CN109179589A - The preparation method of carbon coating vanadium phosphate sodium electrode material and its application in hydridization capacitive deionization technology - Google Patents
The preparation method of carbon coating vanadium phosphate sodium electrode material and its application in hydridization capacitive deionization technology Download PDFInfo
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- CN109179589A CN109179589A CN201811098070.XA CN201811098070A CN109179589A CN 109179589 A CN109179589 A CN 109179589A CN 201811098070 A CN201811098070 A CN 201811098070A CN 109179589 A CN109179589 A CN 109179589A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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Abstract
The invention discloses a kind of preparation method of carbon coating vanadium phosphate sodium electrode material and its applications in hydridization capacitive deionization technology.Principle of this method based on faraday's capacitor and electric double layer capacitance storage charge, in capacitor deionizing instrument, in the case where certain voltage, one pole is with indefinite form carbon coating vanadium phosphate sodium for faraday's capacitive adsorption sodium ion, another pole is using active carbon as electric double layer capacitance adsorbing chloride ions, to remove sodium chloride, achieve the purpose that desalination, alive size is applied by control and adjusts material can be realized to chloride ion and sodium ion in positive and negative anodes circulation absorption and desorption, it is easy to operate, it is without secondary pollution, and assisted without other chemical substances.Circulation can reach 6.449mmolg to the adsorption capacity of sodium chloride to this method for the first time‑1, and the rate of adsorption can reach 0.40307mmolg‑1·min‑1, it is a kind of desalination process of great prospect.
Description
Technical field
The invention belongs to high-energy source electrochemical technology fields, are related to a kind of preparation side of carbon coating vanadium phosphate sodium electrode material
Method and its application in hydridization capacitive deionization technology.
Background technique
As the problems such as world population increases severely, environmental pollution, gradually aggravates, facing mankind severe drinking water safety danger
Machine.In addition, China is also faced with increasingly severe water resources shortage problem.Show China's fresh water per capita according to related data
Owning amount is only 2200 cubic metres, ranks 121, the world, and the one third of insufficient world's per capita water resource belongs to the whole world per capita
Most deficient one of 13 countries of water resource.However the water consumption in China maintains higher level for a long time, adds water pollution
The problem of increasing bitter accounting, resulting in the shortage of water resources of China's sternness.
For the problem of drinking water sources shortage, most common method is the bitter that will not directly quote or sea
Water is purified, to alleviate freshwater resources crisis in short supply.
Traditional capacitance deionization technology is to add external voltage at porous carbon-based electrode both ends, makes zwitterion in electrostatic field
To the electrode movement with opposite-sign under effect, to be adsorbed on the electrode, water resource is carried out by short circuit or reversal connection power supply
Regeneration.But often there is circulation easily generation anodizing for a long time in traditional carbon-based electrode, adsorption capacity is by material
There is the problems such as coion efficiency influences charge efficiency, therefore need the electrode for occurring novel in the influence of specific surface area
Material carries out desalination processes.
Summary of the invention
It is an object of the present invention to overcome the technology and electrode material itself on the basis of traditional capacitance deionization technology
Deficiency, the preparation method that a kind of carbon coating vanadium phosphate sodium electrode material is provided and its answering in hydridization capacitive deionization technology
With.
A kind of carbon coating vanadium phosphate sodium electrode material is prepared first, which passes through faraday under the action of voltage
Reaction carries out the embedding sodium of removing sodium, and it is smaller by electrode influences to compare traditional carbon electrode；Secondly answering in hydridization capacitive deionization technology
Have higher adsorption capacity with traditional capacitance deionization technology is compared, i.e., add external voltage at porous electrode both ends, make yin-yang from
Son, to the electrode movement with opposite-sign, to be adsorbed on the electrode, is carried out under the action of electrostatic field by reversal connection power supply
Regeneration.Traditional carbon electrode is compared, it is de- to carry out embedding sodium by the way that faraday's reaction occurs for carbon-coated vanadium phosphate sodium system
Sodium, with good electrochemical window, biggish specific capacitance and good stability, to have in capacitive deionization field
There is good application prospect.
In order to achieve the above object, the technical scheme adopted by the invention is that:
A kind of preparation of carbon coating vanadium phosphate sodium electrode material:
(1) ammonium metavanadate and citric acid that molar ratio is 2:3 is added, into deionized water with 150~1000rmin-1?
