CN107565161A - A kind of gel polymer electrolyte of blended fiber element and preparation method and application - Google Patents
A kind of gel polymer electrolyte of blended fiber element and preparation method and application Download PDFInfo
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- CN107565161A CN107565161A CN201710761574.4A CN201710761574A CN107565161A CN 107565161 A CN107565161 A CN 107565161A CN 201710761574 A CN201710761574 A CN 201710761574A CN 107565161 A CN107565161 A CN 107565161A
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Abstract
The present invention discloses a kind of gel polymer electrolyte of blended fiber element and preparation method and application, belongs to field of lithium ion battery.This method comprises the following steps：Poly- (vinylidene hexafluoropropene) and cellulose acetate phthalate are dissolved in acetone, stirred, until polymer is completely dissolved, the gel solution of water white transparency, i.e. polymer blend solution is presented；Blank non-woven fabrics is immersed in polymer blend solution, rapid pull-up after several seconds, is dried in vacuo after being placed in air drying；The gelatin polymer barrier film of porous blended fiber element is prepared；During assembled battery, it is that can obtain the plain gel polymer electrolyte of blended fiber that gelatin polymer barrier film is added dropwise into electrolyte in upper and lower surface.Preparation technology of the present invention is simple, and the time is short, and production efficiency is high, and high mechanical strength, and cyclical stability is excellent, and obtained polymer film has splendid absorbency and liquid-maintaining capacity, has good ionic conductivity and interface stability.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of gel polymer electrolyte of blended fiber element and its
Preparation method and application.
Background technology
After the concept of lead-acid battery is suggested, using performances such as high specific energy, long-life and safety as the two of target
Primary cell experienced lead-acid battery, Ni-Cr battery, Ni-MH battery successively.The lithium ion battery stage.And in all energy-storage batteries
In, lithium ion battery has the advantages that energy density is high, had extended cycle life, self discharge is small, memory-less effect, environmentally friendly,
Therefore it is widely used in the fields such as electronic product, power vehicle, is the secondary electricity of the best new green environment protection of current combination property
Pond.However, most of commercial Li-ion batteries use liquid organic electrolyte at present, due to liquid electrolyte flash-point, steam
Force down, mobility it is strong, therefore seepage easily occurs, the potential safety hazard such as burning or even blast be present.To solve safety issue, it is proposed that
Gel polymer electrolyte (GPE), i.e., using polymeric matrix absorbed electrolyte, the organic bath of flowing is held onto, by
Liquid is converted into gel state, reduces the electro-chemical activity of liquid electrolyte.This method is directly effective, and polymer battery chemistry is steady
It is qualitative, cycle life is preferable, but it is low to still suffer from ionic conductivity at room temperature；The problems such as mechanical strength is not high enough, therefore compel to be essential
Want the further research of researcher.
The content of the invention
The shortcomings that in order to overcome prior art and deficiency, primary and foremost purpose of the invention are to provide a kind of blended fiber element
Method for preparing gel polymer electrolyte.This method is simple to operation.
Performance of the invention by comparing the gel polymer electrolyte of the cellulose of blending different proportion, search out machinery
Intensity is good, and chemical stability is strong, the optimal blending ratio of good combination property.
Preparation technology of the present invention is simple, and the time is short, and production efficiency is high, and high mechanical strength, and cyclical stability is excellent, obtains
Polymer film has splendid absorbency and liquid-maintaining capacity.
Another object of the present invention is to provide the gelatin polymer by blended fiber element made from above-mentioned preparation method
Electrolyte.
