CN113097644A - Preparation method of SOFs-P5G/PVDF lithium ion battery diaphragm - Google Patents
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Abstract
The invention discloses a preparation method of a SOFs-P5G/PVDF lithium ion battery diaphragm, which comprises the steps of synthesizing a supermolecule organic frame SOFs-P5G, then adding the supermolecule organic frame SOFs-P5G into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder to continue to ultrasonically disperse, then adding an acetic acid solution, heating to 60-70 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane; and (4) taking down the fiber membrane obtained in the step (S3), placing the fiber membrane in a dopamine solution, carrying out soaking modification at 45-50 ℃ for 4-6 h, taking out the fiber membrane, and drying to obtain the diaphragm.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of an SOFs-P5G/PVDF lithium ion battery diaphragm.
Background
The lithium ion battery has the characteristics of large energy density, long cycle life, wide working temperature range, rapid charge and discharge and the like, so that the lithium ion battery is widely applied to the fields of mobile phones, notebook computers, aerospace, electric automobiles and the like. In the construction of lithium ion batteries, the separator is one of the key internal layer components. The diaphragm is arranged between the positive electrode and the negative electrode and mainly plays a role in separating active materials of the positive electrode and the negative electrode and preventing the two electrodes from being short-circuited due to contact. Meanwhile, because the diaphragm is provided with a large number of tortuous micropores, necessary electrolyte can be kept during electrochemical reaction, and a channel for moving ions is formed. The diaphragm is an important component of the lithium ion battery, and has great influence on the capacity, the cycle stability, the safety and the like of the lithium ion battery. Security, etc. have a great impact. Currently commercially available separators are polyolefin separators including polypropylene (PP) separators, Polyethylene (PE) separators, and three-layer composite PP/PE/PP separators. Due to the existence of polyolefin macromolecular chains, PE and PP separators form a structure with high crystallinity and low surface energy, and can hardly be swelled by electrolyte, so that the affinity of the polyolefin battery separators to the electrolyte is not ideal.
Disclosure of Invention
The invention aims to provide a preparation method of a SOFs-P5G/PVDF lithium ion battery diaphragm, which comprises the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalamide derivative into an acetonitrile solvent, reacting for 45-50 h at 80-85 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing a sample, loading the sample on a column, and eluting to obtain a yellow solid product.
2) Adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, performing magnetic stirring reflux for 16-20 h at 95-100 ℃, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing for 3-5 times by using acetonitrile, washing for 3-6 times by using ethanol, and drying to obtain a yellow-green powder product.
3) Synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 55-70 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 0.5-1 h, and drying to obtain the supermolecule organic framework SOFS-P5G.
S2: and (4) adding the supermolecule organic framework SOFS-P5G obtained in the step (S1) into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 60-70 ℃, stirring and dissolving, then transferring to a high-pressure injection pump, and electrostatically spinning to obtain the fiber membrane.
S3: and (4) taking down the fiber membrane obtained in the step (S3), placing the fiber membrane in a dopamine solution, carrying out soaking modification at 45-50 ℃ for 4-6 h, taking out the fiber membrane, and drying to obtain the diaphragm.
Preferably, the mass-to-volume ratio of the acetonitrile to the brominated pillared [5] arene P5 to the naphthalimide derivative is (45-60) mL, (0.48-0.69) g, (0.36-0.48) g.
Preferably, the elution is carried out by adopting petroleum ether and ethyl acetate in a volume ratio of (10-15): (2-8).
Preferably, the mass-to-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is (100-150) mL, and the mass-to-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is (1.88-2.26) g, and the mass-to-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is (5..
Preferably, the mass-volume ratio of the supermolecule organic framework SOFS-P5G, the polyvinylidene fluoride, the acetic acid and the distilled water is (0.82-0.96) g, (5.4-9.6) g, (18-25) mL and (100-150) mL.
Preferably, the mass-to-volume ratio of the yellow solid product in the step 1) to the yellow-to-green powder product in the step 2) to cyclohexanol is (0.49-0.56) g, (0.54-0.67) g, (20-40) mL.
Preferably, the injection voltage of the electrostatic spinning is 19-22 kV, the injection rate is 4-4.6 mL/h, and the injection distance is 10-15 cm.
