CN109336227A - Unformed phosphoric acid iron electrode material of graphene coated and preparation method thereof - Google Patents
Unformed phosphoric acid iron electrode material of graphene coated and preparation method thereof Download PDFInfo
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- CN109336227A CN109336227A CN201811020100.5A CN201811020100A CN109336227A CN 109336227 A CN109336227 A CN 109336227A CN 201811020100 A CN201811020100 A CN 201811020100A CN 109336227 A CN109336227 A CN 109336227A
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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 belongs to electrode material preparation technical field, a kind of unformed ferric phosphate of graphene coated and preparation method thereof is disclosed.The preparation method includes: that six ferrous sulfate hydrate ammoniums are dissolved in graphene oxide solution, and lauryl sodium sulfate, phosphoric acid and urea are added thereto, is vigorously stirred later 10 minutes.Obtained solution is transferred in water heating kettle, the hydro-thermal 12h at 80 DEG C.Obtained mixture is filtered, and for several times with distilled water and ethanol washing, obtained solid is dried for 24 hours at 60 DEG C, the unformed ferric phosphate of graphene coated can be prepared.Inventing the graphene coated iron phosphate nano ball prepared can be effectively reduced charge transfer resistance, improves capacity, has good effect in hydridization capacitive deionization technology.
Description
Technical field
The invention belongs to electrode material preparation technical field, more particularly to a kind of simple and easy graphene coated are unformed
Phosphoric acid iron electrode material and preparation method thereof.
Background technique
With the increase of population and freshwater resources pollution aggravation, the problem of shortage of water resources, is got worse.Sea water desalination is then
It is a kind of effective way to solve the above problems.It is such as evaporated compared to traditional sea water desalination mode, reverse osmosis technology, capacitor
Deionization technology has the advantages such as quick, low energy consumption, without secondary pollution.But that there is adsorption capacities is low (especially in height for itself
In salinity water) and two drawbacks of charge low efficiency.And one of porous carbon electrodes then are become having by hydridization capacitive deionization
There is the electrode material such as titanium phosphate sodium, sodium manganese oxide, vanadium phosphate sodium etc. of faraday's reaction, this improvement can be improved effectively
Its desalting ability and charge efficiency inhibit the side reaction being difficult to avoid that in traditional capacitance deionization technology.
Unformed ferric phosphate is a kind of common sodium-ion battery material, compared to other materials, with high capacity (reason
It is 178mAh/g by capacity), the advantages that preparation process is simple, low in cost, and nonhazardous acts on, be hydridization capacitive deionization technology
In good material.But the simple unformed ferric phosphate disadvantages such as that there is conductivities is low, charge transfer resistance is big.
Summary of the invention
It is an object of the present invention to overcome the deficiencies of the prior art and provide a kind of unformed phosphoric acid ferroelectricity of graphene coated
Pole material and preparation method thereof.Graphene has good electric conductivity, capacitive character and excellent as a kind of two-dimentional Carbon Materials
Specific surface area, the present invention are effectively improved the defect of unformed ferric phosphate script by the way that graphene and unformed ferric phosphate is compound,
Improve its effect in hydridization capacitive deionization field.
In order to achieve the above object, the technical scheme adopted by the invention is that:
A kind of preparation method of the unformed phosphoric acid iron electrode material of graphene coated, using graphene oxide as oxidation
Agent, six ferrous sulfate hydrate ammoniums form a kind of meso-hole structure of graphene coated by one step hydro thermal method as reducing agent
Iron phosphate nano ball, meso-hole structure are conducive to the infiltration of electrolyte, improve the diffusion rate of sodium ion, improve desalination rate.
