CN108281661A - A kind of graphene carbon nanotube modified anode material stand-by provision and preparation method - Google Patents
A kind of graphene carbon nanotube modified anode material stand-by provision and preparation method Download PDFInfo
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- CN108281661A CN108281661A CN201810087901.7A CN201810087901A CN108281661A CN 108281661 A CN108281661 A CN 108281661A CN 201810087901 A CN201810087901 A CN 201810087901A CN 108281661 A CN108281661 A CN 108281661A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/60—Heating or cooling; Temperature control
- H01M10/61—Types of temperature control
- H01M10/613—Cooling or keeping cold
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/60—Heating or cooling; Temperature control
- H01M10/65—Means for temperature control structurally associated with the cells
- H01M10/655—Solid structures for heat exchange or heat conduction
- H01M10/6554—Rods or plates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/60—Heating or cooling; Temperature control
- H01M10/65—Means for temperature control structurally associated with the cells
- H01M10/656—Means for temperature control structurally associated with the cells characterised by the type of heat-exchange fluid
- H01M10/6567—Liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of graphene carbon nanotube modified anode material stand-by provision and preparation methods.The stand-by provision processed referred in the present invention, pass through the setting of ultrasonic oscillator, ultrasonic wave dispersion can be carried out to case substance in vivo, by the setting of heating plate for being heated in babinet, pass through being equipped with for motor, shaft and agitator arm, to effectively being stirred in babinet, by being equipped with for water filling port and cold rinse bank, cold water can be injected to carry out water-bath.The preparation method referred in the present invention is related to chemistry redox method and hydro-thermal method, redox graphene is prepared by chemical method first, then LiFePO4 is prepared by solwution method, using one kettle way by redox graphene and business carbon nano-tube modification LiFePO4, it is simple and reliable, it is suitble to industrialized production, the stand-by provision processed provided that multiple operating procedures in preparation method can be made to be carried out in the same device, it is simplified, preparation efficiency is made to improve.
Description
Technical field
The present invention relates to lithium ion power battery cathode material preparing technical field, specific field is that a kind of graphene carbon is received
Mitron modified anode material stand-by provision and preparation method.
Background technology
With the fast development of new-energy automobile, lithium-ion-power cell is also expanded rapidly.Therefore to lithium ion battery
Performance requirement it is also higher and higher, the negative material of lithium-ion-power cell is one of current battery area research hot spot.
Graphene and carbon nanotube are all the carbon materials of nano-scale, have great specific surface area, good electric conductivity
And the characteristics such as outstanding mechanical performance.Suitable method is selected to prepare Graphene/carbon nanotube composite material, between them
A kind of synergistic effect can be generated, its various physical and chemical performance is made to be enhanced, thus both carbon materials are in many fields
There is great application prospect.
LiFePO4 is a kind of new type lithium ion battery electrode material.Its main feature is that discharge capacity is big, and it is cheap, it is nontoxic
Property, do not cause environmental pollution.Just competitively realize industrialization production in countries in the world.But the disadvantage one that LiFePO4 bulk density is low
Directly by the ignorance of people and avoidance, solution is not yet received, hinders the practical application of material.Therefore modified phosphate iron lithium anode
Material is one of current research hotspot.
The industrialization and popularization and application of LiFePO4 improve battery security, expand lithium to reducing lithium ion battery cost
Ion battery industry promotes lithium ion battery enlargement, high powerization to have very great meaning, lithium ion battery will be made to exist
Application in middle large-capacity ups, medium-and-large-sized energy-storage battery, electric tool, electric vehicle becomes a reality.Therefore it needs simple and convenient
Preparation method and the mating equipment of reliable graphene and LiFePO4.
Invention content
The purpose of the present invention is to provide a kind of graphene carbon nanotube modified anode material stand-by provision and preparation sides
Method, to solve the problems mentioned in the above background technology.
