CN101069821A - Cross-linked modified PVOF-HFP superfine fiber film and preparing method - Google Patents
Cross-linked modified PVOF-HFP superfine fiber film and preparing method Download PDFInfo
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- CN101069821A CN101069821A CN 200710056880 CN200710056880A CN101069821A CN 101069821 A CN101069821 A CN 101069821A CN 200710056880 CN200710056880 CN 200710056880 CN 200710056880 A CN200710056880 A CN 200710056880A CN 101069821 A CN101069821 A CN 101069821A
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- superfine fibre
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- vinylidene fluoride
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Abstract
The present invention relates to a crosslinking modified PVDF-HFP superfine fibre membrane and its preparation method. The described crosslinking modified PVDF-HFP superfine fibre membrane is a superfine fibre membrane whose thickness is 10 micrometers-60 micrometers which is made up by using superfine fibres of PEGDMA whose mass content is 10-35% and PVDF-HFP whose mass content is 90-65% and whose diameter is 50nm-500nm. Its preparation method includes the following steps: in the DMF and acetone mixed solvent adding PVDF-HFP, PEGDMA and AIBN initiating agent to prepare electric spinning solution, utilizing said electric spinning solution to make electrostatic spinning so as to obtain the membrane formed from superfine fibre whose diameter is 50nm-500nm, then making the formed superfine fibre membrane undergo the processes of vacuum-drying, removing residual solvent and crosslinking reaction for 0.5-15h at 80-135deg.C so as to 8obtain the invented crosslinking modified PVDF-HFP superfine fibre membrane.
Description
Technical field
The present invention relates to a kind of crosslinking modified PVDF-HFP superfine fibre membrane and preparation method thereof, belong to vinylidene fluoride-hexafluoropropylene copolymer function filter membrane technology.
Background technology
Method by electrospinning can prepare the nano grade polymer superfine fibre film.Owing to have characteristics such as high porosity, aperture are little, electrospun fiber membrane has wide application prospect in fields such as biomedical, photoelectricity and Textile Engineerings.Yet, since electrospinning fibre typically have a diameter from the hundreds of nanometer, make that the mechanical property of electrospun fiber membrane is generally relatively poor, be difficult to make it the occasion that is applicable to that mechanical property requirements is higher.
By the way of chemical crosslinking, the mechanical property of electrospinning film is slightly improved.For example, with glyoxal cross-linking polyvinyl alcohol electrospun fiber membrane, not only making it water resistance has improved, and its hot strength also has increase slightly, but greatly reduce its elongation at break (Ding B, Kim HY, Lee SC, et al. " Preparation andcharacterization of a nanoscale poly (vinyl alcohol) fiber aggregate producedby an electrospinning method ", Journal of Polymer Science-Polymer Physics2002,40:1261-1268).Heating anneal is handled, be that another kind of post processing improves the method for its performance to electrospun fiber membrane, as L-polylactic acid electrospinning fibre film is continued heating 30min or 60min in 180 ℃ of baking ovens, can make its hot strength bring up to 4.14MPa and 4.19MPa respectively by 3.59MPa, elongation at break is brought up to 102.5% and 35.5% (You Y respectively by 12.8% simultaneously, Lee SW, Lee SJ, et al. " Thermal interfiber bonding ofelectrospun poly (L-lactic acid) nanofibers ", Materials Letters 2006,60:1331-1333).
(polyvinylidenefluoride-hexafluoropropylene PVDF-HFP) compares with Kynoar (PVDF) vinylidene fluoride-hexafluoropropylene copolymer, owing to introduced-CF on the main chain
3Side group makes it under the situation that does not influence the main chain flexibility, has increased the closelypacked resistance of strand, thereby reduces its crystallizing power effectively, more helps the infiltration of electrolyte and the migration of ion, is more suitable for being used among the lithium ion battery than homopolymers PVDF.The glass transition temperature of PVDF-HFP is about-40 ℃, and this makes the PVDF-HFP superfine fibre film after the electrospinning compare with the electrospinning pvdf membrane, and feel is clamminess, and is not easy to and receives metal aluminum foil peel off.
Summary of the invention
The objective of the invention is to provide a kind of crosslinking modified PVDF-HFP superfine fibre membrane and preparation method thereof, described crosslinking modified PVDF-HFP superfine fibre membrane has the good mechanical performance, uses extensively, and its preparation method process is simple.
For achieving the above object, the present invention is realized by following technical proposals: a kind of crosslinking modified PVDF-HFP superfine fibre membrane, it is characterized in that, this crosslinking modified PVDF-HFP superfine fibre membrane is that 10～35% polyethylene glycol dimethacrylate (PEGDMA) and mass content are that the diameter of 90～65% vinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP) is that the thickness that the superfine fibre of 50nm～500nm forms is the superfine fibre film of 10 μ m～60 μ m with mass content.
