CN106222728B - A kind of preparation method of Kynoar-hexafluoropropene membrane - Google Patents
A kind of preparation method of Kynoar-hexafluoropropene membrane Download PDFInfo
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- CN106222728B CN106222728B CN201610581797.8A CN201610581797A CN106222728B CN 106222728 B CN106222728 B CN 106222728B CN 201610581797 A CN201610581797 A CN 201610581797A CN 106222728 B CN106222728 B CN 106222728B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/04—Electrophoretic coating characterised by the process with organic material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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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 preparation methods of Kynoar hexafluoropropene membrane, comprise the following steps：S1 weighs following material in proportion：Kynoar hexafluoropropene powder, solid-state iodine and acetone；Kynoar hexafluoropropene powder and acetone are added in reaction vessel, reaction vessel are placed in the water-bath of certain temperature, stirs to Kynoar hexafluoropropene powder and is dispersed in acetone by S2；S3 adds in the solid-state iodine of weighing into reaction vessel, in certain temperature water-bath, continues stirring to solid-state iodine and is dissolved in acetone, electrolyte is made；Two panels electrode plates are inserted into electrolyte by S4, through electrophoresis, obtain Kynoar hexafluoropropene membrane.The Kynoar hexafluoropropene membrane prepared by this method is fine and close, even pore distribution；Preparation process is simple, easily operated, and Production Time is short, efficient, suitable for industrialized production and application.
Description
Technical field
The invention belongs to lithium battery material technical fields, and in particular to a kind of system of Kynoar-hexafluoropropene membrane
Preparation Method.
Background technology
Polymer Li-ion battery has gradually attracted the interest of more and more researchers.With now widely used liquid lithium
Ion battery is compared, and polymer Li-ion battery has many advantages, such as can thin type, arbitrary areaization and arbitrary shape.Use aluminium
The lithium polymer battery that modeling laminated film makees shell can reach higher specific capacity, polymer Li-ion battery specific energy
More than 20% can be improved compared to current liquid lithium ionic cell；Polymer Li-ion battery, which also has, to be minimized, is slim
Change, light-weighted feature, can meet the needs of each side such as the micromation of novel electron equipment, lightness, flexibility.Therefore,
Occupancy volume can gradually increase polymer Li-ion battery in the market, have very wide application prospect, be rare
Business opportunities.
In four big critical materials of polymer Li-ion battery, negative material, electrolyte and positive electrode are realized substantially
Production domesticization substitutes, and the localization process of membrane has just started, and in polymer battery cost, membrane accounts for very big ratio
Example, reaches as high as 20%.Membrane primarily serves two big functions in the battery：On the one hand isolation battery plus-negative plate, both avoid because
It contacts directly and that self discharge occurs is even short-circuit；On the other hand lithium ion is allowed by undertaking positive and negative interpolar ion stream circulation passage.
The property of membrane, for example, thickness and uniformity, mechanical (stretching) intensity and puncture intensity, high-temperature behavior, the size of micropore, hole
Footpath is distributed and porosity, to the wetability, imbibition rate and holding capacity of electrolyte, chemistry and electrochemical stability, and air penetrability, with
Interface stability between electrode, skew ratio etc., the strong influence overall performance of battery.Therefore, find a kind of outstanding
Synthesis membrane method come the excellent membrane of synthesis performance to improve battery comprehensive performance play an important role.
At present, the main method for industrially preparing polymer lithium cell diaphragm PVDF-HFP is " phase inversion method ".It concludes
Ground says, " phase inversion method ", which refers to dissolve a polymer at high temperature in the solvent of higher boiling low volatility, forms homogeneous liquid, then drops
Temperature cooling causes the liquid-solid phase separation of solution generation or liquid-liquid phase separation again volatile reagent to be selected to extract high boiling solvent
Out by the dry porous membranes for obtaining certain planform.This method has as a drawback that：1st, carry out at high temperature,
Condition is more demanding, and expends energy；2nd, step is comparatively laborious, and the consuming time is too long, inefficient；3rd, drug needs to volatilize
It goes out, causes medicine loss big, it is not beneficial to environment；4th, membrane distribution of pores is difficult to control, and distribution of pores is uneven, causes electric current
It is unevenly distributed, the final generation for triggering dendrite lithium or dead lithium.