It is still another object of the present invention to provide the application of the gel polymer electrolyte of above-mentioned blended fiber element.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing gel polymer electrolyte of blended fiber element, comprises the following steps：
(1) polymer blend solution is prepared：By poly- (biasfluoroethylene-hexafluoropropylene) (P (VdF-HFP)) and phthalic acid
Cellulose acetate (CAP) is dissolved in acetone, stirring, until polymer is completely dissolved, the gel solution of water white transparency is presented, i.e., common
Mixed polymer solution；
(2) gelatin polymer barrier film is prepared：Blank non-woven fabrics is immersed in polymer blend solution made from step (1),
Rapid pull-up after several seconds, is dried in vacuo after being placed in air drying；The gelatin polymer of porous blended fiber element is prepared
Barrier film；
(3) gel polymer electrolyte is prepared：During assembled battery, by gelatin polymer barrier film made from step (2) upper
It is the gel polymer electrolyte that can obtain blended fiber element that electrolyte, which is added dropwise, in lower two sides.
Poly- (biasfluoroethylene-hexafluoropropylene) (P (VdF-HFP)) and cellulose acetate described in step (1)
The mass ratio of plain (CAP) is (1~4)：1；Preferably 2：1.
It is poly- (biasfluoroethylene-hexafluoropropylene) (P (VdF-HFP)) and adjacent in polymer blend solution described in step (1)
The total mass fraction of cellulose acetate phthalate (CAP) is 10%~14%；Preferably 12%；
Stirring described in step (1) is 0.5~2h of stirring at 30 DEG C；Preferably 1h is stirred at 30 DEG C；
Non-woven fabrics described in step (2) is polyethylene film, polypropylene screen and polypropylene-ethylene-propylene sandwich diaphragm
In one kind.
The time of air drying described in step (2) is 1~2 hour；Preferably 1h；In atmosphere due to acetone
Volatilization forms porous structure, enables cannot have preferable performance as the barrier film of lithium ion battery originally.
Vacuum drying condition described in step (2) is 40~60 DEG C of 12~24h of vacuum drying；Preferably 60 DEG C of vacuum
Dry 12h；
The thickness of gelatin polymer barrier film described in step (2) is 45~50 μm.
Electrolyte described in step (3) is lithium hexafluoro phosphate (LiPF6), ethylene carbonate (EC), methyl ethyl carbonate
(EMC) formed with diethyl carbonate (DEC), wherein EC：EMC：DEC mass ratioes are 3：5：2, LiPF6Molar concentration be 1mol/
L。
A kind of gel polymer electrolyte of blended fiber element, is prepared by above-mentioned preparation method.
Application of the gel polymer electrolyte of described blended fiber element in lithium ion battery is prepared, specific steps are such as
Under：The gel polymer electrolyte barrier film of above-mentioned blended fiber element is placed between positive pole diaphragm and cathode membrane, you can assembling
Into gel polymer electrolyte lithium-ion battery, above operation is completed in glove box.
The active material of described positive pole diaphragm be cobalt acid lithium, LiMn2O4, lithium nickelate, nickel ion doped, nickle cobalt lithium manganate or
LiFePO4；The active material of described cathode membrane is Delanium, native graphite, carbonaceous mesophase spherules, mesocarbon fibre
Dimension, soft carbon, hard carbon or metal lithium sheet；Described gel polymer electrolyte lithium-ion battery is button cell or soft-package battery.
The principle of the present invention is as follows：
Blending P (VdF-HFP)/CAP polymer that the present invention synthesizes while there is the advantages of P (VdF-HFP) and CAP, use
Infusion method is prepared for being blended the lithium ion battery gel polymer film of the cellulose of different proportion.Because cellulose is a kind of yield
Huge renewable resource, there is fully biodegradable, nontoxic, pollution-free, easily modified, good biocompatibility is renewable
Etc. advantage, its intramolecular also has special hydrogen bond action, the preferable heat resistance of cellulose is assigned, to the wellability of electrolyte
Can preferably, electrochemical stability is good, and the electrical conductivity to improving polymer film, mechanical strength and security performance have certain contribution.
