First carry out pre- carbonization treatment, in electric furnace, in nitrogen atmosphere
In with the programming rate of 2 DEG C/min, be warmed up to 850 DEG C, and be incubated 1 hour；Then carry out high-temperature roasting, sintering temperature is
900 DEG C, a length of 1 hour during roasting.
Electrode block head product after roasting carries out machining, and described being machined in stock-removing machine is carried out, and adopts
Machining, cut into the length of side be 20cm, thickness be 1mm square electrode to be activated.
Electrode to be activated carries out activating process, and described capacitive deionization device-specific activated carbon electrodes block is obtained；Described
Activating process is：First carry out physical activation method in activation furnace, using steam activation, 850 DEG C of activation temperature, activate duration 1
Hour.Then, then carry out chemical activation, electrode immersion mass fraction is in 110% potassium hydroxide solution, in 80 DEG C of temperature
Under, soak 7 hours.Then take out electrode to be placed in electric furnace, in a nitrogen atmosphere, at 450 DEG C, activate 1 hour.Finally, spend
Ionized water is washed, until the pH of cleaning solution is reduced to 7, final electrode finished product is obtained.
Choose two plate electrode finished products, electric conductivity test is carried out using universal meter to electrode, probe contacts the two of electrode respectively
Individual relative side, spacing is 20cm, and the resistance recording is 7.8 Ω and 8.3 Ω, shows that the electric conductivity of electrode is very good.Use electronics
Balance claim electrode slice quality be respectively 41.4g and 42.1g.
The capacitive deionization module that activated carbon electrodes are formed, carries out sodium chloride desalting performance test to it：Take in two panels
State the activated carbon electrodes that method is obtained, assembling is grown up and the wide capacitive deionization module being 20cm.Electrode slice surface spreads respectively
A layer thickness is 0.05mm, the PP non-woven fabrics of a diameter of 5 μm of filter opening, and between electrode slice, one piece of thickness of arrangement is the square of 1mm
Frame-shaped silica gel pad, thus form electrode spacing and the water flow passage of 1mm.The a length of 22cm in outside of silica gel pad, inner edge is a length of
19.5cm.Clamp two panels electrode and pad with two panels fixed plate again, then with screw by module fixation.Dc source is positive and negative
Pole, is connected on electrode with wire respectively.Prepare 1000mL, electrical conductivity is 920us/cm sodium chloride solution.Desalination is tested to follow
The mode of ring test is carried out, with the electrical conductivity of the thunder magnetic DDSJ-308F conductivity meter monitor in real time aqueous solution.Operating voltage 1.6V,
Discharge is 100mL/min, 29 DEG C of water temperature.
Through the Electro Sorb desalination processes of 40min, the electrical conductivity of sodium chloride solution is reduced to 476us/cm from 920us/cm.
Close power supply afterwards, the both positive and negative polarity of electrode slice wire short circuit carries out electrode regeneration.Through the regenerative process of 34min, solution
Electrical conductivity return to 917us/cm.Calculating this silica aerogel electrode tablet quality absorption ration is 2.66mg/g, and volume ratio is inhaled
Attached amount is 2.78mg/cm3.Therefore, this activated carbon electrodes has preferable electro adsorption capacity, is suitable as capacitive deionization equipment
Electrode.
Embodiment 2：
Take cocoanut active charcoal 600g, phenolic resin 150g, methenamine 12g, carbon fiber 20g, conductive carbon black 40g, expansion
Graphite 10g.The particle diameter of activated carbon is 5.4 μm, and specific surface area is 1840m2/g.Phenolic resin model is 2123.Carbon fiber diameter
For 5 μm, length is 1cm.Expanded graphite powder is 50 mesh, phosphorus content 93%.The resistivity of conductive black is 1.2 Ω m.
Phenolic resin is dissolved with the ethanol of 10 times of quality, then with the siccative particle in addition to binding agent with electronic
Mixer mixing 1h, adds methenamine, continues mixing 30min, prepared slurry.
