CN105540765B - A kind of capacitive adsorption desalination molecular sieve/porous carbon composite electrode material and preparation method thereof - Google Patents
A kind of capacitive adsorption desalination molecular sieve/porous carbon composite electrode material and preparation method thereof Download PDFInfo
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- CN105540765B CN105540765B CN201610073872.XA CN201610073872A CN105540765B CN 105540765 B CN105540765 B CN 105540765B CN 201610073872 A CN201610073872 A CN 201610073872A CN 105540765 B CN105540765 B CN 105540765B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The present invention relates to a kind of capacitive adsorption desalination molecular sieve/porous carbon composite electrode material and preparation method thereof, the mass fraction of the molecular sieve structure material and porous carbon materials is than 10~40%：60~90%.Preparation method includes：In deionized water by porous carbon materials and the dispersion of molecular sieve structure material, obtain dispersion liquid, adhesive be added, obtains mixed liquor, stir, drying obtains composite material, soaks, roll-in cover on inert conductor to get.The present invention compound is prepared into electrode by porous carbon materials and molecular sieve structure are compound doped, the molecular sieve adulterated can effectively improve the charge efficiency of capacitor, improve desalting performance, possess potential application prospect in terms of capacitive desalination, it can be widely used for the desalination of bitter and seawater, the fields such as water softening.
Description
Technical field
The invention belongs to electrode material and its preparation field, more particularly to a kind of capacitive adsorption desalination molecular sieve/porous
Carbon composite electrode material and preparation method thereof.
Background technology
Capacitive adsorption desalination is a kind of Electrostatic Absorption desalting technology based on electric double layer capacitance principle.In the work of additional power source
Under, anions and canons to opposite electrode movement and adsorb on the electrode under the action of electrostatic field in solution, realize desalination salt
The purpose of water.
The electrode material for preparing low-consumption high-efficiency is always the key point of capacitive adsorption desalting technology.Porous carbon materials are because of it
Have many advantages, such as that high-specific surface area, hole are flourishing, electric conductivity is good, derive from a wealth of sources and be widely used in terms of electrode material.Wherein
The materials such as activated carbon, charcoal-aero gel, carbon nanotube, graphene, carbon fiber have been used for the research of capacitive adsorption desalination electrode.But
It is actual capacitance desalination in application, during applying power source charges, due to the repulsive interaction of coion, electrode interior is identical
Ion consumption electric energy is rejected in solution, is caused desalting efficiency and electrode efficiency to reduce, is increased its energy consumption.This problem limits
Application of the porous carbon electrode material in capacitive adsorption desalination field.
Molecular sieve structure has duct and the prodigious hole of marshalling, internal surface area of uniform pore diameter, while molecular sieve
With good ion exchangeable, center polarity is very strong, and the charged group that surface has is capable of the Zeta electricity of modulation material
Position, can play the role of ion transimission and storage, be conducive to ion diffusion and absorption, be a kind of separation absorption haveing excellent performance
Agent.
Invention content
Technical problem to be solved by the invention is to provide a kind of capacitive adsorption desalination molecular sieve/porous carbon composite electrodes
Material and preparation method thereof, this method is easy to operate, at low cost, is easy to industrialized production and application；Molecular sieve/porous carbon of preparation
Combination electrode can improve the adsorptive selectivity to ion, improve its desalting performance.
A kind of capacitive adsorption desalination molecular sieve/porous carbon composite electrode material of the present invention, the molecular sieve structure material
The mass fraction ratio of material and porous carbon materials is 10~40%：60~90%.
A kind of preparation method of capacitive adsorption desalination molecular sieve/porous carbon composite electrode material of the present invention, including：
(1) in deionized water by porous carbon materials and the dispersion of molecular sieve structure material, dispersion liquid is obtained, bonding is added
Agent obtains mixed liquor, stirs, and drying obtains composite material；The mass fraction of molecular sieve structure material and porous carbon materials ratio is
10~40%：60~90%；Adhesive accounts for the 6~10% of molecular sieve structure material and porous carbon materials quality sum；
(2) the composite material material in step (1) is soaked, roll-in covers on inert conductor, obtains capacitive adsorption desalination
With molecular sieve/porous carbon composite electrode material.
Porous carbon materials are in activated carbon, electrically conductive graphite, carbon nanotube, carbon fiber and carbon aerogels in the step (1)
At least one.
The particle diameter of molecular sieve structure material is 50 nanometers -20 microns in the step (1).
In the step (1) molecular sieve structure material be Si-Al molecular sieve, aluminium phosphate molecular sieve, molecular screen containing heteroatom and
At least one of metal-organic framework.