Even stirring is generated with bubble, and when solution is in yellow transparent, the sodium carbonate and phosphoric acid of molar ratio 1.5:3 are added thereto
Ammonium dihydrogen continues to stir 15-30min with above-mentioned stirring rate, obtains yellow solution A；
(2) by yellow solution A obtained by step (1) as on magnetic stirring apparatus with 150~1000rmin-1Stirring speed
Rate, 70-80 DEG C of thermostatic stir 7-12 hours, so that it is dry to be transferred to vacuum after fading to blue sol B by yellow solution A
Dry case, 50-70 DEG C freeze-day with constant temperature 12-24 hours, obtain fluffy blue cellular precursor C；
(3) precursor C obtained by grinding steps (2) obtains powder, it is transferred in tube furnace, under an argon atmosphere, 10
DEG C/min heating rate, 300-350 DEG C pre-burning 4 hours, after in same atmosphere, identical heating rate is warming up to 700-900 DEG C, permanent
Temperature 7 hours, obtains final product carbon coating vanadium phosphate sodium electrode material.
Further, sodium carbonate described in step (1) can be substituted with the sodium bicarbonate of 2 times of molar ratios.
Further, step (3) the argon atmosphere gas flow rate is 0.3-1ml/min.
Further, the particle size of carbon coating vanadium phosphate sodium electrode material obtained by step (3) is in the micron-scale.
A kind of application of carbon coating vanadium phosphate sodium electrode material in hydridization capacitive deionization technology:
Firstly, the preparation of carbon coating vanadium phosphate sodium electrode and activated carbon electrodes:
(1) after the carbon coating vanadium phosphate sodium electrode material grinding being prepared into above-mentioned, according to mass ratio be 8-10:1:1 with
PVDF, acetylene black are mixed about 6-12 hours and obtain uniformly mixed slurries, slurries is applied on graphite paper collector, very
Empty 60 DEG C of drying, can be obtained indefinite form carbon coating vanadium phosphate sodium electrode；
(2) activated carbon electrodes preparation method is similar to above, and vanadium phosphate sodium is replaced with active carbon.
Then, the assembling of hydridization capacitor deionizing instrument:
(3) according to fixed plate, silica gel pad, collector, vanadium phosphate sodium electrode, organic glass catch basin, diaphragm, anion
Exchange membrane, activated carbon electrodes, collector, silica gel pad, fixed plate sequence successively assemble constitute hydridization capacitor deionizing instrument.
Wherein, organic glass catch basin is hollow plate, is provided with intake-outlet, to achieve the purpose that circulation water inlet.
Finally, desalting performance is tested:
(4) after the assembling of hydridization capacitor deionizing instrument, progress desalting performance test in desalination process is accessed.It is de-
Salt process includes sodium chloride collecting-tank, peristaltic pump, hydridization capacitor deionizing instrument, conductivity meter, and each device is connected by hose.
When work, peristaltic pump fills sodium chloride brine from sodium chloride collecting-tank with the hydridization capacitive deionization that certain rate input is powered
It sets, after absorption, is circulated back to sodium chloride collecting-tank test electrical conductivity of solution.
(5) process of desorption can be realized in reversal connection voltage, and operation is consistent with absorption.
The principle of chlorination sodium ion in the hydridization capacitive deionization technology removal water body are as follows: carbon coating vanadium phosphate sodium is outside
Under conditions of connecing voltage, intracell sodium ion abjection, sodium ion of the reversal connection voltage then in solution can be embedded in lattice again,
To remove the sodium ion in water body, correlated response equation such as Eq (1)；And chloride ion is under the action of external voltage, to activity
Carbon electrode is mobile, is formed on its surface electric double layer and is stored, and when being reversely connected voltage, electric double layer disappears, and chloride ion is desorbed from electrode
Out；Reach the process of material adsorption/desorption circular regeneration as a result,.
The anion-exchange membrane is the common-ion effect reduced in reaction process, to increase charge efficiency.
The peristaltic pump recirculated water flow velocity can be 15ml/min-50ml/min.
The circular regeneration condition are as follows: when absorption, leading to DC voltage is 0.8-2.0V；When desorption, DC voltage is -0.8
~-2.0V.
The influent concentration are as follows: influent concentration 10mM-100mM.