Slurry carries out next step moulding process, and moulding process selects isostatic pressing process：By the filled therewith mixing to rubber
In mould, vacuumized after sealing, discharged the air in space, then rubber mold is put into and be situated between equipped with liquid such as water or oil
In the high-pressure bottle of matter, put in cold isostatic press, be pressurized to 120MPa, dwell time 15min, being pressed into the length of side is 20cm's
Square
Then shaping raw embryo is carried out roasting, roasting technique：First carry out pre- carbonization treatment, in electric furnace, in nitrogen atmosphere
In with the programming rate of 2 DEG C/min, be warmed up to 800 DEG C, and be incubated 1 hour；Then carry out high-temperature roasting, sintering temperature is
850 DEG C, a length of 1 hour during roasting.
Electrode block head product after roasting carries out machining, and described being machined in stock-removing machine is carried out, and adopts
Machining, cut into the length of side be 20cm, thickness be 1mm square electrode to be activated.
Electrode to be activated carries out activating process, and described capacitive deionization device-specific activated carbon electrodes block is obtained；Described
Activating process is：First carry out physical activation method in activation furnace, using carbon dioxide activation, 800 DEG C of activation temperature, activate duration
1 hour.Then, then carry out chemical activation, electrode immersion mass fraction is in 110% potassium hydroxide solution, in 80 DEG C of temperature
Under degree, soak 5 hours.Then take out electrode and put in electric furnace, in a nitrogen atmosphere, at 450 DEG C, activate 1 hour.Finally, use
Deionized water is washed, until the pH of cleaning solution is reduced to 7, final electrode finished product is obtained.
Choose two plate electrode finished products, electric conductivity test is carried out using universal meter to electrode, probe contacts the two of electrode respectively
Individual relative side, spacing is 20cm, and the resistance recording is 5.6 Ω and 5.8 Ω, shows that the electric conductivity of electrode is very good.Use electronics
Balance claim electrode slice quality be respectively 35.6g and 35.2g.
The capacitive deionization module that activated carbon electrodes are formed, carries out sodium chloride desalting performance test to it：Take in two panels
State the activated carbon electrodes that method is obtained, assembling is grown up and the wide capacitive deionization module being 20cm.Electrode slice surface spreads respectively
A layer thickness is 0.05mm, the PP non-woven fabrics of a diameter of 5 μm of filter opening, and between electrode slice, one piece of thickness of arrangement is the square of 1mm
Frame-shaped silica gel pad, thus form electrode spacing and the water flow passage of 1mm.The a length of 22cm in outside of silica gel pad, inner edge is a length of
19.5cm.Clamp two panels electrode and pad with two panels fixed plate again, then with screw by module fixation.Dc source is positive and negative
Pole, is connected on electrode with wire respectively.Prepare 1000mL, electrical conductivity is 920us/cm sodium chloride solution.Desalination is tested to follow
The mode of ring test is carried out, with the electrical conductivity of the thunder magnetic DDSJ-308F conductivity meter monitor in real time aqueous solution.Operating voltage 1.6V,
Discharge is 100mL/min, 29 DEG C of water temperature.
Through the Electro Sorb desalination processes of 40min, the electrical conductivity of sodium chloride solution is reduced to 426us/cm from 920us/cm.
Close power supply afterwards, the both positive and negative polarity of electrode slice wire short circuit carries out electrode regeneration.Through the regenerative process of 32min, solution
Electrical conductivity return to 912us/cm.Calculating this silica aerogel electrode tablet quality absorption ration is 3.39mg/g, and volume ratio is inhaled
Attached amount is 3.09mg/cm3.Therefore, this activated carbon electrodes has preferable electro adsorption capacity, is suitable as capacitive deionization equipment
Electrode.
Claims (9)
1. a kind of preparation method of capacitive deionization device-specific activated carbon electrodes block is it is characterised in that methods described is：
Activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black is taken to be raw material, through mixing, shaping, roasting, machinery
Processing, activation, are obtained described capacitive deionization device-specific activated carbon electrodes block；
Described activated carbon, binding agent, carbon fiber, expanded graphite powder, the mass fraction of conductive carbon black be active carbon powder 60～
90%, binding agent 8～25%, carbon fiber 0.5～2.5%, expanded graphite 1～10%, conductive black 2～10%.
2. the method for claim 1 is it is characterised in that the method comprising the steps of：
(1) take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black to be raw material, obtain thickener through hybrid technique,
Described hybrid technique is wet blending process after kneading technique or dissolving；
(2), through moulding process, the raw embryo of prepared solid shape, described moulding process is using molding, extruding, vibration moulding for thickener
Or isostatic pressing process；
(3) raw embryo of solid shape, through high-temperature roasting, makes the binding agent in green compact carbonize, obtains electrode block head product；Described
Sintering temperature is 850～1250 DEG C；
(4) the electrode block head product after roasting carries out machining, and described being machined in stock-removing machine is carried out, using cutting
Cut processing, the size needing, shape, precision make electrode to be activated according to electrode；
(5) electrode to be activated carries out activating process, and described capacitive deionization device-specific activated carbon electrodes block is obtained.