The content of the invention
Present invention aim to address the above problems, provide a kind of efficient, inexpensive Kynoar-hexafluoropropene
The preparation method of membrane.
In order to solve the above technical problems, the technical scheme is that：A kind of system of Kynoar-hexafluoropropene membrane
Preparation Method comprises the following steps：
S1：Following material is weighed in proportion：
Raw material：Kynoar-hexafluoropropene powder and solid-state iodine；
Solvent：Acetone；
S2：Kynoar-hexafluoropropene powder and acetone are added in reaction vessel, reaction vessel is placed in a constant temperature
In the water-bath of degree, stir to Kynoar-hexafluoropropene powder and be dispersed in acetone；
S3：The solid-state iodine of weighing is added in into reaction vessel, in certain temperature water-bath, continues stirring to solid-state iodine and is dissolved in
In acetone, electrolyte is made；
S4：Two panels electrode plates are inserted into electrolyte, through electrophoresis, obtain Kynoar-hexafluoropropene membrane.
In above-mentioned preparation method, in step S1 the mass ratio of Kynoar-hexafluoropropene powder and solid-state iodine for 40~
60：1.Solid-state iodine can not only make Kynoar-hexafluoropropene powder charged, and shifting can be oriented under the action of electric field
It is dynamic, moreover it is possible to accelerate the speed of its electrophoresis.Iodine can also be kept completely separate by cleaning and drying with obtained membrane simultaneously.This
Outside, acetone can be good at dissolving and disperse the wherein most important effect of Kynoar-hexafluoropropene powder and is for use as
Scattered Kynoar-hexafluoropropene powder, the system of solid-state iodine, as long as dosage is enough scattered Kynoar-hexafluoro third
Alkene powder, solid-state iodine on this basis, change acetone dosage, film forming speed and thickness can be influenced, for polyvinylidene fluoride
Alkene-hexafluoropropene membrane nature has no substantial effect.
In above-mentioned preparation method, in step S2, the purpose of stirring in water bath is to make Kynoar-hexafluoropropene powder
It is dispersed in acetone, routine may be employed in bath temperature and mixing time.According to the research of inventor, bath temperature 30
~60 DEG C, mixing time can reach good mixing effect for 2~10min.
In above-mentioned preparation method, the purpose of stirring in water bath is in order to which iodine is made to be dissolved in acetone, and it is equally distributed to form solute
Routine may be employed in electrolyte, bath temperature and mixing time.According to the research of inventor, bath temperature is 15~30 DEG C, is stirred
Good mixing effect can be reached for 5~20min by mixing the time.
In above-mentioned preparation method, electrode plates are common electrode plates in electrophoretic procedures in step S2, and pole piece material can
To select but be not limited to one kind in electro-conductive glass, copper foil, graphite flake.Consider from film-formation result and post-processing efficiency, at this
In invention, it is preferred to use graphite flake as anode pole piece, be coated with the copper foil of graphite as cathode sheet.Polyvinylidene fluoride during electrophoresis
Alkene-hexafluoropropene is adsorbed under the action of electric field force, is deposited in graphite linings, forms Kynoar-hexafluoropropene membrane material
The complex of material and battery cathode material.
In above-mentioned preparation method, application condition in step S4 electrophoretic procedures is held time and electrode spacing can adopt
With routine, the purpose is to Kynoar-hexafluoropropene membrane is generated on cathode sheet；The voltage of application can be with DC voltage
It can also be pulse voltage.Applying alive size and applying mode mainly influences the cause of the thickness of film, film forming speed and film
Close property.It is studied according to inventor, considers that it is preferably 35-80V to apply voltage, and electrophoresis time can root from the effect angle of film forming
It is determined according to voltage and the Kynoar-hexafluoropropene membrane finally set is applied.In the present invention, 1~5cm of electrode spacing,
Electrophoresis time is 5~20min.After the completion of electrophoretic procedures, cathode sheet is removed, natural air drying or drying obtain polyvinylidene fluoride
Alkene-hexafluoropropene membrane.
