CN106395814B - A kind of preparation method of capacitive deionization device-specific activated carbon electrodes block - Google Patents
A kind of preparation method of capacitive deionization device-specific activated carbon electrodes block Download PDFInfo
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- 238000002242 deionisation method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 82
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000011230 binding agent Substances 0.000 claims abstract description 56
- 238000001994 activation Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
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- 238000012545 processing Methods 0.000 claims abstract description 4
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- 239000003795 chemical substances by application Substances 0.000 claims description 7
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- 239000011294 coal tar pitch Substances 0.000 claims description 6
- 238000010237 hybrid technique Methods 0.000 claims description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
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- 239000012190 activator Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
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- HMGUIQPKFUZDPV-UHFFFAOYSA-L disodium;bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate Chemical group [Na+].[Na+].C1C2C=CC1C(C(=O)[O-])C2C([O-])=O HMGUIQPKFUZDPV-UHFFFAOYSA-L 0.000 claims description 4
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- 238000005255 carburizing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
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- 239000002904 solvent Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 238000003763 carbonization Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 claims 1
- 150000004040 pyrrolidinones Chemical class 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000000072 sodium resin Substances 0.000 claims 1
- 238000003754 machining Methods 0.000 abstract description 6
- 238000011033 desalting Methods 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 15
- 239000007772 electrode material Substances 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 5
- 238000010612 desalination reaction Methods 0.000 description 5
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- 239000003610 charcoal Substances 0.000 description 4
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- 238000012360 testing method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
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- 235000010299 hexamethylene tetramine Nutrition 0.000 description 3
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 3
- 229960004011 methenamine Drugs 0.000 description 3
- 238000009656 pre-carbonization Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000011300 coal pitch Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 description 1
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
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- 239000003292 glue Substances 0.000 description 1
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- 230000015689 metaplastic ossification Effects 0.000 description 1
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- 239000002243 precursor Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- Analytical Chemistry (AREA)
- Molecular Biology (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention provides a kind of preparation method of capacitive deionization device-specific activated carbon electrodes block：Active carbon powder, binding agent, carbon fiber, expanded graphite powder and conductive black are fitted into hopper and mixed, is uniformly mixed, is kneaded into plasticity thickener, the thickener mixed is shaped to have figurate green compact in former.Green compact are under inserts protection, carry out high-temperature roasting in loading heating furnace, obtain electrode block head product.To head product is used into machining, electrode size, shape required for being made, precision.Activation process finally is carried out to electrode, electrode final finished is made.The method preparation cost is cheap, is easy to mass produce.Binder free remains in electrode, good conductivity, electrode good integrity, and high mechanical strength is cleavable into various required shapes.This electrode can be used for prepare capacitor deionizing instrument, for the desalting processing of water, or in water the harmful ion such as heavy metal ion, hardness, fluorine ion removal.
Description
Technical field
The present invention relates to the preparation side of field of waste water treatment, more particularly to capacitive deionization device-specific activated carbon electrodes block
Method.
Background technology：
Capacitive deionization (CDI) is also known as Electro Sorb technology (EST), and its general principle is based on the electric double layer reason in electrochemistry
By using the electrochemical properties on charged electrode surface, to realize the absorption of charged particle in water and removal, the decomposition of organic matter etc.
Purpose.CDI has that operating cost is low, need not add medicine, non-secondary pollution, water quality requirement is low, operation and maintenance is simple, de- to entering
The advantages that salt rate is adjustable, Water Sproading rate is 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 materials, usual CDI electrodes are typically by activated carbon, conductive agent (Graphon) and adhesive by being molded or being coated with
It is made.Activated carbon is the electrode material for being most hopeful to carry out large-scale industrial application as most cheap carbon-based electrode material.But
Activated carbon electrodes resistance itself is excessive and the application that the defects of resistance to mass tranfer limits it be present.In addition, carbon electrode generally existing
One it is fatal the problem of be to be unable to self-supporting to use as absolute electrode.Inevitably to bonding in electrode process is made
The use of the materials such as agent, conductive agent and collector, these materials will block most of aperture of traditional carbon material, reduce
Current efficiency, the electrical conductivity of electrode are also affected, so as to reduce desalting efficiency and adsorbance.