Traditional capacitance deionization technology is to fall ion remaval using carbon-based electrode by forming electric double layer, have absorption
The deficiencies of capacity is small.Electric double layer behavior is compared, battery behavior (i.e. generating body phase faraday's reaction) has bigger specific capacitance, in advance
Show that it is applied and has bigger adsorption capacity in capacitive deionization field.And the present invention utilize hydridization capacitive deionization technology, one
Faraday's reaction occurs for pole, and another pole is still carbon-based electrode；In combination with double advantages of electric double layer behavior and battery behavior, both
Biggish adsorption capacity can be obtained, and can guarantee the rate of adsorption.
Compared with prior art, the beneficial effects of the present invention are: 1. the present invention is based on faraday's capacitor and electric double layer electricity
Hold sodium chloride in removal water body, and can reach recycling.2. adsorption capacity of the present invention is big, the rate of adsorption is high, stablizes
Property is good, can work in high concentration salt water.
Detailed description of the invention
Fig. 1 is the carbon coating vanadium phosphate sodium TEM figure that the embodiment of the present invention 1 provides.
Fig. 2 is the schematic diagram for the hydridization capacitive deionization electrode that the embodiment of the present invention 2 provides.
Fig. 3 is the embedding sodium process schematic of carbon coating vanadium phosphate sodium removing sodium that the embodiment of the present invention 2 provides.
Fig. 4 is the hydridization capacitive deionization adsorption capacity figure that the embodiment of the present invention 2 provides.
Fig. 5 is the concentration that the embodiment of the present invention 3 provides when being 100mM sodium chloride, hydridization capacitive deionization removal rate figure.
Fig. 6 is voltage and current variation schematic diagram during the adsorption/desorption that the embodiment of the present invention 3 provides recycles.
Specific embodiment
The following examples are not intended to limit the scope of the invention to further explanation of the invention.
Embodiment 1
The preparation of carbon coating vanadium phosphate sodium:
(1) it weighs citric acid and ammonium metavanadate is respectively that 3.84g, 2.34g are added in 100ml deionized water, with 200r
min-1Uniform stirring is generated with bubble, when solution is in yellow transparent, is added in solution 1.59g is gradually added thereto
Sodium carbonate and 3.45g ammonium dihydrogen phosphate continue to stir 30min with above-mentioned stirring rate, obtain yellow solution A；
(2) by yellow solution A obtained by step (1) as on magnetic stirring apparatus with 500rmin-1Stirring rate, 80 DEG C
Thermostatic stir 12 hours so that vacuum oven is transferred to after fading to blue sol B by yellow solution A, in 60 DEG C of perseverances
Temperature is 24 hours dry, obtains fluffy blue cellular precursor C；
(3) precursor C obtained by grinding steps (2) obtains powder, it is transferred in tube furnace, under an argon atmosphere, 10
DEG C/min heating rate, 350 DEG C pre-burning 4 hours, after in same atmosphere, identical heating rate is warming up to 900 DEG C, constant temperature 7 hours,
Obtain final product carbon coating vanadium phosphate sodium electrode material.Obtained vanadium phosphate sodium TEM is as shown in Figure 1.
Embodiment 2
Application of the carbon coating vanadium phosphate sodium electrode material in hydridization capacitive deionization technology.
The preparation of carbon coating vanadium phosphate sodium electrode and activated carbon electrodes:
The carbon coating vanadium phosphate sodium and active carbon that will be prepared into are respectively 8:1:1 and PVDF according to mass ratio, and acetylene black is mixed
It closes to be added NMP stir about 6 hours and obtains uniformly mixed slurries, slurries are applied on graphite paper collector, 60 DEG C of vacuum bakings
It is dry to can reach indefinite form carbon coating vanadium phosphate sodium electrode and activated carbon electrodes；
Desalting performance test:
Using 10mM sodium chloride solution rinse hydridization capacitor deionizing instrument, back testing solution tank in 45ml chlorine is added
Change sodium solution, constantly recycle, until conductivity is basicly stable；On the basis of above-mentioned steps, constant electricity is added to electrode both ends
Pressure starts desalination, while the variation of record current and electrical conductivity of solution, and wherein the every 5s record of electric current is primary, the every 30s note of conductivity
Record is primary；When electrical conductivity of solution reaches it is basicly stable when, i.e., experiment absorption complete.Adsorption process schematic diagram is shown in that Fig. 2, sodium ion exist
To vanadium phosphate sodium electrode movement under the action of electric field, chloride ion is mobile to activated carbon electrodes.It is reversely connected voltage, continues experiment, experiment
Data are exported by computer after the completion.Fig. 3 illustrates the material variation of sodium ion in body phase lattice during adsorption and desorption
Process.Its absorption property compares the carbon-based capacitive deionization absorption of tradition as shown in figure 4, adsorption capacity has reached 2.0365mol/g
Capacity increases, and has wider application prospect.