After the gel polymer electrolyte is assembled into battery, electro-chemical test shows：The gel polymer electrolyte chemical property
It is stable, there is good ion transmission performance.P (VdF-HFP)/CAP gel electrolytes are blended and are ensureing that original gel electrolyte is steady
On the premise of qualitative energy, ionic conductivity and mechanical strength improve, and non-woven fabrics reduces as substrate, cost, dirty
Dye reduces.Preparation method is simple to operation.Combination property consideration, the 2 of P (VdF-HFP)/CAP：1 ratio is optimal.
This is bright relative to prior art, has the following advantages and effect：
(1) low cost of raw materials of the present invention, easily obtain, synthesis technique is simple, and yield is high, is produced for technology
Condition is provided, easily carries out Industry Promotion and utilization.
(2) solvent used in the present invention is acetone, and nontoxic, environmental pollution is small, while can also reduce production cost.
(3) polymer film that the present invention is obtained has preferable absorbency and protects fluidity, preferable mechanical strength and boundary
Face stability.
(4) cellulose has been blended in the present invention, than no blending P (VdF-HFP) polymer dielectric have it is higher from
Electron conductivity, mechanical strength and interface stability.
Brief description of the drawings
Fig. 1 is the pick up for the polymer film that 1-4 of the embodiment of the present invention and reference examples 1-2 are prepared, and electrical conductivity is bent
Line.
The mechanical strength curve for the polymer film that Fig. 2 is the embodiment of the present invention 2 and reference examples 1-2 is prepared.
The electrochemical impedance curve for the polymer film that Fig. 3 is the embodiment of the present invention 2 and reference examples 1-2 is prepared；Its
In, (a)：Reference examples 1；(b)：Reference examples 2；(c)：Embodiment 2.
The cycle performance curve for the polymer film that Fig. 4 is the embodiment of the present invention 2 and reference examples 1-2 is prepared.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) 30 DEG C of oil bath pan constant temperature, it is 1 by mass ratio:1 P (VdF-HFP) and CAP are added to three mouthfuls equipped with acetone
In flask, machinery, which continuously stirs to be allowed within one hour fully dissolve, obtains the gel polymer solution that mass fraction is 12%, wherein
Mixing speed is 250r/min, i.e. polymer blend solution.
(2) the polymer blend solution that step (1) obtains is poured into beaker, non-woven fabrics then is immersed into above-mentioned blending gathers
In polymer solution, rapid pull-up after soaking several seconds, 60 DEG C of vacuum drying oven is transferred to after solvent is volatilized 1 hour in atmosphere and is relayed
It is continuous to dry 12 hours, obtain the gelatin polymer barrier film of blended fiber element.The thickness of the film is 45~50 μm.
(3) gelatin polymer barrier film made from step (2) is cut into a diameter of 18mm circular dimension, in glove box
In, electrolyte (1mol/L LiPF are added dropwise on membrane for polymer6+ EC+EMC+DEC, EC：EMC：DEC mass ratioes are 3：5：2),
Obtain the gel polymer electrolyte of the blended fiber element of lithium ion battery.
(4) in glove box, using cobalt acid lithium as positive electrode, using lithium piece as negative pole, gel polymer electrolyte is placed in
Between positive pole and negative pole, button cell is assembled into.
Embodiment 2
(1) 30 DEG C of oil bath pan constant temperature, it is 2 by mass ratio:1 P (VdF-HFP) and CAP are added to three mouthfuls equipped with acetone
In flask, machinery, which continuously stirs to be allowed within one hour fully dissolve, obtains the gel polymer solution that mass fraction is 12%, wherein
Mixing speed is 250r/min, i.e. polymer blend solution.
(2) the polymer blend solution that step (1) obtains is poured into beaker, non-woven fabrics then is immersed into above-mentioned blending gathers
In polymer solution, rapid pull-up after soaking several seconds, 60 DEG C of vacuum drying oven is transferred to after solvent is volatilized 1 hour in atmosphere and is relayed
It is continuous to dry 12 hours, obtain the gelatin polymer barrier film of blended fiber element.The thickness of the film is 45~50 μm.