To achieve the above object, one aspect of the present invention provides a kind of graphene carbon nanotube modified anode material preparation dress
It sets, including babinet, ultrasonic oscillator is uniformly provided in the bottom of the babinet, the bottom centre of the babinet is equipped with leakage fluid dram,
The lateral wall lower end of the leakage fluid dram is equipped with drain shut-off valve, and the madial wall upper end of the leakage fluid dram is connected with fixing sleeve, described
The lower end of fixing sleeve is installed with filter screen, and lifting ear is arranged at the upper end opening of the fixing sleeve, the fixing sleeve
Madial wall upper end is connected with stopper, and the upper end of the stopper is fixed with the lower end of pull rod, and the upper end of the pull rod is equipped with draw ring, institute
It states and is equipped with heating plate on the left and right madial wall of babinet, it is symmetrical on the rear wall of the babinet to be installed with motor branch
Frame, the symmetrically arranged one end of the support of motor far from the babinet are installed with motor, symmetrically arranged institute
The equal axis connection of output end for stating motor has shaft, the symmetrically arranged shaft to run through the front-rear side walls of the babinet, institute
The rear and front end for stating shaft is socketed with sealing ring at the babinet, and the outside of the sealing ring is socketed with axle sleeve, institute
It states axle sleeve to be clamped with the babinet, agitator arm, the case uniformly is installed in the middle part of the lateral wall of the symmetrically arranged shaft
Cold rinse bank is equipped in the middle part of body, the right side wall of the babinet is equipped with water filling port, and the water filling port is equipped with water filling shut-off valve,
The water filling port is connected to the cold rinse bank, and observation cover, the upper end of the observation cover are connected at the upper end opening of the babinet
It is arranged with handle before and after middle part, is connected with infusion port on the left of the upper end of the observation cover, the infusion port is equipped with defeated
The left side wall of liquid shut-off valve, the babinet is equipped with control cabinet, and power switch and control panel are respectively equipped in the control cabinet,
The power switch is connect with external power supply and the control panel respectively by electric conductor, and the control panel passes through electric conductor
It is connect respectively with the ultrasonic oscillator, the motor and the heating plate.
Preferably, the front left side of the control cabinet is hinged with control chamber door.
Preferably, the stopper is made of anti-corrosive rubber material.
Preferably, the observation cover is made of transparent corrosion-resistant plastic material.
Preferably, the lower surface quadrangle of the babinet is respectively and fixedly provided with the upper end of stabilizer blade, and the lower end of the stabilizer blade is equipped with wheel
Son.
Another aspect of the present invention provides a kind of preparation method of graphene carbon nanotube modified anode material, preparation method
Include the following steps：
1）At room temperature, a certain amount of powdered natural graphite is weighed, a certain amount of sodium nitrate is added, is placed in cryostat；It adds certain
Measure the concentrated sulfuric acid；Within a certain period of time, it by the average reaction system of addition several times of a certain amount of potassium permanganate, is kept in reaction process
Temperature of reaction system is not higher than 30 degrees Celsius.Cryostat is withdrawn, 30-40 degrees centigrades are heated to, and is sufficiently stirred 1-3 hours,
Obtain the suspension of brown viscous.A certain amount of water droplet is added in brown suspension, diluted suspension is at 80-100 degrees Celsius
Lower reaction certain time.Wait for that the temperature of suspension is down to 40 degrees Celsius hereinafter, the mixed of certain proportion hydrogen peroxide and distilled water is added
Liquid is closed, glassy yellow graphite oxide dispersion is obtained.It centrifuges, removes supernatant, obtained solid is washed with a certain amount of distillation
It washs, is then washed twice as stated above with 30% hydrochloric acid and ethyl alcohol respectively, finally, with petroleum ether precipitation, then poly- four
Vinyl fluoride membrane filtration obtains yellowish-brown graphene oxide solid after dry.
2）It is raw material by lithium carbonate, ferrous oxalate, ammonium dihydrogen phosphate, acetone is medium, and wet ball grinding 5 to 12 hours dries
It is dry, under protection of argon gas, certain time is calcined, LiFePO4 is obtained.