United States Patent (USP) (US 6787235B2) reports a kind of preparation method and its use of unformed activated carbon agglomerated materials
On the way, the shape of needs can be cut into by activated carbon block made from high temperature high pressure process, there is high specific capacitance, available for electricity
Hold deionization technical field.But such a 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 more
Hole carbon, conductive agent and polytetrafluoroethylene (PTFE) are ground mixing, and then carrying out high energy with roller rolls obtained combination electrode material.
The volume preparation method of this electrode material is simple, but the polytetrafluoroethylene (PTFE) binding agent mixed 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, add graphene oxide and inorganic or have
Machine amine, then presoma is obtained through hydro-thermal method, finally precursor is heated again and carries 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 such a 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, surpasses
Level capacitance electrode material is added in the glue of binding agent, capacitance electrode slurries is made by mechanical agitation, 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 mixed
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 slurries are made, then by slurries compression molding, are then placed in electric furnace
Middle activation.Electrode material electric conductivity made from this method and specific capacitance are all very good.But the cost of NACF is too high,
And electrode material intensity is bad.
The content of the invention
It is an object of the present invention to provide a kind of good conductivity, specific surface area is big and specific capacitance is high active carbon electrode block
Preparation method, binder free remains in electrode, electrode good integrity, and high mechanical strength is cleavable into various required shapes.
The technical solution adopted by the present invention is：
A kind of preparation method of capacitive deionization device-specific activated carbon electrodes block, methods described are：
It is raw material to take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black, by mixing, being molded, being calcined,
Machining, activation, are made the capacitive deionization device-specific activated carbon electrodes block；
The 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 are 5~100 μm, 1500~2000m of specific surface area2/g。
Described binding agent is coal tar pitch, humic acid sodium salt, polyethylene adjoin pyrrolidone, sodium cellulose glycolate, phenolic aldehyde tree
It is more than one or both of fat or polyvinyl butyral resin.The molecular weight of binding agent is smaller, and the blocking to activated carbon capillary is got over
Seriously；
Described carbon fiber is 5~10 μm of diameter, and length is 1mm~100mm chopped carbon fiber, and fiber surface is without upper
Starch agent；
Described expanded graphite powder is generally 50~100 mesh.
Further, the method for the invention comprises the following steps：
(1) it is raw material to take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black, is obtained by hybrid technique
Thickener, the hybrid technique are wet blending process after kneading technique or dissolving；
(2) thickener passes through moulding process, and the raw embryo of solid shape is made, and the moulding process can use and be molded, extrudes, shake
Dynamic shaping or isostatic pressing process；
(3) raw embryo of solid shape passes through high-temperature roasting, carbonizes the binding agent in green compact, obtains electrode block head product；
The sintering temperature is 850~1250 DEG C；
(4) the electrode block head product after being calcined is machined, and described being machined in stock-removing machine is carried out, and is adopted
With machining, electrode to be activated is made in the size needed according to electrode, shape, precision；
(5) electrode to be activated carries out activating process, and the capacitive deionization device-specific activated carbon electrodes block is made；
In the step (1), the hybrid technique uses different mixed methods by different binding agents, and binding agent drips for coal
When green grass or young crops, phenolic resin, polyvinylpyrrolidone or polyvinyl butyral resin, mixed using kneading technique；The binding agent
For humic acid sodium salt, sodium cellulose glycolate or phenolic resin when, mixed using wet blending process after dissolving, i.e., first will described in
Binding agent is dissolved with solvent, is then mixed with the siccative particle in addition to binding agent with mixer.