Specifically, the preparation method of the unformed phosphoric acid iron electrode material of graphene coated, includes the following steps:
(1) certain density graphite oxide solution is configured in beaker, is put into ultrasound 2h in Ultrasound Instrument, is made former graphite oxide
Graphene oxide solution is separated into ultrasonic procedure；
(2) a certain amount of six ferrous sulfate hydrates ammonium is added in the graphene oxide solution described in step (1), stirring is mixed
It closes uniformly, obtains mixed solution；
(3) a certain amount of lauryl sodium sulfate, phosphoric acid, urea, 800r/ is added into mixed solution obtained by step (2)
It is vigorously stirred 10min under min, obtains reaction system；
The more fully mixed of original material can be made by being vigorously stirred 10min under present invention selection 800r/min, can make Fe2+
More uniform is dispersed on GO lamella, that is to say, that product can be more evenly distributed.
(4) reaction system obtained by step (3) is transferred in water heating kettle, the hydro-thermal reaction 12h at 80 DEG C, it is cooling later old
Change certain time, obtains head product；
Ageing time influences crystallization degree.In the present invention, the time of cooling aging is 4h, system after hydro-thermal reaction
Standby ferric phosphate out does not have obvious lattice, and pattern is mesoporous.
(5) product is obtained by filtration in the head product being prepared in step (4), and for several times with distilled water and ethanol washing,
It is dry at 60 DEG C later, prepare the unformed phosphoric acid iron electrode material of powdered graphene coated.
Further, the concentration of step (1) described graphene oxide is 0.2~0.5mg/mL.
Further, the mass ratio of six ferrous sulfate hydrate ammoniums described in step (2) and graphene oxide described in step (1)
Example is 1:5-1:10.
Further, the molar ratio of six ferrous sulfate hydrate ammoniums described in step (2) and phosphoric acid described in step (3) is 1:
1-1:2。
Further, the matter of lauryl sodium sulfate described in step (3) and six ferrous sulfate hydrate ammoniums described in step (2)
Amount ratio is 1:1-1.5:1
Further, the mass ratio of urea described in step (3) and six ferrous sulfate hydrate ammoniums described in step (2) is
15:1-40:1。
Further, cold described in step (4) to go ageing time for 3-4h.
The present invention is using graphene oxide as oxidant, six ferrous sulfate hydrate ammoniums as reducing agent, in unreacted, band
There is the graphene oxide of negative electricity under electrostatic interaction, by Fe2+It is adsorbed on its surface, oxidation in situ occurs under conditions of hydro-thermal
Reduction and coprecipitation reaction, the unformed iron phosphate nano ball so as to form graphene coated, with meso-hole structure.This hair
Charge transfer resistance can be effectively reduced in the graphene coated iron phosphate nano ball of bright preparation, improves capacity.
Compared with prior art, the beneficial effects of the present invention are: 1. material prepared by the present invention by by graphene with
Unformed ferric phosphate is combined with each other, and improves the electric conductivity of unformed ferric phosphate, reduces charge transfer resistance, can be improved
Its desalting performance and rate.2. prepared by hydro-thermal method of the present invention, during hydro-thermal, unformed ferric phosphate can generate mesoporous
Structure, to improve its specific surface area, the scattering and permeating for being conducive to electrolyte, improve its reaction rate.3. compared to multistep processes
For, the present invention uses one-step method, has simple process, the advantages such as low in cost, product property is good.
Detailed description of the invention
Fig. 1 is the unformed ferric phosphate TEM figure of 1 graphene coated of embodiment.
Fig. 2 is the unformed ferric phosphate high power TEM figure of 1 graphene coated of embodiment
Fig. 3 is the unformed ferric phosphate XRD diagram of 2 graphene coated of embodiment.
Fig. 4 is the unformed ferric phosphate hydridization capacitive deionization performance curve of 2 graphene coated of embodiment.
Specific embodiment
The following examples are not intended to limit the scope of the invention to further explanation of the invention.
Embodiment 1
A kind of preparation method of the unformed phosphoric acid iron electrode material of graphene coated, includes the following steps:
(1) 0.25mg/L graphite oxide solution is configured in 250mL volumetric flask, is put into ultrasonic disperse 2h in Ultrasound Instrument and is obtained
Graphene oxide solution.
