CN113550071A - Polymer film with high lithium ion conductivity and electrostatic spinning preparation method thereof - Google Patents
Polymer film with high lithium ion conductivity and electrostatic spinning preparation method thereof Download PDFInfo
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- CN113550071A CN113550071A CN202010991708.3A CN202010991708A CN113550071A CN 113550071 A CN113550071 A CN 113550071A CN 202010991708 A CN202010991708 A CN 202010991708A CN 113550071 A CN113550071 A CN 113550071A
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- electrostatic spinning
- lithium ion
- ion conductivity
- polymer
- polymer film
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- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 67
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 51
- 229920006254 polymer film Polymers 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 125000001165 hydrophobic group Chemical group 0.000 claims abstract description 4
- 229920005594 polymer fiber Polymers 0.000 claims abstract description 3
- 239000004793 Polystyrene Substances 0.000 claims description 27
- 239000002033 PVDF binder Substances 0.000 claims description 23
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 23
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 21
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 7
- 229920002223 polystyrene Polymers 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004642 Polyimide Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229960001701 chloroform Drugs 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 15
- 230000005684 electric field Effects 0.000 abstract description 5
- 238000001523 electrospinning Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 51
- 239000000243 solution Substances 0.000 description 38
- 238000009987 spinning Methods 0.000 description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- -1 polypropylene Polymers 0.000 description 17
- 239000004743 Polypropylene Substances 0.000 description 11
- 239000012528 membrane Substances 0.000 description 11
- 229920001155 polypropylene Polymers 0.000 description 11
- 239000010409 thin film Substances 0.000 description 11
- CIUQDSCDWFSTQR-UHFFFAOYSA-N [C]1=CC=CC=C1 Chemical compound [C]1=CC=CC=C1 CIUQDSCDWFSTQR-UHFFFAOYSA-N 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 238000012512 characterization method Methods 0.000 description 9
- 238000013329 compounding Methods 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 8
- 125000003277 amino group Chemical group 0.000 description 7
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 description 5
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 description 4
- JUUXYSDWEGIGHM-UHFFFAOYSA-N (4-nitrophenyl)diazene Chemical group [O-][N+](=O)C1=CC=C(N=N)C=C1 JUUXYSDWEGIGHM-UHFFFAOYSA-N 0.000 description 3
- GHDZRIQTRDZCMV-UHFFFAOYSA-N 2-[n-(2-hydroxyethyl)-4-[(4-nitrophenyl)diazenyl]anilino]ethanol Chemical compound C1=CC(N(CCO)CCO)=CC=C1N=NC1=CC=C([N+]([O-])=O)C=C1 GHDZRIQTRDZCMV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- WCVOGSZTONGSQY-UHFFFAOYSA-N 2,4,6-trichloroanisole Chemical compound COC1=C(Cl)C=C(Cl)C=C1Cl WCVOGSZTONGSQY-UHFFFAOYSA-N 0.000 description 1
- OAFMCWZFMIQFBI-UHFFFAOYSA-N 2-[n-ethyl-4-[2-(4-nitrophenyl)ethenyl]anilino]ethanol Chemical compound C1=CC(N(CCO)CC)=CC=C1C=CC1=CC=C([N+]([O-])=O)C=C1 OAFMCWZFMIQFBI-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
- D01D5/0038—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion the fibre formed by solvent evaporation, i.e. dry electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
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- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/56—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/4282—Addition polymers
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention relates to a polymer film with high lithium ion conductivity and an electrostatic spinning preparation method thereof. The polymer fiber composite film containing the chromophore is prepared by adopting an electrostatic spinning process, the generating group molecules are uniformly oriented under the action of a high-voltage electric field in the electrospinning process, and the transmission of lithium ions in the polymer composite film is improved by combining the synergistic effect of hydrophilic groups and hydrophobic groups at two ends of the generating group molecule structure, so that the higher lithium ion conductivity is realized. The electrospinning fiber polymer/chromophore composite film prepared by the method is particularly suitable for being used as a lithium ion battery diaphragm, and provides a new idea for preparing a high-efficiency lithium ion battery diaphragm.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a polymer film with high lithium ion conductivity and an electrostatic spinning preparation method thereof.