Embodiment 3
Application of the carbon coating vanadium phosphate sodium electrode material in hydridization capacitive deionization technology.
The preparation of carbon coating vanadium phosphate sodium electrode and activated carbon electrodes:
The carbon coating vanadium phosphate sodium and active carbon being prepared into are respectively 10:1::1 and PVDF according to mass ratio, and acetylene black is mixed
It closes to be added NMP stir about 12 hours and obtains uniformly mixed slurries, slurries are applied on graphite paper collector.60 DEG C of vacuum bakings
It is dry to can reach indefinite form carbon coating vanadium phosphate sodium electrode and activated carbon electrodes；
Desalting performance test:
Using 100mM sodium chloride solution rinse test device, back testing solution tank in 45ml sodium chloride solution is added,
Constantly circulation, until conductivity is basicly stable；On the basis of above-mentioned steps, constant voltage is added to electrode both ends, starts to take off
Salt, while the variation of record current and electrical conductivity of solution, wherein the every 5s record of electric current is primary, and the every 30s record of conductivity is primary；When
When electrical conductivity of solution reaches basicly stable, i.e. experiment absorption is completed, and is reversely connected voltage, is repeatedly recycled, data are exported after the completion of experiment,
As a result such as Fig. 5.Known by Fig. 5, the rate of adsorption has reached 0.403mmol/min, higher than the suction of the carbon-based capacitive deionization technology of tradition
Attached capacity.In addition, Fig. 6 shows the variation tendency of electric current and voltage in the first two cyclic process, illustrate carbon coating vanadium phosphate sodium
Electrode is with good stability in desalination processes.
Foregoing description is only the description to present pre-ferred embodiments, is not any restriction to the scope of the invention.Appoint
Any change or modification what those skilled in the art makes according to the technology contents of the disclosure above should all regard
For equivalent effective embodiment, the range of technical solution of the present invention protection is belonged to.
Claims (10)
1. a kind of preparation method of carbon coating vanadium phosphate sodium electrode material, which comprises the steps of:
(1) ammonium metavanadate and citric acid that molar ratio is 2:3 is added, into deionized water with 150~1000rmin-1Uniformly stir
It mixes, is generated with bubble, when solution is in yellow transparent, the sodium carbonate and biphosphate of molar ratio 1.5:3 are added thereto
Ammonium continues to stir 15-30min with above-mentioned stirring rate, obtains yellow solution A；
(2) by yellow solution A obtained by step (1) as on magnetic stirring apparatus with 150~1000rmin-1Stirring rate, 70-
80 DEG C of thermostatic stirs 7-12 hours, so that it is transferred to vacuum oven after fading to blue sol B by yellow solution A,
50-70 DEG C freeze-day with constant temperature 12-24 hours, obtain fluffy blue cellular vanadium phosphate sodium precursor C；
(3) vanadium phosphate sodium precursor C obtained by grinding steps (2) obtains powder, it is transferred in tube furnace, in argon atmosphere
Under, 10 DEG C/min heating rate, 300-350 DEG C pre-burning 4 hours, after in same atmosphere, identical heating rate is warming up to 700-900
DEG C, constant temperature 7 hours, obtain final product carbon coating vanadium phosphate sodium.
2. the preparation method of carbon coating vanadium phosphate sodium electrode material according to claim 1, it is characterised in that: step (1)
Described in the sodium bicarbonates of 2 times of molar ratios of sodium carbonate substitute.
3. the preparation method of carbon coating vanadium phosphate sodium electrode material according to claim 1, it is characterised in that: step (3)
The gas flow rate of the argon atmosphere is 0.3-1ml/min.
4. a kind of carbon coating vanadium phosphate sodium electrode material that the preparation method as described in claims 1 to 3 is any obtains.
5. carbon coating vanadium phosphate sodium electrode material according to claim 4, it is characterised in that: the carbon coating vanadium phosphate sodium
The particle size of electrode material is in the micron-scale.