Further, described kneading technique includes two processes of dry blend wet mixing, wherein dry-mixed carried 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 no more than viscous
Tie the carburizing temperature of agent.
Further, the kneading technique preferably operates in accordance with the following methods：First the siccative particle in addition to binding agent is added
Enter kneading machine, middle progress is dry-mixed under normal temperature, and the dry-mixed time is 20~35min, is well mixed various raw materials, while makes different grains
The solid carbonaceous material of degree size is equably mixed and filled, and improves the compactness of compound；Then again toward adding in kneading machine
Binding agent, carries out wet mixing, and the binding agent is in coal tar pitch, phenolic resin, polyvinylpyrrolidone or polyvinyl butyral resin
One or more, 40~55min of wet mixing time, temperature is higher than 50~80 DEG C of binding agent softening point, and no more than viscous
Tie the carburizing temperature of agent；During wet mixing, liquid adhesive even spread and infiltration particle surface, one layer of tack coat is formed,
All materials are bonded to each other, and then form the plasticity thickener of homogeneous, are advantageous to be molded.Meanwhile portion of binder soaks
Carbonaceous material internal voids are arrived thoroughly, further increase the density and caking property of thickener.Thickener after kneading carry out in next step into
Type technique.
When the 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 for the mass fraction 5~20% that quality is water,
Stirring obtains binder solution, then the siccative particle in addition to binding agent is mixed with binder solution, use to abundant dissolving
Electric blender mixes.
When the binding agent is phenolic resin, it can be mixed using kneading technique, also can be by phenolic resin solvent
After dissolving, mixed using wet blending process, the technique is specially：The phenolic resin ethanol of 10 times of quality is dissolved, so
1h is mixed with electric blender with the siccative particle in addition to binding agent afterwards, adds quality as binding agent quality 6~10%
Curing agent, continue 30~40min of mixing.The curing agent can be methenamine.
In the step (2), the moulding process can use molding, extruding, vibration moulding or isostatic pressing method, system
Into the raw embryo product of fixed character.Molding uses vertical hydraulic press, is generally used for preparing low-grade pellet electrode.Extrusion forming is adopted
With Horizontal hydraulic extruder or screw extruder.Vibration moulding uses vibrating forming machine, can prepare that compactness is good, and mechanical performance is excellent
Electrode block.Isostatic pressing uses iso-static pressure shaping machine, and it is homogeneous to prepare Density Distribution, uniform texture, and density is high, burns
It is small to tie shrinkage factor, complex-shaped, the good electrode of machining property.
Further, preferably moulding process is from extruding or isostatic pressing mode.The extruding is preferably squeezed in carbon pole
Carried out in press, technique is：The thickener that step (1) obtains is cooled to 90~120 DEG C) after, fed successively, precompressed and squeeze
Press three processes.
Further, the charging process is point 2~3 blankings, and then 4~10MPa is compacted；The pre-pressing process is：Pressure
20~25MPa of power, 3~5min of time, is vacuumized simultaneously, is de-gassed；The extrusion process is：Pressure is 5~15MPa, system
It is bar-shaped or it is block shaping raw embryo described in isostatic pressing process be：The thickener that step (1) is obtained, after being cooled to 90~120 DEG C, is filled out
It is charged in rubber mold, is vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, is vacuumized after sealing, discharges powder
The air of intergranular.Then rubber mold is put into the high-pressure bottle equipped with the liquid medium such as water or oil, it is pressurized to 100~
200MPa, 10~20min of dwell time, it is pressed into cylinder or the shaping raw embryo of cuboid.
In the step (3), described high-temperature roasting is in one or both of inert atmosphere, ammonia atmosphere, vapor
Carried out under mixed atmosphere above, concrete technology is：Shaping raw embryo is subjected to pre- carbonization treatment, with 2 DEG C/min's in electric furnace
Programming rate, 800~900 DEG C are warming up to, and are incubated 1~2 hour；Then high-temperature roasting is carried out, a length of 1~2 is small during roasting
When, temperature is 850~1250 DEG C.High-temperature roasting carbonizes the binding agent in green compact, obtains electrode block head product.