(2) graphene oxide solution of 60mL is added in beaker, six ferrous sulfate hydrate ammonium of 0.1176g, stirring is added
It is uniformly mixed, obtains mixed solution.
(3) 0.3g lauryl sodium sulfate, 123uL phosphoric acid and 3.6g urea, 800r/ is added into mixed solution again
10min is stirred under min, obtains reaction system.
(4) reaction system is transferred in water heating kettle, the hydro-thermal 12h at 80 DEG C is cold to remove aging 3h, obtains head product.
(5) obtained head product is obtained by filtration product, and with deionized water and washes of absolute alcohol, then at 60 DEG C
Drying for 24 hours, obtains the unformed phosphoric acid iron electrode material of graphene coated.
Fig. 1 is the unformed ferric phosphate TEM figure of 1 graphene coated of embodiment.It can be seen from the figure that unformed ferric phosphate is in
Existing spherical shape, wherein the part of white is present in unformed ferric phosphate mesoporous (being marked with white box), while in sphere
There is one layer of curved graphene layers (being marked with white dashed line) for periphery, it was demonstrated that the clad structure of graphene.
Fig. 2 is the unformed ferric phosphate high power TEM figure of 1 graphene coated of embodiment.Black is unformed ferric phosphate in figure,
It can be seen that illustrating it wherein without obvious lattice for unformed shape, peripheral spacing of lattice is the theory of 0.35nm and graphene
Spacing 0.34nm is close, illustrates graphene oxide reduction sufficiently, while can be seen that graphene for the packet of unformed ferric phosphate
It covers.
Embodiment 2
A kind of preparation method of the unformed phosphoric acid iron electrode material of graphene coated, includes the following steps:
(1) 0.25mg/L graphite oxide solution is configured in 250mL volumetric flask, is put into ultrasonic disperse 2h in Ultrasound Instrument and is obtained
Graphene oxide solution.
(2) graphene oxide solution of 60mL is added in beaker, six ferrous sulfate hydrate ammonium of 0.1176g, stirring is added
It is uniformly mixed, obtains mixed solution.
(3) 0.3g lauryl sodium sulfate, 58.4uL phosphoric acid and 3.6g urea, 800r/ is added into mixed solution again
10min is stirred under min, obtains reaction system.
(4) reaction system is transferred in water heating kettle, the hydro-thermal 12h at 80 DEG C is cold to remove aging 4h, obtains head product.
(5) by obtained head product filter, and use deionized water and washes of absolute alcohol, then at 60 DEG C dry for 24 hours,
Obtain the unformed iron-phosphate complex of graphene coated.
Fig. 3 is the unformed ferric phosphate XRD diagram of 2 graphene coated of embodiment.It can be seen from the figure that not occurring apparent
Peak, it was demonstrated that prepared material is unformed sample, and the peak of calcined sample is the peak of ferric phosphate, it was demonstrated that graphene
Unformed ferric phosphate is coated to synthesize really.
Fig. 4 is the unformed ferric phosphate hydridization capacitive deionization performance curve of 2 graphene coated of embodiment.It can from figure
Out, as time increases, the conductance of solution takes the lead in reducing, rear to increase.In three circulations, conductivity is raised and reduced
It is the same when value, it was demonstrated that this process is reversible.The desalination for being calculated from the formula the unformed ferric phosphate of graphene coated is held
Amount is 85.94mg/g.
Embodiment 3
(1) 0.25mg/L graphite oxide solution is configured in 250mL volumetric flask, is put into ultrasonic disperse 2h in Ultrasound Instrument and is obtained
Graphene oxide solution.
(2) graphene oxide solution of 20mL is added in beaker, six ferrous sulfate hydrate ammonium of 0.0392g, stirring is added
It is uniformly mixed, obtains mixed solution.
(3) 0.1g lauryl sodium sulfate, 41uL phosphoric acid and 1.5g urea, 800r/min is added into mixed solution again
Lower stirring 10min, obtains reaction system；
(4) reaction system is transferred in water heating kettle, the hydro-thermal 12h at 80 DEG C is cold to remove aging 4h, obtains head product.