The Si-Al molecular sieve is at least one of faujasite, modenite, ZSM-5, β type and L-type molecular sieve；Phosphorus
Sour aluminum molecular screen is at least one of AlPO-5 and AlPO-11 molecular sieves.
A concentration of 20~80mg/mL of dispersion liquid in the step (1).
Adhesive is at least one of polytetrafluoroethylene (PTFE) and polyvinylidene fluoride in the step (1).
Stirring is mechanical agitation under room temperature, normal pressure in the step (1), stir speed (S.S.) 200-500r/min, when stirring
Between be 2~4h；The temperature of drying is 80~100 DEG C.
Wetting is with a small amount of ethanol wet in the step (2).
Inert conductor is at least one of titanium, graphite and nickel foam in the step (2).
The thickness of combination electrode material is 0.1-2mm in the step (2).
Combination electrode material is directly as in the preparation of application of electrode to capacitor in the step (2).
Electrode prepared by the present invention can effectively reduce the repulsive interaction of coion, have high current efficiency, high desalination amount
Etc. excellent desalting performance, it is applied to the desalination of seawater and bitter, there is application value.
The present invention prepares molecular sieve/porous using molecular sieve structure compound as additive and porous carbon materials doping and blending
Carbon composite electrode material.The doping of one side molecular sieve structure compound can improve the hydrophily of electrode, be conducive to ion
Migration and transmission, another aspect molecular sieve structure compound can adjust the surface potential distribution of activated adoption location proximate, subtract
The repulsion of few coion, improves the ion selectivity of electrode, to improve the current efficiency of capacitor.By to molecular sieve structure
The Zeta potential and polarographic analysis of compound, molecular sieve/porous carbon materials are compound is assembled into asymmetric capacitor, this method for research
The molecular sieve of preparation/porous carbon composite electrode can improve the adsorptive selectivity to ion, improve its desalting performance.
It, will since molecular sieve has flourishing porous structure and good ion exchangeable and hydrophily in the present invention
It is added in carbon material, can play the role of ion transimission and storage；It simultaneously can be according to the charged group of molecular sieve surface
Also can modulation electrode Zeta potential, more conducively ion diffusion and absorption.The molecular sieve adulterated can effectively improve capacitor
Charge efficiency improves desalting performance, potential application prospect is possessed in terms of capacitive desalination, can be widely used for bitter and seawater
Desalination, the fields such as water softening.
Advantageous effect
(1) electrode preparation method of the invention is easy to operate, at low cost, is easy to industrialized production and application；
(2) molecular sieve of the invention is mainly bear charge characteristic, therefore prepares electrode and assemble asymmetric electricity as cathode
Hold desalter and carry out desalination, the transmission to cation can be improved, reduces electrode surface coion and repel；It is effectively improved common
The problem of current efficiency of electrode is low, high energy consumption.
Description of the drawings
Fig. 1 is the SEM shape appearance figures of HSZ-1/AC electrodes in embodiment 1；
Fig. 2 is asymmetric capacitor in embodiment 1 (AC | | HSZ-1/AC) conductivity and electricity under constant current charge-discharge pattern
Press versus time curve；
Fig. 3 is the SEM shape appearance figures of HSZ-2/AC electrodes in embodiment 2；
Fig. 4 is asymmetric capacitor in embodiment 2 (AC | | HSZ-2/AC) conductivity and electricity under constant current charge-discharge pattern
Press versus time curve.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
It is doping component to take high silicon content H-type beta-molecular sieve HSZ-1, and property is as follows：SiO2/Al2O3Molar ratio is 40：1,
Specific surface area is 530m2/ g, particle diameter size are 4 microns.
Compound concentration is the dispersion liquid (dispersion is in deionized water) of 50mg/mL activated carbons and HSZ-1 molecular sieves, is added
PTFE emulsion (mass fraction 60%), activated carbon, HSZ-1 molecular sieves and PTFE mass ratioes are 90:10:After 7, mechanical agitation 2h,
Drying obtains cotton-shaped molecular sieve/Mixture of Activated Carbon in 95 DEG C of baking ovens.A small amount of ethanol wet is added into gained mixture,
Roll-in is in blocks and is pressed in titanium net, obtains HSZ-1/ activated carbons (HSZ-1/AC) electrode.
Fig. 1 is the SEM shape appearance figures of HSZ-1/AC electrodes.
The asymmetric capacitive desalination device of assembling, using molecular sieve combination electrode HSZ-1/AC as cathode, pure activated carbon electrodes are
Anode is assembled into symmetric capacitor (AC | | HSZ-1/AC), in the NaCl solution of 500mg/L, setting by voltage 1.2V, into
Row constant current charge-discharge test.Fig. 2 is asymmetric capacitor (AC | | HSZ-1/AC) conductivity and electricity under constant current charge-discharge pattern
Press versus time curve.AC | | the single cycle desalination amount of HSZ-1/AC electrodes is 9.5mg/g, current efficiency 65%.