(3) handled by the step of embodiment 1 (3).
(4) handled by the step of embodiment 1 (4).
Embodiment 3
(1) 30 DEG C of oil bath pan constant temperature, it is 3 by mass ratio:1 P (VdF-HFP) and CAP are added to three mouthfuls equipped with acetone
In flask, machinery, which continuously stirs to be allowed within one hour fully dissolve, obtains the gel polymer solution that mass fraction is 12%, wherein
Mixing speed is 250r/min, i.e. polymer blend solution.
(2) the polymer blend solution that step (1) obtains is poured into beaker, non-woven fabrics then is immersed into above-mentioned blending gathers
In polymer solution, rapid pull-up after soaking several seconds, 60 DEG C of vacuum drying oven is transferred to after solvent is volatilized 1 hour in atmosphere and is relayed
It is continuous to dry 12 hours, obtain the gelatin polymer barrier film of blended fiber element.The thickness of the film is 45~50 μm.
(3) handled by the step of embodiment 1 (3).
(4) handled by the step of embodiment 1 (4).
Embodiment 4
(1) 30 DEG C of oil bath pan constant temperature, it is 4 by mass ratio:1 P (VdF-HFP) and CAP are added to three mouthfuls equipped with acetone
In flask, machinery, which continuously stirs to be allowed within one hour fully dissolve, obtains the gel polymer solution that mass fraction is 12%, wherein
Mixing speed is 250r/min, i.e. polymer blend solution.
(2) the polymer blend solution that step (1) obtains is poured into beaker, non-woven fabrics then is immersed into above-mentioned blending gathers
In polymer solution, rapid pull-up after soaking several seconds, 60 DEG C of vacuum drying oven is transferred to after solvent is volatilized 1 hour in atmosphere and is relayed
It is continuous to dry 12 hours, obtain the gelatin polymer barrier film of blended fiber element.The thickness of the film is 45~50 μm.
(3) handled by the step of embodiment 1 (3).
(4) handled by the step of embodiment 1 (4).
Reference examples：
In addition to not adding CAP (reference examples 2) in step (1), other steps are same as Example 1.In addition, it is right
There is blank non-woven fabrics (reference examples 1) as usual.
Test case：
1st, pick up and ionic conductivity test
In embodiment 1-4 and reference examples 1,2, pick up, the conductance of the blending different proportion cellulose membrane being prepared
Rate curve is as shown in Figure 1.Pick up test is carried out in glove box, and electrical conductivity test is that polymer film is assembled into SS/GPE/
SS forms (SS is steel disc, and GPE is gel polymer electrolyte).It can be seen that the gel polymer electrolyte of blended fiber element
Pick up and electrical conductivity compared to blank control group will be high, and wherein ratio is 2:The imbibition of 1 gel polymer electrolyte
Rate and electrical conductivity highest, this may be attributed to its pore structure, and pick up and ionic conductivity height contribute to the transmission of lithium ion.
2nd, mechanical strength test
In embodiment 2 and reference examples 1,2, the mechanical strength for the blended fiber element film being prepared is as shown in Figure 2.When altogether
After in mixed CAP to P (VdF-HFP), the mechanical strength increase of polymer film, blended fiber element plays product to polymeric membrane mechanical strength
The effect of pole.
3rd, electrochemical impedance is tested
In embodiment 2 and reference examples 1,2, the electrochemical impedance for the blended fiber element film being prepared changes with time
Spectrogram is as illustrated, polymer film assembling form is Li/GPE/Li, and when just starting, electrochemical impedance is more or less the same, over time
Increase, impedance becomes big successively, and as seen from the figure, it is smaller to be mixed with the interface impedance of the polymer film of cellulose, with lithium electricity
The compatibility of pole is more preferable.