The beneficial effects of the invention are as follows：
1st, economize on resources, reduce pollution.In preparation method of the present invention, Kynoar-hexafluoropropene powder, acetone and
Iodine can reuse, and after completing an electrophoresis, can add in appropriate Kynoar-hexafluoropropene powder in acetone again
Or iodine continues electrophoresis next time, greatly reduces the loss of acetone, is conducive to save great amount of cost, while reduces industry
Produce the pollution to environment；
2nd, film speed is fast, efficient.Preparation method provided by the invention, film step is simple, is easily achieved, and entire
Film-forming process need not be for a long time.Laboratory is prepared separately a film and can be completed in 30 minutes, commercial scale institute
It takes time shorter.Each due to film can be carried out at the same time step by step, disregard embathe, baking step, industrially about 20 minutes
A collection of membrane can be prepared, compared to traditional " phase inversion method ", production efficiency is substantially improved.
3rd, membrane thicknesses, controlled shape.The conditions such as time, temperature, ingredient dose by controlling electrophoresis can change every
The thickness of film can change the shape of membrane by the shape for changing cathode sheet.
4th, preparation method provided by the invention, it is several when the direct electrophoretic deposition of the membrane of preparation is when on battery cathode material
There is no the problem of skew ratio, the battery short circuit that dislocation occurs and directly results between membrane and pole piece can be effectively avoided, is carried
The yield rate of high battery production, and reduce the number of assembling steps of industrial upper diaphragm and electrode, industrial production can be effectively improved
Efficiency.
5th, using preparation method provided by the invention, the membrane even pore distribution of preparation, porosity is high, to electrolyte
Wetability, imbibition rate and holding capacity are strong.In addition, the good bending property for the membrane produced, meets the requirement in terms of flexible battery.
Description of the drawings
Fig. 1 is electrolyte preparation facilities used in the preparation method of Kynoar of the present invention-hexafluoropropene membrane；
Fig. 2 is electrophoretic apparatus used in the preparation method of Kynoar of the present invention-hexafluoropropene membrane.
Reference sign：1st, magnetic agitation water-bath；2nd, round-bottomed flask；3rd, bottle stopper；4. temperature sensor；5th, capping；
6th, electrophoresis tank；7th, graphite flake；8th, electro-conductive glass；9th, copper foil.
Specific embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the drawings and specific embodiments pair
The present invention is described in further detail.
As shown in Figure 1, mixed liquor used in the preparation method of Kynoar of the present invention-hexafluoropropene membrane prepares dress
It puts, including magnetic agitation water-bath 1, round-bottomed flask 2, temperature sensor 3.Round-bottomed flask 2 is positioned over magnetic agitation water-bath 1
In, bottle mouth position is plugged with bottle stopper 3.3 one end of temperature sensor is positioned over magnetic agitation water-bath 1.Magnetic agitation water-bath 1 is used
Kynoar-hexafluoropropene precipitation is prevented in agitating solution, and provides isoperibol to ensure being smoothed out for reaction process.
Round-bottomed flask 2 is the place of the dissolution of raw material such as Kynoar-hexafluoropropene powder, iodine and acetone and reaction.Using such as circle
The arrow-necked bottle of bottom flask 2 can reduce the volatilization of acetone.Aperture is offered on bottle stopper 3, is further subtracted while equilibrium air pressure
The volatilization of few acetone.Temperature sensor 4 for perceive water temperature variation, in order to control temperature, make reaction under controlled condition into
Row.
As shown in Fig. 2, electrophoretic apparatus used in the preparation method of Kynoar of the present invention-hexafluoropropene membrane, bag
Include electrophoresis tank 6.Electrophoresis tank 6 is used to hold electrolyte and provides the reacting environment of electrophoresis process.Capping 5, slot are set on electrophoresis tank 6
Lid 5 is covered when electrophoresis carries out, and can effectively place acetone volatilization.Anode pole piece graphite flake 7 and electro-conductive glass 8 are respectively placed in
The both ends of electrophoresis tank, electro-conductive glass 8 is for conducting electric current and carries cathode sheet copper foil 9.
Embodiment 1
In the present embodiment, Fig. 1 and Fig. 2 shown devices are respectively adopted, electrophoresis is prepared and implemented for electrolyte.