Preferably, the dopamine solution is prepared from polydopamine and deionized water with a mass-volume ratio of (4-8) g (15-28) mL.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, a supermolecule organic frame material SOFs-P5G is adopted as an additive to be compounded with polyvinylidene fluoride, then, electrostatic spinning is carried out to prepare the lithium ion battery diaphragm, and then dopamine is used to modify the fiber membrane, so that the obtained diaphragm material has good liquid absorption rate, wherein the supermolecule organic frame material SOFs-P5G effectively improves the liquid absorption effect of the modified diaphragm, and the supermolecule organic frame material mainly has high porosity, does not contain metal ions, has good compounding effect with the polyvinylidene fluoride, and further can improve the discharge capacity and the cycling stability of the battery.
Drawings
FIG. 1 is a voltage-capacity curve at different current densities for a separator prepared according to example 1 of the present invention;
FIG. 2 is a graph of the cycling performance of the separator prepared in example 1 of the present invention at a current density of 0.5C.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of an SOFs-P5G/PVDF lithium ion battery diaphragm specifically comprises the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalimide derivative into an acetonitrile solvent, reacting for 45h at 80 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing the sample and loading the column, and eluting by adopting petroleum ether and ethyl acetate in a volume ratio of 10:2 to obtain a yellow solid product, wherein the mass volume ratio of the acetonitrile to the brominated column [5] arene P5 to the naphthalimide derivative is 45mL:0.48g:0.36 g.
2) Adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, then carrying out magnetic stirring reflux for 16h at 95 ℃, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing for 3 times by using acetonitrile, then washing for 3 times by using ethanol, and drying to obtain a yellow-green powder product; wherein the mass-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is 100mL to 1.88g to 5.52 g.
3) Synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 55 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 0.5-1 h, and drying to obtain supermolecular organic framework SOFS-P5G; wherein the mass volume ratio of the yellow solid product in the step 1), the yellow-green powder product in the step 2) and cyclohexanol is 0.49g:0.54g:20 mL.
S2: adding the supermolecule organic framework SOFs-P5G obtained in the step S1 into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 60-70 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane; wherein the mass-volume ratio of the supermolecule organic framework SOFS-P5G to the polyvinylidene fluoride to the acetic acid to the distilled water is 0.82g to 5.4g to 18mL to 100 mL; the injection voltage of the electrospinning was 19kV, the injection rate was 4mL/h, and the injection distance was 10 cm.
S3: taking down the fiber membrane obtained in the step S3, placing the fiber membrane in a dopamine solution, soaking and modifying the fiber membrane at 45 ℃ for 4 hours, taking out the fiber membrane, and drying the fiber membrane to obtain the diaphragm; wherein the dopamine solution is polydopamine and deionized water with the mass volume ratio of 4g:15 mL.
Example 2
A preparation method of an SOFs-P5G/PVDF lithium ion battery diaphragm specifically comprises the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalimide derivative into an acetonitrile solvent, reacting for 50h at 85 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing the sample and loading the column, and eluting by adopting petroleum ether and ethyl acetate in a volume ratio of 15:8 to obtain a yellow solid product, wherein the mass volume ratio of the acetonitrile to the brominated column [5] arene P5 to the naphthalimide derivative is 60mL:0.69g:0.48 g.
2) Adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, then carrying out magnetic stirring reflux at 100 ℃ for 20h, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing 5 times by using acetonitrile, then washing 6 times by using ethanol, and drying to obtain a yellow-green powder product; wherein the mass-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is 150mL to 2.26g to 8.86 g.
3) Synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 70 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 1h, and drying to obtain supermolecular organic frameworks (SOFs-P5G); wherein the mass volume ratio of the yellow solid product in the step 1), the yellow-green powder product in the step 2) and cyclohexanol is 0.56g:0.67g:40 mL.
S2: adding the supermolecule organic framework SOFs-P5G obtained in the step S1 into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 60-70 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane; wherein the mass-volume ratio of the supermolecule organic framework SOFS-P5G to the polyvinylidene fluoride to the acetic acid to the distilled water is 0.96g to 9.6g to 25mL to 150 mL; the injection voltage for electrospinning was 22kV, the injection rate was 4.6mL/h, and the injection distance was 15 cm.
S3: taking down the fiber membrane obtained in the step S3, placing the fiber membrane in a dopamine solution, soaking and modifying the fiber membrane at 50 ℃ for 6 hours, taking out the fiber membrane, and drying the fiber membrane to obtain the diaphragm; wherein the dopamine solution is polydopamine and deionized water with the mass volume ratio of 8g to 28 mL.