After high-temperature roasting, binding agent is also burnt till activated carbon, but after shaping compacting before, binding agent forms jail
Solid skeleton structure, will not be loose after roasting so as to there is certain intensity.
For broken or crack unqualified roasting base after roasting, further processing can be reclaimed, is soaked with binding agent
Stain and after baking, concrete technology are：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 dipping is further taken out, at 700~800 DEG C
Roasting 1~2 hour.
In the step (5), described activating process is：Physical activation method is first carried out in activation furnace, using vapor
Or CO2Gas activation, 800~900 DEG C of activation temperature, activation duration 1~2 hour.Then, then chemical activation is carried out, chemistry is living
Change method is to immerse electrode in the activator aqueous solution, is soaked 5~7 hours at a temperature of 80 DEG C, then takes out electrode, be put into electric furnace
In, in nitrogen or argon gas atmosphere, activate 1~2 hour at 450 DEG C, finally, washed with deionized water, until cleaning solution
PH is 6~7.The potassium hydroxide that the activator solution can be the phosphoric acid solution of mass fraction 40%, mass fraction is 110%
One kind in the 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 being prepared according to the method described above.
Described capacitive deionization device-specific activated carbon electrodes block can be used for preparing capacitor deionizing instrument, further,
Available for the desalting processing of water, or in water the harmful ion such as heavy metal ion, hardness, fluorine ion removal.
The beneficial effects of the present invention are
1. the method preparation cost is cheap, it is easy to mass produce.Ripe graphite electrode or sintering activity charcoal may be selected
Preparation technology and equipment are amplified metaplasia production as reference.
2. electrode good integrity made from the method, high mechanical strength, disintegration and slag-off phenomenon are less prone to, can be according to setting
Standby assembling requires, cuts into various required shapes.
3. comparing common cold spraying or mould pressing method, binder free remains in electrode made from the method, avoids
The problem of blocking duct because of binding agent and reduce electric conductivity.Thus electrode hole is flourishing, and specific surface area is high.
4. compare common sintering activity charcoal preparation technology, the present invention from super capacitor special-purpose activated charcoal as mainly into
Point, containing more mesoporous, thus the electric conductivity of obtained electrode material and than constant volume function admirable, it is highly suitable for electric capacity and goes
Application in ion device.
5. calcine technology can realize the crystallization to binding agent and activated carbon granule and graphitization control in the present invention, both really
The unformed form and voids content of activated carbon granule main body have been protected, has realized the graphitization of binding agent and amount of activated charcoal again,
So as to obtain all moderate electrode product of electric conductivity and specific surface area.
6. the carbon fiber and conductive black that are added in the method can improve the electric conductivity of electrode, and can improve electricity
The mechanical strength of pole block and blockiness.
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, specific surface area 1550m2/g.Medium temperature coal pitch softening temperature is 80~86 DEG C.Carbon fiber diameter
For 5 μm, length 1.5cm.Expanded graphite powder is 50 mesh, phosphorus content 93%.The resistivity of conductive black is 1.2 Ω m.
First siccative particle in addition to coal tar pitch is added in kneading machine and carries out dry-mixed under normal temperature, the dry-mixed time is 20min,
Then again toward coal tar pitch is added in kneading machine, wet mixing, wet mixing 40min are carried out, 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 into rubber mold, is vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, is taken out after sealing
Vacuum, the air between powder particle is discharged, then rubber mold is put into the high-pressure bottle equipped with the liquid medium such as water or oil,
It is put into cold isostatic press, is pressurized to 100MPa, dwell time 10min, is pressed into the square that the length of side is 20cm.