Background
With the increase of the world energy consumption, the development of new energy is imminent. Accordingly, more attention has been paid to energy storage to cope with the environmental adverse effects of current fossil fuels. High performance lithium ion batteries are widely used in energy storage devices due to their high energy density, environmental friendliness, and long cycle life. The lithium ion diaphragm is used as an important part of the lithium ion battery, the ionic conductivity of the battery diaphragm is always one of important points concerned by the industry, and the ionic conductivity directly influences the overall performance of the lithium ion battery. The polypropylene film is a lithium battery diaphragm material applied earlier, and the ionic conductivity of the polypropylene film is only 1.7ms-1. This is because the lithium ion conductivity is difficult to increase due to the low porosity of the thin film. In patent CN102629679A and patent CN105374970A, the lithium ion battery polymer diaphragm with a fiber structure is prepared by using an electrostatic spinning technology, so that the porosity of the film is significantly improved, and the lithium ion conductivity is significantly improved. However, with the advancement of science and technology and the rapid development of the social energy field, people have higher performance requirements on lithium ion batteries, so that on the basis of the prior art and previous achievements, it is imperative to explore a method and a technology capable of further improving the lithium ion conductivity of a polymer film.
Disclosure of Invention
The invention relates to a polymer film with high lithium ion conductivity and an electrostatic spinning preparation method thereof. The raw materials used in the invention are all conventional materials and can be obtained through commercial channels.
The invention provides a polymer film with high lithium ion conductivity and an electrostatic spinning preparation method thereof, which comprises the following steps:
(1) dissolving a polymer and a generating group molecule with certain mass in an organic solvent under the stirring action to obtain a mixed solution with certain concentration;
(2) preparing a polymer fiber film by using the mixed solution and adopting an electrostatic spinning method;
(3) and testing the lithium ion conductivity of the composite film prepared under different electrostatic spinning voltages.
Preferably, the polymer in step (1) is one or a mixture of two of polyvinylidene fluoride, polyacrylonitrile, polystyrene, polyimide, polyurethane, polyvinyl alcohol and other high polymers.
Further, the molecular weight of the polymer in the step (1) is 10000-500000, and is preferably 12000-300000.
The group-generating molecule in step (1) is a dipolar molecule (D-pi-A structure molecule) with hydrophilic and hydrophobic groups connected to two ends of the molecule, preferably one or more of the molecular structures shown in figure 12, figure 13, figure 14 and figure 15.
Further, the voltage in the electrospinning process described in step (2) is 2kv to 60kv, preferably 10kv to 40kv, and most preferably 14kv to 30 kv.
Further, the solvent in the step (1) is one or a mixture of several of N, N-dimethylformamide, N-dimethylacetamide, chlorobenzene, acetone, trichloromethane, N-dimethylpyrrolidone and dimethyl sulfoxide.
Further, the mass concentration of the chromophore molecule in the step (1) is 0.01wt% to 6.0wt%, preferably 0.5wt% to 3.0 wt%.
Further, the mass concentration of the polymer in the step (1) is 5.0wt% to 30wt%, preferably 15wt% to 25 wt%.
Further, the propelling speed of the injection pump in the electrostatic spinning process in the step (2) is 0.1ml.h-1～1.5ml.h-1。
Compared with the prior art, the method has the innovation points that:
in the electrostatic spinning process, the solvent is gradually volatilized, the chromophore molecules are in an activated state, and a high-voltage electric field is applied to the generating group molecules under the action of an electrostatic field, so that the generating group molecules with dipole structures are uniformly oriented under the action of the electric field; meanwhile, the synergistic effect of hydrophilic and hydrophobic groups at two ends of the molecular structure of the generating group is combined, so that the lithium ion conductivity of the film is obviously enhanced.
Drawings
FIG. 1: the invention relates to an electrostatic spinning experimental device diagram. In the figure: 1. an injector; 2. a high voltage power supply; 3. receiving a plate; 4. a needle.
FIG. 2: PVDF/DR prepared in inventive example 11The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 3: PVDF/DR prepared in inventive example 219The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 4: PVDF/DR prepared in inventive example 398The ion conductivity number of the composite film is in a relation graph with electrostatic spinning voltage.
FIG. 5: PAN/DR prepared in inventive example 41The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 6: PAN/DR prepared in inventive example 519The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 7: PAN/DR prepared in inventive example 698The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 8: PS/DR prepared in inventive example 71The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 9: in example 8 of the present inventionPrepared PS/DR19The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 10: PS/DR prepared in inventive example 998The ionic conductivity of the composite film is plotted against the electrostatic spinning voltage.