Example 3
A preparation method of an SOFs-P5G/PVDF lithium ion battery diaphragm specifically comprises the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalimide derivative into an acetonitrile solvent, reacting for 48h at 82 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing the sample and loading the column, and eluting by adopting petroleum ether and ethyl acetate in a volume ratio of 12:4 to obtain a yellow solid product, wherein the mass volume ratio of the acetonitrile to the brominated column [5] arene P5 to the naphthalimide derivative is 50mL:0.55g:0.41 g.
2) Adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, performing magnetic stirring reflux at 96 ℃ for 18h, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing 4 times by using acetonitrile, washing 4 times by using ethanol, and drying to obtain a yellow-green powder product; wherein the mass-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is 120mL to 1.95g to 6.66 g.
3) Synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 60 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 0.8h, and drying to obtain supermolecular organic framework SOFS-P5G; wherein the mass volume ratio of the yellow solid product in the step 1), the yellow-green powder product in the step 2) and cyclohexanol is 0.52g:0.59g:30 mL.
S2: adding the supermolecule organic framework SOFs-P5G obtained in the step S1 into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 65 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane; wherein the mass-volume ratio of the supermolecule organic framework SOFS-P5G to the polyvinylidene fluoride to the acetic acid to the distilled water is 0.88g to 7.3g to 20mL to 120 mL; the injection voltage of the electrospinning was 20kV, the injection rate was 4.2mL/h, and the injection distance was 12 cm.
S3: taking down the fiber membrane obtained in the step S3, placing the fiber membrane in a dopamine solution, carrying out soaking modification at 48 ℃ for 5h, taking out the fiber membrane, and drying to obtain the diaphragm; wherein the dopamine solution is polydopamine and deionized water with the mass volume ratio of 6g to 20 mL.
Example 4
A preparation method of an SOFs-P5G/PVDF lithium ion battery diaphragm specifically comprises the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalimide derivative into an acetonitrile solvent, reacting for 48h at 84 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing the sample and loading the column, and eluting by adopting petroleum ether and ethyl acetate in a volume ratio of 14:6 to obtain a yellow solid product, wherein the mass volume ratio of the acetonitrile to the brominated column [5] arene P5 to the naphthalimide derivative is 55mL:0.65g:0.47 g.
2) Adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, then carrying out magnetic stirring reflux for 19h at 100 ℃, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing 5 times by using acetonitrile, then washing 5 times by using ethanol, and drying to obtain a yellow-green powder product; wherein the mass-volume ratio of the acetonitrile to the 1, 10-dibromodecane to the 4, 4-bipyridine is 140mL to 2.22g to 8.83 g.
3) Synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 65 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 0.9h, and drying to obtain supermolecular organic framework SOFS-P5G; wherein the mass volume ratio of the yellow solid product in the step 1), the yellow-green powder product in the step 2) and cyclohexanol is 0.55g:0.65g:35 mL.
S2: adding the supermolecule organic framework SOFs-P5G obtained in the step S1 into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 68 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane; wherein the mass-volume ratio of the supermolecule organic framework SOFS-P5G to the polyvinylidene fluoride to the acetic acid to the distilled water is 0.95g to 9.2g to 24mL to 140 mL; the injection voltage for electrospinning was 21kV, the injection rate was 4.5mL/h, and the injection distance was 14 cm.
S3: taking down the fiber membrane obtained in the step S3, placing the fiber membrane in a dopamine solution, carrying out soaking modification at 48 ℃ for 5h, taking out the fiber membrane, and drying to obtain the diaphragm; wherein the dopamine solution is polydopamine and deionized water with the mass volume ratio of 6g:26 mL.
Examples of the experiments
Performance test-mechanical properties were tested using a tensile tester, stretching at a strain rate of 1 mm/min; the imbibition rate test was performed by placing a diaphragm in the electrolyte (1M LiPF)6Dissolving in EC/DMC/EMC 1:1:1), weighing the diaphragm mass before and after absorption saturation, and calculating the liquid absorption rate by using the following formula:
wherein EU is the liquid absorption rate, W0And W is the weight of the separator before and after soaking in the electrolyte;
the separators prepared in examples 1 to 4 were assembled into batteries, wherein the positive electrode material of the lithium battery was NCM811, the negative electrode material was graphite, and the assembled batteries were subjected to voltage-capacity test, cycle performance test and charge transfer resistance test at different rates, and the results are shown in table 1 or fig. 1,
the test results are shown in table 1,
table 1. test results:
as can be seen from table 1, the battery separators prepared in examples 1 to 4 of the present invention all had a mechanical strength of 43MPa or more, a liquid absorption rate of 298.9 wt.% or more, and a charge transfer resistance of 15.4 Ω or less, indicating that the battery separators of the present invention have good mechanical strength and excellent liquid absorption rate; and after the test of the cycle performance for 100 circles, the discharge capacity and the coulombic efficiency are still good.