Then shaping raw embryo is calcined, roasting technique：Pre- carbonization treatment is first carried out, in electric furnace, in nitrogen atmosphere
In with 2 DEG C/min programming rate, be warming up to 850 DEG C, and be incubated 1 hour；Then high-temperature roasting is carried out, sintering temperature is
900 DEG C, a length of 1 hour during roasting.
Electrode block head product after roasting is machined, and described being machined in stock-removing machine is carried out, and is used
Machining, cut into the square electrode to be activated that the length of side is 20cm, thickness is 1mm.
Electrode to be activated carries out activating process, and the capacitive deionization device-specific activated carbon electrodes block is made；Described
Activating process is：Physical activation method is first carried out in activation furnace, using steam activation, 850 DEG C of activation temperature, activates duration 1
Hour.Then, then chemical activation is carried out, electrode is immersed in the potassium hydroxide solution that mass fraction is 110%, 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 made.
Two plate electrode finished products are chosen, electric conductivity test are carried out to electrode using universal meter, probe contacts the two of electrode respectively
Individual relative side, spacing 20cm, the resistance measured are 7.8 Ω and 8.3 Ω, show that the electric conductivity of electrode is very good.Use electronics
Balance claim the quality of electrode slice is respectively 41.4g and 42.1g.
The capacitive deionization module that activated carbon electrodes are formed, sodium chloride desalting performance test is carried out to it：Take in two panels
Activated carbon electrodes made from method are stated, assembling growth and width are 20cm capacitive deionization module.Electrode slice surface is spread respectively
A layer thickness is 0.05mm, the PP non-woven fabrics of a diameter of 5 μm of filter opening, and the square that one piece of thickness is 1mm is arranged between electrode slice
Frame-shaped silica gel pad, so as to form 1mm electrode spacing and water flow passage.The a length of 22cm in outside of silica gel pad, inner edge are a length of
19.5cm.Again two panels electrode and pad are clamped with two panels fixed plate, then with screw by module fixation.Dc source is positive and negative
Pole, it is connected to respectively with wire on electrode.1000mL is prepared, electrical conductivity is 920us/cm sodium chloride solutions.Desalination is tested to follow
The mode of ring test is carried out, and monitors the electrical conductivity of the aqueous solution in real time with thunder magnetic DDSJ-308F conductivity meters.Operating voltage 1.6V,
Water-carrying capacity is 100mL/min, 29 DEG C of water temperature.
By 40min Electro Sorb desalination processes, the electrical conductivity of sodium chloride solution is reduced to 476us/cm from 920us/cm.
Power supply is closed afterwards, by the both positive and negative polarity of electrode slice wire short circuit, carries out electrode regeneration.By 34min regenerative process, solution
Electrical conductivity return to 917us/cm.It is 2.66mg/g that this silica aerogel electrode tablet quality absorption ration, which is calculated, 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, specific surface area 1840m2/g.Phenolic resin model is 2123.Carbon fiber diameter
For 5 μm, length 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 to mix 30min, slurry is made.
Slurry carries out next step moulding process, and moulding process selects isostatic pressing process：By the filled therewith of mixing to rubber
In mould, vacuumized after sealing, discharge the air in space, then rubber mold is put into and is situated between equipped with the liquid such as water or oil
In the high-pressure bottle of matter, it is put into cold isostatic press, is pressurized to 120MPa, dwell time 15min, it is 20cm's to be pressed into the length of side
Square
Then shaping raw embryo is calcined, roasting technique：Pre- carbonization treatment is first carried out, in electric furnace, in nitrogen atmosphere
In with 2 DEG C/min programming rate, be warming up to 800 DEG C, and be incubated 1 hour；Then high-temperature roasting is carried out, sintering temperature is
850 DEG C, a length of 1 hour during roasting.
Electrode block head product after roasting is machined, and described being machined in stock-removing machine is carried out, and is used
Machining, cut into the square electrode to be activated that the length of side is 20cm, thickness is 1mm.