FIG. 11: the relationship graph of the ionic conductivity and the electrostatic spinning voltage of the PS/2- [ ethyl [4- [2- (4-nitrophenyl) vinyl ] phenyl ] amino ] ethanol composite film prepared in the embodiment 10 of the invention is shown.
FIG. 12: examples of the present invention are N-ethyl-N- [ 2-hydroxyethyl ]]-4- [ 4-nitrophenylazo ]]Aniline (DR for short)1) Schematic diagram of the molecular structure of (a).
FIG. 13: examples of the present invention are 2,2- [ [4- [ (4-nitrophenyl) azo ]]Phenyl radical]Amino group]Bis-ethanol (DR for short)19) Schematic diagram of the molecular structure of (a).
FIG. 14: examples of the present invention are 2- [ 3-methyl-4- [ [ 4-nitrophenyl)]Azo compounds]Phenyl radical]Ethylamino group]Ethanol (DR for short)98) Schematic diagram of the molecular structure of (a).
FIG. 15: the molecular structure of 2- [ ethyl [4- [2- (4-nitrophenyl) vinyl ] phenyl ] amino ] ethanol in the embodiment of the invention is shown in the figure.
FIG. 16: PVDF/DR in inventive example 11Raman spectrum of the fiber composite film.
FIG. 17: PVDF/DR in inventive example 11Scanning electron microscope image of the surface topography of the fiber composite film.
The specific implementation method comprises the following steps: in order to illustrate the present invention more clearly, the following examples are given without any limitation to the scope of the present invention.
Example 1: weighing certain mass of Polyvinylidene fluoride (PVDF (Mw = 175000), N-ethyl-N- [ 2-hydroxyethyl)]-4- [ 4-nitrophenylazo ]]Aniline (discrete red 1, DR)1) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is placed in a conical flask and stirred to be dissolved, so as to prepare a spinning solution (PVDF: 20wt%, DR1: 2.0 wt%); the prepared spinning solution is placed in an injector of electrostatic spinning equipment,in the spinning process, the advancing speed of the injector is 0.8ml.h-1The distance from the receiving plate to the needle is 18cm, and PVDF/DR is prepared by electrostatic spinning process under the action of different external electric fields1And (3) compounding the fiber membrane.
Prepared PVDF/DR1The composite film was fabricated using alternating current impedance method (EIS) at CHI600E electrochemical workstation with a test range of 0.01Hz-10^6Hz with an amplitude of 5mv, and then the ionic conductivity was calculated according to the formula. The calculation formula is as follows:
where σ is the ionic conductivity (ms.cm)-1) Then R isbThe bulk resistance (Ω) is shown. d represents the thickness (cm) of the film, S represents the effective contact area (cm) of the sample2）。
The results are shown in FIG. 2: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polyethylene film (by more than 10 times). PVDF/DR1The raman spectrum of the composite film is shown in fig. 16: at 1388cm-1And 1132cm-1The absorption peak is a characteristic peak of N = N tensile vibration and Ph-N = N stretching vibration; at 1334cm-1And 1103cm-1The absorption peak is-NO2And Ph-NO2A characteristic peak of stretching vibration. The data show that the characteristic peaks in the raman spectrum are gradually enhanced with the increase of the spinning voltage, which indicates that the clustered molecules are uniformly oriented under the action of the electric field, so that the ionic conductivity is gradually increased (as shown in fig. 2). FIG. 17 is a scanning electron microscope examination of the composite film showing: the fiber membrane prepared by electrostatic spinning has higher porosity and is beneficial to the absorption of electrolyte.
The Raman spectra and scanning electron microscopy data for examples 2-10 are the same as for example 1, and are not individually analyzed in the following examples.
Example 2: weighing a certain mass of Polyvinylidene fluoride (PVDF), (b) and (c)Mw = 175000), 2,2- [ [4- [ (4-nitrophenyl) azo]Phenyl radical]Amino group]Bis-ethanol (dispersered 19, DR)19) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is stirred and dissolved in a conical flask to prepare a spinning solution (PVDF: 20wt%, DR19: 0.7 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the advancing speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 18cm, and PVDF/DR is prepared by electrostatic spinning process under the action of different external electric fields19And (3) compounding the fiber membrane.