4th, cycle performance is tested
Barrier film in embodiment 2 and reference examples 1,2 is assembled into button cell, its structure is that negative pole (Li)/gel gathers
Polymer electrolyte/positive pole (LiCoO2), carry out circulating battery stability test.The test condition of button cell is：Room temperature, 0.5C
Electric current, 3.0~4.4V voltage ranges.It is as shown in Figure 4 to test obtained curve.As seen from the figure, blank non-woven fabrics is due to its aperture
It is too big, battery micro-short circuit is caused, is enclosed so circulation is several with regard to capacity with regard to rapid decay, and the polymer film of unmixed cellulose assembles
Battery capability retention compared to addition cellulose battery capacity it is low.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of method for preparing gel polymer electrolyte of blended fiber element, it is characterised in that comprise the following steps：
(1) polymer blend solution is prepared：Poly- (biasfluoroethylene-hexafluoropropylene) and cellulose acetate phthalate are dissolved in third
In ketone, stirring, until polymer is completely dissolved, the gel solution of water white transparency, i.e. polymer blend solution is presented；
(2) gelatin polymer barrier film is prepared：Blank non-woven fabrics is immersed in polymer blend solution made from step (1), several seconds
Rapid pull-up afterwards, it is dried in vacuo after being placed in air drying；The gelatin polymer barrier film of porous blended fiber element is prepared；
(3) gel polymer electrolyte is prepared：During assembled battery, by gelatin polymer barrier film made from step (2) upper and lower two
It is to obtain the gel polymer electrolyte of blended fiber element that electrolyte, which is added dropwise, in face.
2. the method for preparing gel polymer electrolyte of blended fiber element according to claim 1, it is characterised in that：
The mass ratio of poly- (biasfluoroethylene-hexafluoropropylene) and cellulose acetate phthalate described in step (1) for (1~
4)：1.
3. the method for preparing gel polymer electrolyte of blended fiber element according to claim 1, it is characterised in that：
Poly- (biasfluoroethylene-hexafluoropropylene) and cellulose acetate in polymer blend solution described in step (1)
The total mass fraction of element is 10%~14%.
4. the method for preparing gel polymer electrolyte of blended fiber element according to claim 1, it is characterised in that：
Stirring described in step (1) is 0.5~2h of stirring at 30 DEG C；
The time of air drying described in step (2) is 1~2 hour；
Vacuum drying condition described in step (2) is 40~60 DEG C of 12~24h of vacuum drying.
5. the method for preparing gel polymer electrolyte of blended fiber element according to claim 1, it is characterised in that：
Non-woven fabrics described in step (2) is in polyethylene film, polypropylene screen and polypropylene-ethylene-propylene sandwich diaphragm
It is a kind of.
6. the method for preparing gel polymer electrolyte of blended fiber element according to claim 1, it is characterised in that：
The thickness of gelatin polymer barrier film described in step (2) is 45~50 μm.
7. a kind of gel polymer electrolyte of blended fiber element, it is characterised in that by described in any one of claim 1~6
Preparation method is prepared.
8. application of the gel polymer electrolyte of the blended fiber element described in claim 7 in lithium ion battery is prepared.
9. application according to claim 8, it is characterised in that：
The gel polymer electrolyte of blended fiber element described in claim 7 is placed between positive pole diaphragm and cathode membrane,
It is assembled into gel polymer electrolyte lithium-ion battery.
10. application according to claim 9, it is characterised in that：
The active material of described positive pole diaphragm is cobalt acid lithium, LiMn2O4, lithium nickelate, nickel ion doped, nickle cobalt lithium manganate or phosphoric acid
Iron lithium；The active material of described cathode membrane is Delanium, native graphite, carbonaceous mesophase spherules, mesophase carbon fiber, soft
Carbon, hard carbon or metal lithium sheet；Described gel polymer electrolyte lithium-ion battery is button cell or soft-package battery.
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| CN107565161B (en) | 2019-12-20 |
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