3. the method for claim 1 is it is characterised in that described binding agent is coal tar pitch, humic acid sodium salt, polyethylene
Adjoin one of pyrrolidone, sodium cellulose glycolate, phenolic resin or polyvinyl butyral resin or two or more.
4. method as claimed in claim 2 is it is characterised in that in described step (1), described hybrid technique presses different binding agents
Using different mixed methods, described binding agent is coal tar pitch, phenolic resin, polyvinylpyrrolidone or polyvinyl butyral resin
When, mixed using kneading technique；Described kneading technique includes dry blend wet mixing；Wherein it is dry mixed first by addition to binding agent
Siccative particle add kneading machine, under normal temperature in be dry mixed, be dry mixed the time be 20～35min；Then add toward in kneading machine again
Binding agent, carries out wet mixing, a length of 40～55min during wet mixing, and operation temperature is higher than 50～80 DEG C of binding agent softening point, and can not surpass
Cross the carburizing temperature of binding agent；When described binding agent is humic acid sodium salt, sodium cellulose glycolate or phenolic resin, using dissolving
Wet blending process is mixed afterwards, that is, first by described binding agent with solvent dissolve, then with the siccative particle in addition to binding agent
Mixed with mixer.
5. method as claimed in claim 2 is it is characterised in that in described step (2), described moulding process from extruding or waits
Hydrostatic profile mode；Described extrusion process is：The thickener that step (1) is obtained is cooled to 90～120 DEG C) after, enter luggage successively
Material, precompressed and three processes of extruding；Described charging process is point 2～3 blankings, then 4～10MPa compacting；Described precompressed work
Skill is：Pressure 20～25MPa, time 3～5min, vacuumize simultaneously, are de-gassed；Described extrusion process is：Pressure be 5～
15MPa, is obtained bar-shaped or block shaping raw embryo；
Described isostatic pressing process is：The thickener that step (1) is obtained, after being cooled to 90～120 DEG C, is filled in rubber mold,
Vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, vacuumized after sealing, discharge the air between powder particle；Then
Rubber mold is put in the high-pressure bottle equipped with liquid mediums such as water or oil, is pressurized to 100～200MPa, dwell time 10～
20min, is pressed into cylinder or the shaping raw embryo of cuboid.
6. method as claimed in claim 2 is it is characterised in that in described step (3), described high-temperature roasting inert atmosphere,
Carry out under one of ammonia atmosphere, vapor or both above mixed atmospheres, roasting technique is：Shaping raw embryo is carried out pre-
Carbonization treatment, with the programming rate of 2 DEG C/min in electric furnace, is warmed up to 800～900 DEG C, and is incubated 1～2 hour；Then enter
Row high-temperature roasting, a length of 1～2 hour during roasting, temperature is 850～1250 DEG C；High-temperature roasting makes the binding agent in green compact carbonize,
Obtain electrode block head product.
7. method as claimed in claim 2 is it is characterised in that in described step (5), described activating process is：First in activation
Carry out physical activation method, using vapor or CO in stove2Gas activation, 800～900 DEG C of activation temperature, activation duration 1～2 is little
When；Then, then carry out chemical activation, chemical activation method is to immerse in the activator aqueous solution by electrode, soaks 5 at a temperature of 80 DEG C
～7 hours, then take out electrode, put in electric furnace, in nitrogen or argon gas atmosphere, 450 DEG C activate 1～2 hour, finally,
Deionized water is washed, until the pH of cleaning solution is 6～7；Described activator solution is that the phosphoric acid of mass fraction 40% is molten
Liquid, mass fraction are the nitric acid of 110% potassium hydroxide solution, the liquor zinci chloridi of mass fraction 25% or mass fraction 8%
One of.
8. the capacitive deionization device-specific activated carbon electrodes block that the method as described in one of claim 1～7 prepares.
9. capacitive deionization device-specific activated carbon electrodes block as claimed in claim 8 is in preparing capacitor deionizing instrument
Application.
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