Electrode to be activated carries out activating process, and the capacitive deionization device-specific activated carbon electrodes block is made；Described
Activating process is：Physical activation method is first carried out in activation furnace, using carbon dioxide activation, 800 DEG C of activation temperature, activates duration
1 hour.Then, then chemical activation is carried out, electrode is immersed in the potassium hydroxide solution that mass fraction is 110%, in 80 DEG C of temperature
Under degree, soak 5 hours.Then take out electrode to be put into 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 made.
Two plate electrode finished products are chosen, electric conductivity test are carried out to electrode using universal meter, probe contacts the two of electrode respectively
Individual relative side, spacing 20cm, the resistance measured are 5.6 Ω and 5.8 Ω, show that the electric conductivity of electrode is very good.Use electronics
Balance claim the quality of electrode slice is respectively 35.6g and 35.2g.
The capacitive deionization module that activated carbon electrodes are formed, sodium chloride desalting performance test is carried out to it：Take in two panels
Activated carbon electrodes made from method are stated, assembling growth and width are 20cm capacitive deionization module.Electrode slice surface is spread respectively
A layer thickness is 0.05mm, the PP non-woven fabrics of a diameter of 5 μm of filter opening, and the square that one piece of thickness is 1mm is arranged between electrode slice
Frame-shaped silica gel pad, so as to form 1mm electrode spacing and water flow passage.The a length of 22cm in outside of silica gel pad, inner edge are a length of
19.5cm.Again two panels electrode and pad are clamped with two panels fixed plate, then with screw by module fixation.Dc source is positive and negative
Pole, it is connected to respectively with wire on electrode.1000mL is prepared, electrical conductivity is 920us/cm sodium chloride solutions.Desalination is tested to follow
The mode of ring test is carried out, and monitors the electrical conductivity of the aqueous solution in real time with thunder magnetic DDSJ-308F conductivity meters.Operating voltage 1.6V,
Water-carrying capacity is 100mL/min, 29 DEG C of water temperature.
By 40min Electro Sorb desalination processes, the electrical conductivity of sodium chloride solution is reduced to 426us/cm from 920us/cm.
Power supply is closed afterwards, by the both positive and negative polarity of electrode slice wire short circuit, carries out electrode regeneration.By 32min regenerative process, solution
Electrical conductivity return to 912us/cm.It is 3.39mg/g that this silica aerogel electrode tablet quality absorption ration, which is calculated, 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 (5)
- A kind of 1. preparation method of capacitive deionization device-specific activated carbon electrodes block, it is characterised in that methods described include with Lower step：(1) it is raw material to take activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black, and thickener is obtained by hybrid technique, The hybrid technique uses different mixed methods by different binding agents, and the binding agent is coal tar pitch, phenolic resin, polyethylene When pyrrolidones or polyvinyl butyral resin, mixed using kneading technique；The kneading technique includes dry blend wet mixing；Its In it is dry-mixed the siccative particle in addition to binding agent is first added into kneading machine, it is middle under normal temperature to carry out dry-mixed, the dry-mixed time is 20~ 35min；Then again toward binding agent is added in kneading machine, wet mixing is carried out, a length of 40~55min during wet mixing, operation temperature is higher than viscous 50~80 DEG C of agent softening point is tied, and no more than the carburizing temperature of binding agent；The binding agent is humic acid sodium salt, methylol fibre When tieing up plain sodium or phenolic resin, mixed, i.e., first dissolved the binding agent with solvent, then using wet blending process after dissolving Mixed with the siccative particle in addition to binding agent with mixer；(2) thickener passes through moulding process, and the raw embryo of solid shape is made；The moulding process is from extruding or isostatic pressing mode；The extrusion process is：The thickener that step (1) is obtained is cold But to after 90~120 DEG C, fed