(5) by obtained head product filter, and use deionized water and washes of absolute alcohol, then at 60 DEG C dry for 24 hours,
Obtain the unformed iron-phosphate complex of graphene coated.
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 (9)
1. a kind of preparation method of the unformed phosphoric acid iron electrode material of graphene coated, it is characterised in that: use graphene oxide
As oxidant, six ferrous sulfate hydrate ammoniums are as reducing agent, and in unreacted, the graphene oxide with negative electricity is made in electrostatic
Under, by Fe2+It is adsorbed on its surface, and then redox and coprecipitation reaction in situ occur by one step hydro thermal method, from
And form a kind of unformed iron phosphate nano ball electrode material of the meso-hole structure of graphene coated.
2. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 1, which is characterized in that
Include the following steps:
(1) certain density graphite oxide solution is configured in beaker, is put into ultrasound 2h in Ultrasound Instrument, makes former graphite oxide super
Graphene oxide solution is separated into during sound；
(2) a certain amount of six ferrous sulfate hydrates ammonium is added in the graphene oxide solution described in step (1), is stirred
It is even, obtain mixed solution；
(3) a certain amount of lauryl sodium sulfate, phosphoric acid, urea are added into mixed solution obtained by step (2), under 800r/min
10min is stirred, reaction system is obtained；
(4) reaction system obtained by step (3) is transferred in water heating kettle, the hydro-thermal reaction 12h at 80 DEG C, later cool aging one
It fixes time, obtains head product；
(5) product is obtained by filtration in the head product being prepared in step (4), and for several times with distilled water and ethanol washing, later
It is dry at 60 DEG C, prepare the unformed phosphoric acid iron electrode material of powdered graphene coated.
3. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
The concentration of step (1) described graphene oxide is 0.2~0.5mg/mL.
4. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
The mass ratio of graphene oxide described in six ferrous sulfate hydrate ammoniums described in step (2) and step (1) is 1:5-1:10.
5. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
The molar ratio of phosphoric acid described in six ferrous sulfate hydrate ammoniums described in step (2) and step (3) is 1:1-1:2.
6. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
The mass ratio of six ferrous sulfate hydrate ammoniums described in lauryl sodium sulfate described in step (3) and step (2) is 1:1-
1.5:1。
7. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
It is cold described in step (4) to go ageing time for 3-4h.
8. the preparation method of the unformed phosphoric acid iron electrode material of graphene coated according to claim 2, it is characterised in that:
The mass ratio of six ferrous sulfate hydrate ammoniums described in urea described in step (3) and step (2) is 15:1-40:1.
9. a kind of unformed phosphoric acid iron electrode material of the graphene coated that preparation method as described in any of the claims 1 to 8 obtains
Material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113443687A (en) * | 2021-06-10 | 2021-09-28 | 安徽工业技术创新研究院六安院 | Asymmetric capacitor deionization device and application thereof in preparation of irrigation water |
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| CN107978753A (en) * | 2017-11-30 | 2018-05-01 | 湘潭大学 | A kind of bowl-shape hollow carbon sphere/graphene composite materials of ferric phosphate@and its preparation method and application |
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| DE102004053479A1 (en) * | 2004-11-05 | 2006-05-11 | Dilo Trading Ag | Lithium-polymer-system based high duty batteries comprises lithium-intercalable titanate as negative electrode and lithium-intercalable iron phosphate as positive electrode |
| CN102185155A (en) * | 2011-04-15 | 2011-09-14 | 南京师范大学 | Nanometer ferric phosphate hollow sphere/graphene lithium ion battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113443687A (en) * | 2021-06-10 | 2021-09-28 | 安徽工业技术创新研究院六安院 | Asymmetric capacitor deionization device and application thereof in preparation of irrigation water |
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Application publication date: 20190215 |