6. application of the carbon coating vanadium phosphate sodium electrode material as claimed in claim 4 in hydridization capacitive deionization technology,
It is characterized in that, comprises the following processes:
The preparation of carbon coating vanadium phosphate sodium electrode and activated carbon electrodes:
It (1) is 8-10:1::1 and PVDF, acetylene black according to mass ratio after grinding the carbon coating vanadium phosphate sodium electrode material
It is mixed about 6-12 hours and obtains uniformly mixed slurries, slurries are applied on graphite paper collector, 60 DEG C of vacuum drying,
Indefinite form carbon coating vanadium phosphate sodium electrode can be obtained；
It (2) is 8-10:1::1 and PVDF according to mass ratio by active carbon, acetylene black, which is mixed, obtains mixing for about 6-12 hours
Slurries are applied on graphite paper collector by even slurries, and activated carbon electrodes can be obtained in 60 DEG C of vacuum drying；
The assembling of hydridization capacitor deionizing instrument:
(3) according to fixed plate, silica gel pad, collector, vanadium phosphate sodium electrode, organic glass catch basin, diaphragm, anion exchange
Film, activated carbon electrodes, collector, silica gel pad, fixed plate sequence be successively assembled in constitute hydridization capacitor deionizing instrument in
Constitute hydridization capacitor deionizing instrument；Wherein, organic glass catch basin is hollow plate, is provided with intake-outlet, follows to reach
The purpose of ring water inlet；
Desalting performance test:
(4) it after the assembling of hydridization capacitor deionizing instrument, is accessed in desalination process, desalination process is catchmented using sodium chloride
Pond, peristaltic pump, hydridization capacitor deionizing instrument, conductivity meter execute, and each device is connected by hose；When work, peristaltic pump will
The hydridization capacitor deionizing instrument that sodium chloride brine is powered from sodium chloride collecting-tank with certain rate input, after absorption, is followed
It is looped back to sodium chloride collecting-tank testing conductivity instrument；
(5) process of desorption can be realized in reversal connection voltage, and operation is consistent with absorption.
7. application according to claim 6, it is characterised in that: the peristaltic pump recirculated water flow velocity is 15ml/min-50ml/
min。
8. application according to claim 6, it is characterised in that: the influent concentration in desalting performance test process is 10mM-
100mM。
9. application according to claim 6, it is characterised in that: the circular regeneration condition in desalting performance test process are as follows:
When absorption, leading to DC voltage is 0.8-2.0V；When desorption, DC voltage is -0.8~-2.0V.
10. application according to claim 6, it is characterised in that: in desalting performance test process, when absorption, vanadium phosphate
Sodium electrode connects cathode absorption sodium ion, and activated carbon electrodes connect positive adsorbing chloride ions；Reversal connection voltage can then arrive the purpose of desorption.
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| CN109607711A (en) * | 2019-01-30 | 2019-04-12 | 东莞理工学院 | A kind of hydridization capacitive deionization desalination module and desalination process |
| CN111252870A (en) * | 2020-02-27 | 2020-06-09 | 广东工业大学 | Magnetic nano-coated cross-linked polymer carbon electrode material and preparation method and application thereof |
| CN111252870B (en) * | 2020-02-27 | 2022-09-06 | 广东工业大学 | Magnetic nano-coated cross-linked polymer carbon electrode material and preparation method and application thereof |
| CN111342022A (en) * | 2020-03-12 | 2020-06-26 | 东莞理工学院 | Carbon-coated Na3MnTi(PO4)3/C composite material electrode and preparation method and application thereof |
| CN111362247A (en) * | 2020-03-12 | 2020-07-03 | 东莞理工学院 | Carbon-coated sodium super-ion conductor Na3Fe2(PO4)3/C composite material and preparation method and application thereof |
| WO2021179581A1 (en) * | 2020-03-12 | 2021-09-16 | 东莞理工学院 | Composite material, and hybrid capacitive deionization module and desalination method thereof |
| CN111729623A (en) * | 2020-05-24 | 2020-10-02 | 同济大学 | Preparation method and application of three-dimensional copper ferricyanide composite polypyrrole/polyvinyl alcohol conductive hydrogel material |
| CN111762769A (en) * | 2020-05-24 | 2020-10-13 | 同济大学 | Preparation method and application of vanadium sodium oxygen fluorophosphate/graphene composite electrode material |
| CN113077996A (en) * | 2021-03-29 | 2021-07-06 | 同济大学 | Preparation method and application of sodium vanadium oxygen fluorophosphate/graphene composite electrode material |
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Application publication date: 20190111 |