S1：Raw material：It is 40 in mass ratio：1 weighs Kynoar-hexafluoropropene powder and solid-state iodine
Solvent：Proper amount of acetone；
S2：Kynoar-hexafluoropropene powder and acetone are added in round-bottomed flask 2, round-bottomed flask 2 is positioned over magnetic
In power stirring water-bath 1, when bath temperature is about 30 DEG C or so, mixing time is about 8-10min, until Kynoar-six
Fluoropropene powder is dispersed in acetone；
S3：The solid-state iodine of weighing is added in into round-bottomed flask 2, when bath temperature is about 15 DEG C or so, mixing time is about
For 15-20min, until solid-state iodine is dissolved in acetone, electrolyte is made；
S4：Electrolyte is poured into electrophoresis tank 6, graphite flake 7 and electro-conductive glass 8 are inserted into electrolyte, is applied big
During the DC voltage of about 35V or so, electrode spacing 1-5cm, electrophoresis about 10-20min obtain Kynoar-hexafluoropropene
Membrane.
Embodiment 2
In the present embodiment, Fig. 1 and Fig. 2 shown devices are respectively adopted, electrophoresis is prepared and implemented for electrolyte.
S1：Raw material：It is 45 in mass ratio：1 weighs Kynoar-hexafluoropropene powder and solid-state iodine
Solvent：Proper amount of acetone；
S2：Kynoar-hexafluoropropene powder and acetone are added in round-bottomed flask 2, round-bottomed flask 2 is positioned over magnetic
In power stirring water-bath 1, when bath temperature is about 40 DEG C or so, mixing time is about 6-8min, until Kynoar-hexafluoro
Propylene powder is dispersed in acetone；
S3：The solid-state iodine of weighing is added in into round-bottomed flask 2, when bath temperature is about 20 DEG C or so, mixing time is about
For 12-17min, until solid-state iodine is dissolved in acetone, electrolyte is made；
S4：Electrolyte is poured into electrophoresis tank 6, graphite flake 7 and electro-conductive glass 8 are inserted into electrolyte, is applied big
During the DC voltage of about 50V or so, electrode spacing 1-5cm, electrophoresis about 8-18min, obtain Kynoar-hexafluoropropene every
Film.
Embodiment 3
In the present embodiment, Fig. 1 and Fig. 2 shown devices are respectively adopted, electrophoresis is prepared and implemented for electrolyte.
S1：Raw material：It is 55 in mass ratio：1 weighs Kynoar-hexafluoropropene powder and solid-state iodine
Solvent：Proper amount of acetone；
S2：Kynoar-hexafluoropropene powder and acetone are added in round-bottomed flask 2, round-bottomed flask 2 is positioned over magnetic
In power stirring water-bath 1, when bath temperature is about 50 DEG C or so, mixing time is about 4-6min, until Kynoar-hexafluoro
Propylene powder is dispersed in acetone；
S3：The solid-state iodine of weighing is added in into round-bottomed flask 2, when bath temperature is about 25 DEG C or so, mixing time is about
For 9-14min, until solid-state iodine is dissolved in acetone, electrolyte is made；
S4：Electrolyte is poured into electrophoresis tank 6, graphite flake 7 and electro-conductive glass 8 are inserted into electrolyte, is applied big
During the DC voltage of about 65V or so, electrode spacing 1-5cm, electrophoresis about 6-16min, obtain Kynoar-hexafluoropropene every
Film.
Embodiment 4
In the present embodiment, Fig. 1 and Fig. 2 shown devices are respectively adopted, electrophoresis is prepared and implemented for electrolyte.
S1：Raw material：It is 60 in mass ratio：1 weighs Kynoar-hexafluoropropene powder and solid-state iodine
Solvent：Proper amount of acetone；
S2：Kynoar-hexafluoropropene powder and acetone are added in round-bottomed flask 2, round-bottomed flask 2 is positioned over magnetic
In power stirring water-bath 1, when bath temperature is about 60 DEG C or so, mixing time is about 2-4min, until Kynoar-hexafluoro
Propylene powder is dispersed in acetone；
S3：The solid-state iodine of weighing, 30 DEG C, mixing time 5-15min of bath temperature, until solid-state are added in into round-bottomed flask 2
Iodine is dissolved in acetone, and electrolyte is made；
S4：Electrolyte is poured into electrophoresis tank 6, graphite flake 7 and electro-conductive glass 8 are inserted into electrolyte, is applied big
About the DC voltage of 80V or so when, electrode spacing 1-5cm, electrophoresis about 5-15min obtain Kynoar-hexafluoropropene
Membrane.