PVDF/DR prepared19The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 3: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 3: weighing certain mass of Polyvinylidene fluoride (PVDF (Mw = 195000), 2- [ 3-methyl-4- [ [ 4-nitrophenyl)]Azo compounds]Phenyl radical]Ethylamino group]Ethanol (discrete red 98, DR)98) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is placed in a conical flask and stirred to be dissolved, so as to prepare a spinning solution (PVDF: 15wt%, DR98: 0.5 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the advancing speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 18cm, and PVDF/DR is prepared by electrostatic spinning process under the action of different external electric fields98And (3) compounding the fiber membrane.
PVDF/DR prepared98The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 4: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 4: weighing a certain mass of polypropyleneNitrile (Polyacrylonitrile, PAN (Mw = 175000), N-ethyl-N- [ 2-hydroxyethyl]-4- [ 4-nitrophenylazo ]]Aniline (discrete red 1, DR)1) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is stirred and dissolved in a conical flask to prepare a spinning solution (PAN: 20wt%, DR1: 2.0 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the advancing speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 18cm, and PAN/DR is prepared by an electrostatic spinning process under the action of different external electric fields1And (3) compounding the fiber membrane.
Prepared PAN/DR1The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 5: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 5: weighing certain mass of Polyacrylonitrile (Polyacrylonitrile, PAN (Mw = 175000), 2,2- [ [4- [ (4-nitrophenyl) azo)]Phenyl radical]Amino group]Bis-ethanol (dispersered 19, DR)19) And an N, N-dimethylacetamide solution, and the mixture is stirred and dissolved in a conical flask to prepare a spinning solution (PAN: 18wt%, DR19: 2.0 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the advancing speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 18cm, and PAN/DR is prepared by an electrostatic spinning process under the action of different external electric fields19And (3) compounding the fiber membrane.
Prepared PAN/DR19The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 6: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 6: weighing a certain mass of polypropyleneAlkenenitrile (Polyacrylonitril, PAN (Mw = 235000), 2- [ 3-methyl-4- [ [ 4-nitrophenyl group]Azo compounds]Phenyl radical]Ethylamino group]Ethanol (discrete red 98, DR)98) And an N, N-dimethylacetamide solution, and the mixture is stirred and dissolved in a conical flask to prepare a spinning solution (PAN: 18wt%, DR98: 2.0 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the injection propulsion speed is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 20cm, and PAN/DR is prepared by an electrostatic spinning process under the action of different external electric fields98And (3) compounding the fiber membrane.
Prepared PAN/DR98The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 7: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 7: weighing Polystyrene (Polystyrene, PS (Mw = 240000), N-ethyl-N- [ 2-hydroxyethyl) with a certain mass]-4- [ 4-nitrophenylazo ]]Aniline (discrete red 1, DR)1) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is stirred and dissolved in a conical flask to prepare a spinning solution (PS: 16wt%, DR1: 0.4 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the propelling speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 20cm, and the PS/DR is prepared by an electrostatic spinning process under the action of different external electric fields1And (3) compounding the fiber membrane.
Prepared PS/DR1The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 8: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 8: weighing a certain mass of polystyrene (Poly)tyrene, PS (Mw = 175000), 2,2- [ [4- [ (4-nitrophenyl) azo]Phenyl radical]Amino group]Bis-ethanol (dispersered 19, DR)19) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is stirred and dissolved in a conical flask to prepare a spinning solution (PS: 20wt%, DR19: 0.7 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the propelling speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 20cm, and the PS/DR is prepared by an electrostatic spinning process under the action of different external electric fields19And (3) compounding the fiber membrane.
Prepared PS/DR19The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 9: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 9: weighing a certain mass of Polystyrene (Polystyrene, PS (Mw = 140000), 2- [ 3-methyl-4- [ [ 4-nitrophenyl group)]Azo compounds]Phenyl radical]Ethylamino group]Ethanol (discrete red 98, DR)98) And an N, N-dimethylacetamide solution, and the N, N-dimethylacetamide solution is stirred and dissolved in a conical flask to prepare a spinning solution (PS: 20wt%, DR98: 0.7 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the propelling speed of the injector is 0.8ml.h in the spinning process-1The distance from the receiving plate to the needle is 20cm, and the PS/DR is prepared by an electrostatic spinning process under the action of different external electric fields98And (3) compounding the fiber membrane.