3）A certain amount of graphene oxide, carbon nanotube, ultrasonic disperse is taken to obtain evenly dispersed solution.Hydrazine hydrate is added
Stirring 3 to 8 hours, is added a certain amount of LiFePO4, stirs 6 to 18 hours, is obtained through graphene, carbon nano-tube modification at room temperature
Lithium iron phosphate positive material.
4）Graphene oxide：The mass ratio of carbon nanotube is 10:1:1 to 50:7:Between 4, with absolute ethyl alcohol mass ratio 1:
10 to 1:Between 50, LiFePO4 temperature programming condition be 5 degrees Celsius per minute, be warming up to 300 degrees Celsius calcine 5 hours, again
600 degrees Celsius are warming up to 10 degrees Celsius per minute to calcine 8 hours, the mass ratio of hydrazine hydrate and graphene oxide is 1:2 to 1:
Between 10,50-180 degrees Celsius of hydrothermal temperature, in 5 to 18 hours reaction time, it is Celsius that vacuum drying oven temperature is adjusted to 50 to 100
Degree is dried, and drying time is 3 to 10 hours
Compared with prior art, the beneficial effects of the invention are as follows：The graphene and carbon nano-tube modification phosphoric acid referred in the present invention
In iron lithium anode material stand-by provision, by the setting of ultrasonic oscillator, ultrasonic wave dispersion can be carried out to case substance in vivo, led to
The setting of leakage fluid dram is crossed, convenient for the waste liquid in babinet is discharged after the reaction, by the setting of drain shut-off valve convenient for opening and closing drain
Mouthful, by the setting of the fixing sleeve with lifting ear, filter screen, convenient for taking out the sediment left after reaction, by being equipped with draw ring
The cooperation of pull rod and stopper setting, avoid part solution flow into leakage fluid dram make reaction carry out it is insufficient cause to waste, and be convenient for
Lift stopper after Fang Fanying, so that the waste liquid after reaction is flowed into leakage fluid dram, by the setting of heating plate for adding in babinet
Heat can pass through sealing ring by being equipped with for motor, shaft and agitator arm to effectively being stirred in babinet
Setting prevents liquid in babinet from being leaked from babinet from shaft, is carried out to the shaft for being cased with sealing ring by the setting of axle sleeve
Support can inject cold water to carry out water-bath, pass through sight by being equipped with for water filling port with water filling shut-off valve and cold rinse bank
It examines the setting of cover and passes through infusion port by the setting of handle convenient for pull-up observation cover convenient for observation box house response situation
Setting, by the setting for shut-off valve of being infused convenient for opening and closing infusion port, passes through control plane convenient for injecting reaction liquid into babinet
Plate, ultrasonic oscillator, motor and heating plate are equipped with, and easily respectively to ultrasonic oscillator, motor and heating
Plate is controlled.The preparation method that the present invention refers to is simple and reliable, is suitble to industrialized production, the stand-by provision processed provided that can make
Multiple operating procedures in preparation method carry out in the same device, are simplified, preparation efficiency is made to improve.
Description of the drawings
Fig. 1 is the main structure diagram of the present invention；
Fig. 2 is the overlooking structure diagram of the present invention；
Fig. 3 is the control cabinet internal structure schematic diagram of the present invention.