Claims (8)
1. A preparation method of a SOFs-P5G/PVDF lithium ion battery diaphragm is characterized by comprising the following steps:
s1: preparation of SOFs-P5G: 1) synthesizing a main body: adding brominated column [5] arene P5 and a naphthalamide derivative into an acetonitrile solvent, reacting for 45-50 h at 80-85 ℃, then cooling to room temperature, performing rotary evaporation to remove the solvent, mixing a sample, loading the sample on a column, and eluting to obtain a yellow solid product;
2) adding 1, 10-dibromosunflower alkane and 4, 4-bipyridine into an acetonitrile solvent, performing magnetic stirring reflux for 16-20 h at 95-100 ℃, cooling to room temperature, filtering by using a Buchner funnel to obtain filter residue, washing 3-5 times by using acetonitrile, washing 3-6 times by using ethanol, and drying to obtain a yellow-green powder product;
3) synthesis of supramolecular organic frameworks (SOFS-P5G): adding the yellow solid product in the step 1) and the yellow green powder product in the step 2) into cyclohexanol, heating to 55-70 ℃, stirring for dissolving, cooling to room temperature, standing, stirring for 0.5-1 h, and drying to obtain supermolecule organic framework SOFS-P5G;
s2: adding the supermolecule organic framework SOFs-P5G obtained in the step S1 into distilled water, ultrasonically stirring and dispersing, then adding polyvinylidene fluoride powder, continuously ultrasonically dispersing, then adding an acetic acid solution, heating to 60-70 ℃, stirring and dissolving, then moving to a high-pressure injection pump, and carrying out electrostatic spinning to obtain a fiber membrane;
s3: and (4) taking down the fiber membrane obtained in the step (S3), placing the fiber membrane in a dopamine solution, carrying out soaking modification at 45-50 ℃ for 4-6 h, taking out the fiber membrane, and drying to obtain the diaphragm.
2. The preparation method of the SOFs-P5G/PVDF lithium ion battery separator according to claim 1, wherein the mass-to-volume ratio of the acetonitrile, the brominated column [5] arene P5 and the naphthalamide derivative is (45-60) mL (0.48-0.69) g (0.36-0.48) g.
3. The preparation method of the SOFs-P5G/PVDF lithium ion battery separator as claimed in claim 1, wherein the elution is performed by using petroleum ether and ethyl acetate in a volume ratio of (10-15) to (2-8).
4. The preparation method of the SOFs-P5G/PVDF lithium ion battery diaphragm according to claim 1, wherein the mass-to-volume ratio of the acetonitrile, the 1, 10-dibromodecane and the 4, 4-bipyridine is (100-150) mL, (1.88-2.26) g, (5.52-8.86) g.
5. The preparation method of the SOFs-P5G/PVDF lithium ion battery diaphragm according to claim 1, wherein the mass-to-volume ratio of the supermolecular organic framework SOFs-P5G, the polyvinylidene fluoride, the acetic acid and the distilled water is (0.82-0.96) g, (5.4-9.6) g, (18-25) mL (100-150) mL.
6. The preparation method of the SOFs-P5G/PVDF lithium ion battery separator according to claim 1, wherein the injection voltage of the electrostatic spinning is 19-22 kV, the injection rate is 4-4.6 mL/h, and the injection distance is 10-15 cm.
7. The preparation method of the SOFs-P5G/PVDF lithium ion battery diaphragm according to claim 1, wherein the dopamine solution is prepared from polydopamine and deionized water in a mass-volume ratio of (4-8) g (15-28) mL.
8. The preparation method of the SOFs-P5G/PVDF lithium ion battery separator membrane as claimed in claim 1, wherein the mass-to-volume ratio of the yellow solid product in the step 1), the yellow-to-green powder product in the step 2) and cyclohexanol is (0.49-0.56) g, (0.54-0.67) g, (20-40) mL.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115312975A (en) * | 2022-07-25 | 2022-11-08 | 陈雄 | Lithium ion battery diaphragm and preparation method thereof |
| CN115312975B (en) * | 2022-07-25 | 2024-01-12 | 上海比杰科技有限公司 | Lithium ion battery diaphragm and preparation method thereof |
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