In conclusion the present invention prepares electrolyte using Kynoar-hexafluoropropene, iodine and acetone, by simple
The electrophoresis easily realized prepares fine and close Kynoar-hexafluoropropene membrane.Kynoar prepared by the preparation method-
Hexafluoropropene membrane shape, thickness are controllable, even pore distribution, are conducive to the various requirement for meeting novel electronic product.Into one
Step ground, the present invention provide a kind of new way for the preparation of battery diaphragm, help to prepare battery diaphragm further
Optimization and improvement.Compared to industrial " phase inversion method ", film speed can be not only substantially improved in preparation method provided by the invention,
Production efficiency is improved, great amount of cost can also be saved.This can not only promote industrialized production and the marketization of battery diaphragm significantly
Sale, moreover it is possible to promote the development and progress of polymer Li-ion battery industry, echo the new energy development strategy in China.
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair
Bright principle, it should be understood that protection scope of the present invention is not limited to such special statement and embodiment.This field
Those of ordinary skill these disclosed technical inspirations can make according to the present invention and various not depart from the other each of essence of the invention
The specific deformation of kind and combination, these deform and combine still within the scope of the present invention.
Claims (7)
1. a kind of preparation method of Kynoar-hexafluoropropene membrane, it is characterised in that：Comprise the following steps：
S1：Following material is weighed in proportion：
Raw material：Kynoar-hexafluoropropene powder and solid-state iodine；
Solvent：Acetone；
The mass ratio of Kynoar-hexafluoropropene powder and solid-state iodine is 40~60：1；
S2：Kynoar-hexafluoropropene powder and acetone are added in reaction vessel, reaction vessel is placed in certain temperature
In water-bath, stir to Kynoar-hexafluoropropene powder and be dispersed in acetone；
S3：The solid-state iodine of weighing is added in into reaction vessel, in certain temperature water-bath, continues stirring to solid-state iodine and is dissolved in acetone
In, electrolyte is made；
S4：Two panels electrode plates are inserted into electrolyte, through electrophoresis, obtain Kynoar-hexafluoropropene membrane；The electricity
Pole pole piece material is electro-conductive glass, one kind in copper foil, graphite flake, and the copper foil surface is coated with graphite linings.
2. the preparation method of Kynoar according to claim 1-hexafluoropropene membrane, it is characterised in that：The step
In rapid S2, bath temperature is 30~60 DEG C.
3. the preparation method of Kynoar according to claim 1-hexafluoropropene membrane, it is characterised in that：The step
In rapid S3, bath temperature is 15~30 DEG C.
4. the preparation method of Kynoar according to claim 1-hexafluoropropene membrane, it is characterised in that：The step
In rapid S2, mixing time is 2~10min.
5. the preparation method of Kynoar according to claim 1-hexafluoropropene membrane, it is characterised in that：The step
In rapid S3, mixing time is 5~20min.
6. the preparation method of Kynoar according to claim 1-hexafluoropropene membrane, it is characterised in that：The step
In rapid S4, deposition condition is：Apply voltage 35-80V, electrophoresis is to setting Kynoar-hexafluoropropene membrane thicknesses；Electrophoresis is complete
Cheng Hou removes cathode sheet, and natural air drying or drying obtain Kynoar-hexafluoropropene membrane.
7. the preparation method of Kynoar according to claim 6-hexafluoropropene membrane, it is characterised in that：The step
In rapid S4,1~5cm of electrode spacing, electrophoresis time is 5~20min.
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| CN110085791A (en) * | 2019-04-11 | 2019-08-02 | 电子科技大学 | A kind of lithium ion battery separator and preparation method thereof |
| CN110289382A (en) * | 2019-07-23 | 2019-09-27 | 深圳锂硫科技有限公司 | A kind of preparation method and lithium battery diaphragm of lithium battery diaphragm |
| CN110408281A (en) * | 2019-08-20 | 2019-11-05 | 西安鸿钧睿泽新材料科技有限公司 | Heat-insulated, energy-saving coating of one kind and preparation method thereof |
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