In figure：1- babinets, 2- ultrasonic oscillators, 3- leakage fluid drams, 4- drains shut-off valve, 5- fixing sleeves, 6- filter screens, 7- are carried
Ear, 8- stoppers, 9- pull rods, 10- draw rings, 11- heating plates, 12- support of motors, 13- motor, 14- shafts, 15- sealing rings,
16- axle sleeves, 17- agitator arms, 18- cold rinse banks, 19- water filling ports, 20- water fillings shut-off valve, 21- observations cover, 22- handles, 23- are defeated
Liquid mouth, 24- infusions shut-off valve, 25- control cabinets, 26- power switches, 27- control panels, 28- controls chamber door, 29- stabilizer blades, 30-
Wheel.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
- 3 are please referred to Fig.1, the present invention provides a kind of technical solution：A kind of graphene carbon nanotube modified anode material preparation
With device, including babinet 1, it is uniformly provided with ultrasonic oscillator 2 in the bottom of the babinet 1, to be carried out to substance in babinet 1
Ultrasonic wave disperses, and the bottom centre of the babinet 1 is equipped with leakage fluid dram 3, described the waste liquid in babinet 1 to be discharged after the reaction
The lateral wall lower end of leakage fluid dram 3 is equipped with drain shut-off valve 4, convenient for opening and closing leakage fluid dram 3, the madial wall upper end card of the leakage fluid dram 3
Be connected to fixing sleeve 5, the lower end of the fixing sleeve 5 is installed with filter screen 6, filter screen 6 be used to leave after reaction leave it is heavy
Starch, is arranged with lifting ear 7 at the upper end opening of the fixing sleeve 5, the setting of lifting ear 7 convenient for pulling, pull lifting ear 7 facilitate by
Fixing sleeve 5 equipped with filter screen 6 is whole to be lifted, and the madial wall upper end of the fixing sleeve 5 is connected with stopper 8, with to avoid part
Solution, which flows into leakage fluid dram 3, makes reaction progress is insufficient to cause to waste, and the upper end of the stopper 8 is fixed with the lower end of pull rod 9, described
The upper end of pull rod 9 is equipped with draw ring 10, and the setting of draw ring 10 is convenient for pulling, and the pull rod 9 with draw ring 10 is pulled to facilitate and will keep off
Plug 8 lifts, and so that the waste liquid after reaction is flowed into leakage fluid dram 3, is equipped with heating plate 11 on the left and right madial wall of the babinet 1, is used for
It is symmetrical on the rear wall of the babinet 1 to be installed with support of motor 12 to being heated in babinet 1, it is symmetrical arranged
The one end of the support of motor 12 far from the babinet 1 be installed with motor 13, it is symmetrically arranged described electronic
The equal axis connection of output end of machine 13 has shaft 14, motor 13 that shaft 14 is driven to rotate, and the symmetrically arranged shaft 14 is passed through
The front-rear side walls of the babinet 1 are worn, the rear and front end of the shaft 14 is socketed with sealing ring 15 at the babinet 1, close
For preventing liquid leakage from babinet 1 from shaft 14 in babinet 1, the outside of the sealing ring 15 is socketed with axis for seal 15
Set 16, the axle sleeve 16 are clamped with the babinet 1, and axle sleeve 16 is supported the shaft 14 for being cased with sealing ring 15, are convenient for shaft
The lateral wall middle part of 14 rotations, the symmetrically arranged shaft 14 is uniformly equipped with agitator arm 17, and shaft 14 drives paddle
17 rotation of wheel can be equipped with cold rinse bank 18, the right side wall of the babinet 1 to being stirred in babinet 1 in the middle part of the babinet 1
Be equipped with water filling port 19, the water filling port 19 is equipped with water filling shut-off valve 20, for being opened and closed water filling port 19, the water filling port 19 with
The cold rinse bank 18 is connected to, and water filling port 19, which is used to inject cold water to cold rinse bank 18, carries out water-bath, at the upper end opening of the babinet 1
It is connected with observation cover 21, for observing 1 internal-response situation of babinet, handle is arranged with before and after the upper center of the observation cover 21
Hand 22 is connected with infusion port 23, for into babinet 1 for pull-up observation cover 21 on the left of the upper end of the observation cover 21
Reaction liquid is injected, the infusion port 23 is equipped with infusion shut-off valve 24, for being opened and closed infusion port 23, a left side for the babinet 1
Side wall is equipped with control cabinet 25, and power switch 26 and control panel 27, the power switch are respectively equipped in the control cabinet 25
26 are connect with external power supply and the control panel 27 respectively by electric conductor, and whole device provides required electricity using external power supply
Can, power switch 26 to control power supply opening and closing, the control panel 27 by electric conductor respectively with the ultrasonic oscillator 2,
The motor 13 and the heating plate 11 connect, and operation and control panel 27 to ultrasonic oscillator 2, motor 13 and can add respectively
Hot plate 11 is controlled.