Prepared PS/DR98The characterization method and the calculation formula of the ion conductivity of the composite film are similar to those of example 1.
The results are shown in FIG. 10: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Example 10: weighing a certain mass of Polystyrene (PS)Mw = 250000), 2- [ ethyl [4- [2- (4-nitrophenyl) vinyl group]Phenyl radical]Amino group]Ethanol (2- [ ethyl [4- [2- (4-nitrophenyl) vinyl)]phenyl]amino]ethanol), and an N, N-dimethylacetylic solution, and the solutions were put in a conical flask and stirred to dissolve, to prepare a spinning solution (PS: 17% by weight of 2- [ ethyl [4- [2- (4-nitrophenyl) vinyl group]Phenyl radical]Amino group]Ethanol: 0.7 wt%); placing the prepared spinning solution into an injector of electrostatic spinning equipment, wherein the propelling speed of the injector is 0.8ml.h in the spinning process-1The distance between the receiving plate and the needle is 20cm, and PS/2- [ ethyl [4- [2- (4-nitrophenyl) vinyl ] is prepared by an electrostatic spinning process under the action of different external electric fields]Phenyl radical]Amino group]Ethanol composite fiber membrane.
The characterization method and the calculation formula of the ionic conductivity of the prepared PS/2- [ ethyl [4- [2- (4-nitrophenyl) vinyl ] phenyl ] amino ] ethanol composite film are similar to those of example 1.
The results are shown in FIG. 11: the lithium ion conductivity of the thin film gradually increases with the increase of the electrostatic spinning voltage. Meanwhile, the lithium ion conductivity of the film is obviously higher than that of a commercial polypropylene film (by more than 10 times).
Claims (9)
1. The invention relates to a polymer film with high lithium ion conductivity and an electrostatic spinning preparation method thereof, which are characterized by comprising the following steps:
(1) dissolving a polymer and chromophore molecules with certain mass in an organic solvent under the stirring action to obtain a mixed solution with certain concentration;
(2) preparing a polymer fiber film by using the mixed solution and adopting an electrostatic spinning method;
(3) and testing the lithium ion conductivity of the composite film prepared under different electrostatic spinning voltages.
2. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the polymer in the step (1) is one or a mixture of two of polyvinylidene fluoride, polyacrylonitrile, polystyrene, polyimide, polyurethane, polyvinyl alcohol and other high polymers.
3. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the molecular weight of the polymer in the step (1) is 10000-500000, and is preferably 12000-300000.
4. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the cluster-generating molecule in step (1) is a dipolar molecule (D-pi-A structure molecule) with hydrophilic and hydrophobic groups respectively connected to two ends of the molecular chain, and preferably is a mixture of one or more of the molecular structures shown in figure 12, figure 13, figure 14 and figure 15.
5. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the voltage in the electrostatic spinning process in the step (2) is 2kv to 60kv, preferably 10kv to 40kv, and most preferably 14kv to 30 kv.
6. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the solvent in the step (1) is one or a mixture of several of N, N-dimethylformamide, N-dimethylacetamide, chlorobenzene, acetone, trichloromethane, N-dimethylpyrrolidone and dimethyl sulfoxide.
7. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the mass concentration of the chromophore molecule in the step (1) is 0.01wt% -6.0 wt%, preferably 0.5wt% -3.0 wt%.
8. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the mass concentration of the polymer in the step (1) is 5.0wt% -30 wt%, and preferably 15wt% -25 wt%.
9. The polymer film with high lithium ion conductivity and the electrostatic spinning preparation method thereof according to claim 1 are characterized in that: the propelling speed of the injection pump in the electrostatic spinning process in the step (2) is 0.1ml.h-1～1.5ml.h-1。
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| CN108385273A (en) * | 2018-05-09 | 2018-08-10 | 长春工业大学 | A kind of regulatable film electrostatic spinning preparation method of parent/hydrophobicity |
| CN110165291A (en) * | 2018-02-11 | 2019-08-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Solid electrolyte and the preparation method and application thereof |
| CN111244367A (en) * | 2020-03-01 | 2020-06-05 | 华中科技大学 | Preparation method of organic-inorganic composite diaphragm for lithium ion battery and product thereof |
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| CN103474610A (en) * | 2013-09-29 | 2013-12-25 | 天津工业大学 | Method for preparing composite lithium-ion battery separator through electrostatic spinning/electrostatic spraying |
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