successively, three processes of precompressed and extruding；The charging process is point 2~3 blankings, so 4~10MPa is compacted afterwards；The pre-pressing process is：20~25MPa of pressure, 3~5min of time, is vacuumized simultaneously, is de-gassed； The extrusion process is：Pressure is 5~15MPa, and bar-shaped or block shaping raw embryo is made；The isostatic pressing process is：The thickener that step (1) is obtained, after being cooled to 90~120 DEG C, is filled into rubber mold, Vibrated by high-frequency electromagnetic so that press-powder obtains closely knit, is vacuumized after sealing, discharges the air between powder particle；Then Rubber mold is put into the high-pressure bottle equipped with the liquid medium such as water or oil, is pressurized to 100~200MPa, the dwell time 10~ 20min, it is pressed into cylinder or the shaping raw embryo of cuboid；(3) raw embryo of solid shape passes through high-temperature roasting, carbonizes the binding agent in green compact, obtains electrode block head product；It is described Sintering temperature is 850~1250 DEG C；(4) the electrode block head product after being calcined is machined, and described being machined in stock-removing machine is carried out, using cutting Processing is cut, electrode to be activated is made in size, shape, the precision needed according to electrode；(5) electrode to be activated carries out activating process, and the capacitive deionization device-specific activated carbon electrodes block is made；The activated carbon, binding agent, carbon fiber, expanded graphite powder, conductive carbon black mass fraction for 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 as described in claim 1, it is characterised in that in the step (3), described high-temperature roasting inert atmosphere, Carried out under mixed atmosphere more than one or both of ammonia atmosphere, vapor, roasting technique is：Shaping raw embryo is carried out in advance Carbonization treatment, with 2 DEG C/min programming rate in electric furnace, 800~900 DEG C are warming up to, and be 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 carbonizes the binding agent in green compact, Obtain electrode block head product.
- 3. the method as described in claim 1, it is characterised in that in the step (5), described activating process is：First activating Physical activation method is carried out in stove, using vapor or CO2Gas activation, 800~900 DEG C of activation temperature, activation duration 1~2 are small When；Then, then chemical activation is carried out, chemical activation method is to immerse electrode in the activator aqueous solution, soaks 5 at a temperature of 80 DEG C ~7 hours, then take out electrode, be put into electric furnace, in nitrogen or argon gas atmosphere, 450 DEG C activate 1~2 hour, finally, Washed with deionized water, until the pH of cleaning solution is 6~7；The activator solution is that the phosphoric acid of mass fraction 40% is molten Liquid, potassium hydroxide solution, the liquor zinci chloridi of mass fraction 25% or the nitric acid of mass fraction 8% that mass fraction is 110% In one kind.
- 4. the capacitive deionization device-specific activated carbon electrodes block that the method as described in one of claims 1 to 3 is prepared.
- 5. capacitive deionization device-specific activated carbon electrodes block as claimed in claim 4 is in capacitor deionizing instrument is prepared Using.
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Denomination of invention: Preparation method of special activated-carbon electrode block for capacitive deionizing equipment Effective date of registration: 20191016 Granted publication date: 20180410 Pledgee: China Co truction Bank Corp Jinhua branch Pledgor: ZHEJIANG DOWAY ADVANCED TECHNOLOGY CO., LTD. Registration number: Y2019330000116 |
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Date of cancellation: 20201229 Granted publication date: 20180410 Pledgee: China Co. truction Bank Corp Jinhua branch Pledgor: ZHEJIANG DOWAY ADVANCED TECHNOLOGY Co.,Ltd. Registration number: Y2019330000116 |
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Denomination of invention: A preparation method of activated carbon electrode block for capacitive deionization equipment Effective date of registration: 20201231 Granted publication date: 20180410 Pledgee: China Co. truction Bank Corp Jinhua branch Pledgor: ZHEJIANG DOWAY ADVANCED TECHNOLOGY Co.,Ltd. Registration number: Y2020330001357 |