Specifically, the front left side of the control cabinet 25 is hinged with control chamber door 28, to protect 25 inside dress of control cabinet
It sets.
Specifically, the stopper 8 is made of anti-corrosive rubber material, it is durable to avoid corroding, and good leak tightness.
Specifically, the observation cover 21 is made of transparent corrosion-resistant plastic material, and it is durable to avoid corroding, convenient for observation
Internal-response situation.
Specifically, the lower surface quadrangle of the babinet 1 is respectively and fixedly provided with the upper end of stabilizer blade 29, stabilizer blade 29 plays babinet 1
The lower end of supporting role, the stabilizer blade 29 is equipped with wheel 30, and the setting of wheel 30 keeps device integrally easy to remove.
Specifically, the graphene carbon nanometer corresponding to the graphene carbon nanotube modified anode material stand-by provision
Pipe modified anode material, preparation method includes the following steps：
1）At room temperature, a certain amount of powdered natural graphite is weighed, a certain amount of sodium nitrate is added, is placed in cryostat；It adds certain
Measure the concentrated sulfuric acid；Within a certain period of time, it by the average reaction system of addition several times of a certain amount of potassium permanganate, is kept in reaction process
Temperature of reaction system is not higher than 30 degrees Celsius.Cryostat is withdrawn, 30-40 degrees centigrades are heated to, and is sufficiently stirred 1-3 hours,
Obtain the suspension of brown viscous.A certain amount of water droplet is added in brown suspension, diluted suspension is at 80-100 degrees Celsius
Lower reaction certain time.Wait for that the temperature of suspension is down to 40 degrees Celsius hereinafter, the mixed of certain proportion hydrogen peroxide and distilled water is added
Liquid is closed, glassy yellow graphite oxide dispersion is obtained.It centrifuges, removes supernatant, obtained solid is washed with a certain amount of distillation
It washs, is then washed twice as stated above with 30% hydrochloric acid and ethyl alcohol respectively, finally, with petroleum ether precipitation, then poly- four
Vinyl fluoride membrane filtration obtains yellowish-brown graphene oxide solid after dry.
2）It is raw material by lithium carbonate, ferrous oxalate, ammonium dihydrogen phosphate, acetone is medium, and wet ball grinding 5 to 12 hours dries
It is dry, under protection of argon gas, certain time is calcined, LiFePO4 is obtained.
3）A certain amount of graphene oxide, carbon nanotube, ultrasonic disperse is taken to obtain evenly dispersed solution.Hydrazine hydrate is added
Stirring 3 to 8 hours, is added a certain amount of LiFePO4, stirs 6 to 18 hours, is obtained through graphene, carbon nano-tube modification at room temperature
Lithium iron phosphate positive material.
4）Graphene oxide：The mass ratio of carbon nanotube is 10:1:1 to 50:7:Between 4, with absolute ethyl alcohol mass ratio 1:
10 to 1:Between 50, LiFePO4 temperature programming condition be 5 degrees Celsius per minute, be warming up to 300 degrees Celsius calcine 5 hours, again
600 degrees Celsius are warming up to 10 degrees Celsius per minute to calcine 8 hours, the mass ratio of hydrazine hydrate and graphene oxide is 1:2 to 1:
Between 10,50-180 degrees Celsius of hydrothermal temperature, in 5 to 18 hours reaction time, it is Celsius that vacuum drying oven temperature is adjusted to 50 to 100
Degree is dried, and drying time is 3 to 10 hours.