Embodiment 2
It is doping component to take high silicon content Na type mordenite molecular sieves HSZ-2, and property is as follows：SiO2/Al2O3Mole
Than being 18:1, Na2O/Al2O3Molar ratio is 1：1, particle diameter size is 12 microns.
Compound concentration is the dispersion liquid (dispersion is in deionized water) of 50mg/mL activated carbons and HSZ-2 molecular sieves, is added
PTFE emulsion (mass fraction 60%), activated carbon, HSZ-2 molecular sieves and PTFE mass ratioes are 90:10:After 7, mechanical agitation 2h,
Drying obtains cotton-shaped molecular sieve/Mixture of Activated Carbon in 95 DEG C of baking ovens.It is added into gained HSZ-2/ Mixture of Activated Carbon
A small amount of ethanol wet, roll-in is in blocks and is pressed in titanium net, obtains HSZ-2/ activated carbons (HSZ-2/AC) electrode.Fig. 3 is HSZ-2/
The SEM shape appearance figures of AC electrodes.
The asymmetric capacitive desalination device of assembling, using molecular sieve combination electrode HSZ-2/AC as cathode, pure activated carbon electrodes are
Anode is assembled into symmetric capacitor (AC | HSZ-2/AC), and in the NaCl solution of 500mg/L, setting is carried out by voltage 1.2V
Constant current charge-discharge test.Fig. 4 is asymmetric capacitor (AC | | HSZ-2/AC) conductivity and voltage under constant current charge-discharge pattern
Versus time curve.AC | | the single loop desalination amount of HSZ-1/AC is 8.6mg/g, current efficiency 64%.
Comparative example 1
The preparation and symmetric capacitor desalination of pure activated carbon electrodes are tested.
Compound concentration is 50mg/mL activated carbon mixed liquors, and PTFE emulsion is added；Activated carbon is 100 with PTFE mass ratioes:7,
After mechanical agitation 2h, is dried in 95 DEG C of baking ovens and obtain mixture.A small amount of ethanol wet is added into gained mixture, is rolled into
Piece is simultaneously pressed in titanium net, obtains pure activated carbon (AC) electrode.
The pure activated carbon electrodes of two panels are taken to be assembled into symmetric capacitor (AC | AC), in the NaCl solution of 500mg/L, setting
By voltage 1.2V, constant current charge-discharge test is carried out.The single cycle desalination amount of the pure activated carbon AC electrodes is 4.5mg/g, electric current
Efficiency is 38%.
Claims (1)
1. a kind of capacitive adsorption desalination preparation method of molecular sieve/porous carbon composite electrode material, including：
(1) in deionized water by activated carbon and high silicon content H-type beta-molecular sieve HSZ dispersions, compound concentration is the work of 50mg/mL
Property charcoal and HSZ molecular sieves dispersion liquid, the PTFE emulsion of mass fraction 60% is added, after mechanical agitation 2h, in 95 DEG C of baking ovens
Drying obtains cotton-shaped molecular sieve/Mixture of Activated Carbon；Wherein, activated carbon, HSZ molecular sieves and PTFE mass ratioes are 90:10:7；
The property of HSZ molecular sieves is as follows：SiO2/Al2O3Molar ratio is 40：1, specific surface area 530m2/ g, particle diameter size are 4 micro-
Rice；
(2) ethanol wet is added in the cotton-shaped molecular sieve/Mixture of Activated Carbon obtained to step (1), roll-in is in blocks and is pressed in
In titanium net, HSZ/ active carbon electrode materials are obtained.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006002469A1 (en) * | 2004-07-02 | 2006-01-12 | U.S. Filter Wastewater Group, Inc | Gas transfer membrane |
| CN104342852A (en) * | 2014-10-27 | 2015-02-11 | 东华大学 | Preparation methods of porous carbon nanofiber felt and porous carbon nanofiber electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006002469A1 (en) * | 2004-07-02 | 2006-01-12 | U.S. Filter Wastewater Group, Inc | Gas transfer membrane |
| CN104342852A (en) * | 2014-10-27 | 2015-02-11 | 东华大学 | Preparation methods of porous carbon nanofiber felt and porous carbon nanofiber electrode |
Non-Patent Citations (1)
| Title |
|---|
| 电容吸附法海水脱钙研究;张运秋;《中国优秀硕士学位论文全文数据库-基础科学辑》;20120415(第4期);第34-49页 * |
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