Operation principle：The preparation method of the graphene and carbon nano-tube modification lithium iron phosphate positive material that are referred in the present invention
It is related to chemistry redox method and hydro-thermal method, redox graphene is prepared by chemical method first, then passes through solution legal system
Standby LiFePO4, using one kettle way by redox graphene and business carbon nano-tube modification LiFePO4.It is carried in the present invention
And graphene and carbon nano-tube modification lithium iron phosphate positive material stand-by provision in, the setting of ultrasonic oscillator 2 is to right
Substance carries out ultrasonic wave dispersion in babinet 1, and the waste liquid in babinet 1 to be discharged after the reaction, drain is cut for the setting of leakage fluid dram 3
Only the setting of valve 4 pulls lifting ear 7 to facilitate and lifts 5 entirety of fixing sleeve equipped with filter screen 6, to take out convenient for opening and closing leakage fluid dram 3
The setting of the sediment left after being reacted in filter screen 6, stopper 8 makes reaction carry out with to avoid part solution inflow leakage fluid dram 3
It is insufficient to cause to waste, it pulls the pull rod 9 with draw ring 10 to facilitate and lifts stopper 8, the waste liquid after reaction is made to flow into leakage fluid dram
3, the setting of heating plate 11 is for being heated in babinet 1, motor 13 to drive the rotation of shaft 14, shaft 14 to drive paddle
17 rotation of wheel, can be to being stirred in babinet 1, and sealing ring 15 is used to prevent liquid in babinet 1 from being let out from babinet 1 from shaft 14
Leakage, axle sleeve 16 is supported the shaft 14 for being cased with sealing ring 15, by water filling port 19 can be injected to cold rinse bank 18 cold water with into
The setting of row water-bath, observation cover 21 observes cover 21 for observing 1 internal-response situation of babinet, the setting of handle 22 convenient for pull-up,
Infusion port 23 is used to inject reaction liquid into babinet 1, and infusion shut-off valve 24 is used for being opened and closed infusion port 23, whole device
External power supply provides required electric energy, and power switch 26, can be respectively to super by operation and control panel 27 to control power supply opening and closing
Acoustic wave transducer 2, motor 13 and heating plate 11 are controlled.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of graphene carbon nanotube modified anode material stand-by provision, including babinet (1), it is characterised in that：The case
Ultrasonic oscillator (2) is uniformly provided in the bottom of body (1), the bottom centre of the babinet (1) is equipped with leakage fluid dram (3), the row
The lateral wall lower end of liquid mouth (3) is equipped with drain shut-off valve (4), and the madial wall upper end of the leakage fluid dram (3) is connected with fixing sleeve
(5), the lower end of the fixing sleeve (5) is installed with filter screen (6), is arranged at the upper end opening of the fixing sleeve (5)
The madial wall upper end of lifting ear (7), the fixing sleeve (5) is connected with stopper (8), and the upper end of the stopper (8) is fixed with pull rod (9)
Lower end, the upper end of the pull rod (9) is equipped with draw ring (10), heating plate is equipped on the left and right madial wall of the babinet (1)
(11), symmetrical on the rear wall of the babinet (1) to be installed with support of motor (12), it is symmetrically arranged described electronic
The one end of machine support (12) far from the babinet (1) is installed with motor (13), the symmetrically arranged motor
(13) the equal axis connection of output end has shaft (14), the symmetrically arranged shaft (14) to run through the front and back of the babinet (1)
The rear and front end of side wall, the shaft (14) is socketed with sealing ring (15), the sealing ring (15) at the babinet (1)
Outside be socketed with axle sleeve (16), the axle sleeve (16) is clamped with the babinet (1), the symmetrically arranged shaft (14)
Agitator arm (17) is uniformly installed in the middle part of lateral wall, cold rinse bank (18), the babinet are equipped in the middle part of the babinet (1)
(1) right side wall is equipped with water filling port (19), and the water filling port (19) is equipped with water filling shut-off valve (20), the water filling port (19)
It is connected to the cold rinse bank (18), observation cover (21) is connected at the upper end opening of the babinet (1), the observation cover (21)
It is arranged with handle (22) before and after upper center, infusion port (23), institute are connected on the left of the upper end of the observation cover (21)
It states infusion port (23) and is equipped with infusion shut-off valve (24), the left side wall of the babinet (1) is equipped with control cabinet (25), the control
Be respectively equipped with power switch (26) and control panel (27) in case (25), the power switch (26) by electric conductor respectively with outside
Connect power supply and the control panel (27) connection, the control panel (27) by electric conductor respectively with the ultrasonic oscillator
(2), the motor (13) and the heating plate (11) connection.
2. a kind of graphene carbon nanotube modified anode material stand-by provision according to claim 1, it is characterised in that：
The front left side of the control cabinet (25) is hinged with control chamber door (28).
3. a kind of graphene carbon nanotube modified anode material stand-by provision according to claim 1, it is characterised in that：
The stopper (8) is made of anti-corrosive rubber material.
4. a kind of graphene carbon nanotube modified anode material stand-by provision according to claim 1, it is characterised in that：
The observation cover (21) is made of transparent corrosion-resistant plastic material.
5. a kind of graphene carbon nanotube modified anode material stand-by provision according to claim 1, it is characterised in that：
The lower surface quadrangle of the babinet (1) is respectively and fixedly provided with the upper end of stabilizer blade (29), and the lower end of the stabilizer blade (29) is equipped with wheel
(30)。
6. a kind of graphene carbon nanotube modified anode material stand-by provision according to claim 1, it is characterised in that：
Graphene carbon nanotube modified anode material corresponding to the graphene carbon nanotube modified anode material stand-by provision,
Preparation method includes the following steps：
1) a certain amount of powdered natural graphite at room temperature, is weighed, a certain amount of sodium nitrate is added, is placed in cryostat；It adds certain
Measure the concentrated sulfuric acid；Within a certain period of time, it by the average reaction system of addition several times of a certain amount of potassium permanganate, is kept in reaction process
Temperature of reaction system is not higher than 30 degrees Celsius.Cryostat is withdrawn, 30-40 degrees centigrades are heated to, and is sufficiently stirred 1-3 hours,
Obtain the suspension of brown viscous.A certain amount of water droplet is added in brown suspension, diluted suspension is at 80-100 degrees Celsius
Lower reaction certain time.Wait for that the temperature of suspension is down to 40 degrees Celsius hereinafter, the mixed of certain proportion hydrogen peroxide and distilled water is added
Liquid is closed, glassy yellow graphite oxide dispersion is obtained.It centrifuges, removes supernatant, obtained solid is washed with a certain amount of distillation
It washs, is then washed twice as stated above with 30% hydrochloric acid and ethyl alcohol respectively, finally, with petroleum ether precipitation, then poly-
Tetrafluoroethene membrane filtration obtains yellowish-brown graphene oxide solid after dry.
2) it is raw material by lithium carbonate, ferrous oxalate, ammonium dihydrogen phosphate, acetone is medium, and wet ball grinding 5 to 12 hours is dried,
Under argon gas protection, certain time is calcined, LiFePO4 is obtained.
3) a certain amount of graphene oxide, carbon nanotube, ultrasonic disperse is taken to obtain evenly dispersed solution.Hydrazine hydrate stirring 3 is added
To 8 hours, a certain amount of LiFePO4 is added, stirs 6 to 18 hours, is obtained through graphene, the phosphorus of carbon nano-tube modification at room temperature
Sour iron lithium anode material.
4) graphene oxide：The mass ratio of carbon nanotube is 10:1:1 to 50:7:Between 4, with absolute ethyl alcohol mass ratio 1:10 to
1:Between 50, LiFePO4 temperature programming condition is 5 degrees Celsius per minute, is warming up to 300 degrees Celsius and calcines 5 hours, and with every
10 degrees Celsius of minute is warming up to 600 degrees Celsius and calcines 8 hours, and the mass ratio of hydrazine hydrate and graphene oxide is 1:2 to 1:10 it
Between, 50-180 degrees Celsius of hydrothermal temperature, 5 to 18 hours reaction time, vacuum drying oven temperature be adjusted to 50 to 100 degrees Celsius into
Row drying, drying time are 3 to 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810087901.7A CN108281661A (en) | 2018-01-30 | 2018-01-30 | A kind of graphene carbon nanotube modified anode material stand-by provision and preparation method |
Applications Claiming Priority (1)
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