The preparation method of above-mentioned crosslinking modified PVDF-HFP superfine fibre membrane, it is characterized in that comprising following process: at N, dinethylformamide (DMF) is (9～6) with acetone by volume: in the mixed solvent of (1～4), the mass ratio of pressing vinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP) and polyethylene glycol dimethacrylate (PEGDMA) is (6.5～9.0): (3.5～1.0), at first be that 480,000 vinylidene fluoride-hexafluoropropylene copolymer adds in the mixed solvent with relative molecular mass, under 40～55 ℃, be that 100～200rpm stirs to clarify solution with rotating speed, to add relative molecular mass be 330～875 polyethylene glycol dimethacrylate and add 0～2% azodiisobutyronitrile (AIBN) initator by the polyethylene glycol dimethacrylate quality to settled solution then, continues to stir to make the electrospinning solution that concentration is 0.10～0.26g/mL.This electrospinning solution is injected in the syringe in the electrostatic spinning apparatus, with receiving range 10cm～25cm, operating voltage 5kV～30kV, to spin by diameter be the film that the superfine fibre of 50nm～500nm forms to static under flow 0.1mL/h～0.5mL/h condition, afterwards, this superfine fibre film is placed vacuum drying oven, is the down dry 12～24h of 200Pa in 25～38 ℃ with vacuum, remove residual solvent in the superfine fibre film, again superfine fibre film is put into the electric heating blast dry oven in 80～135 ℃ of generation cross-linking reaction 0.5～15h, made crosslinking modified PVDF-HFP superfine fibre membrane.
The invention has the advantages that: this preparation method's process is simple and convenient, prepared crosslinking modified PVDF-HFP superfine fibre membrane, have high specific area and porosity, as the lithium ion battery separator material, good with the electrolyte wellability, the pick up height, bonding firmly with both positive and negative polarity, and good mechanical performance.Also can be used as polymer dielectric film, filter membrane.
The specific embodiment
Embodiment 1
With the 1.6g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 6mL DMF and 4mL acetone, under 45 ℃ be that 100rpm stirs 2h and makes it to dissolve fully and obtain settled solution with the rotating speed, add the 0.36mL relative molecular mass then and be 330 PEGDMA, continue to stir 1.5h.Under receiving range 15cm, operating voltage 15kV, flow 0.47mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.The PVDF-HFP/PEGDMA superfine fibre film is placed vacuum drying oven, is dry 24h under the 200Pa in 25 ℃ with vacuum.Treat in the superfine fibre film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 125 ℃ of heating, takes out behind the reaction 2h, promptly obtains the crosslinking modified PVDF-HFP superfine fibre membrane by PEGDMA.
Embodiment 2
With the 2.0g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 7mLDMF and 3mL acetone, under 50 ℃ be that 120rpm stirs 1.8h and makes it to dissolve fully and obtain settled solution with the rotating speed, add the 0.50mL relative molecular mass then and be 550 PEGDMA, continue to stir 1.3h.Under receiving range 20cm, operating voltage 18kV, flow 0.2mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.PVDF-HFP/PEGDMA electrospun fibers film is placed vacuum drying oven, is dry 20h under the 200Pa in 28 ℃ with vacuum.Treat in the film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 135 ℃ of heating, takes out behind the reaction 0.5h, promptly obtains the crosslinking modified PVDF-HFP superfine fibre membrane by PEGDMA.
Embodiment 3
With the 1.2g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 8mLDMF and 2mL acetone.Under 50 ℃ be that 150rpm stirs 1.5h and makes it to dissolve fully and obtain settled solution, add the 0.25mL relative molecular mass then and be 875 PEGDMA and the AIBN of 5.5mg, continue to stir 1.2h with the rotating speed.Under receiving range 12cm, operating voltage 12kV, flow 0.4mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.PVDF-HFP/PEGDMA electrospun fibers film is placed vacuum drying oven, is dry 24h under the 200Pa in 25 ℃ with vacuum.Treat in the film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 80 ℃ of heating, takes out behind the reaction 15h, promptly obtains the crosslinking modified PVDF-HFP superfine fibre membrane by PEGDMA.
Embodiment 4
With the 1.6g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 9mLDMF and 1mL acetone.Under 45 ℃ be that 180rpm stirs 1.3h and makes it to dissolve fully and obtain settled solution, add the 0.58mL relative molecular mass then and be 330 PEGDMA and the AIBN of 7.2mg, continue to stir 1.1h with the rotating speed.Under receiving range 15cm, operating voltage 15kV, flow 0.2mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.PVDF-HFP/PEGDMA electrospun fibers film is placed vacuum drying oven, is dry 12h under the 200Pa in 38 ℃ with vacuum.Treat in the film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 90 ℃ of heating, takes out behind the reaction 5h, promptly obtains the cross-linking modified PYDF-HFP superfine fibre film by PEGDMA.
Embodiment 5
With the 1.6g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 6mLDMF and 4mL acetone.Under 45 ℃ be that 200rpm stirs 1.0h and makes it to dissolve fully and obtain settled solution, add the 0.77mL relative molecular mass then and be 330 PEGDMA, continue to stir 1h with the rotating speed.Under receiving range 15cm, operating voltage 15kV, flow 0.2mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.PVDF-HFP/PEGDMA electrospun fibers film is placed vacuum drying oven, is dry 12h under the 200Pa in 38 ℃ with vacuum.Treat in the film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 135 ℃ of heating, takes out behind the reaction 0.5h, promptly obtains the crosslinking modified PVDF-HFP superfine fibre membrane by PEGDMA.
Embodiment 6
With the 1.6g relative molecular mass is that 480,000 PVDF-HFP is dissolved in the mixed solvent of 6mLDMF and 4mL acetone.Under 55 ℃ be that 170rpm stirs 1.35h and makes it to dissolve fully and obtain settled solution, add the 0.16mL relative molecular mass then and be 330 PEGDMA and the AIBN of 3.0mg, continue to stir 1.2h with the rotating speed.Under receiving range 15cm, operating voltage 15kV, flow 0.2mL/h condition, it is carried out electrostatic spinning.Just can obtain to contain the PVDF-HFP electrospun fibers film of PEGDMA behind the 3h.PVDF-HFP/PEGDMA electrospun fibers film is placed vacuum drying oven, is dry 12h under the 200Pa in 38 ℃ with vacuum.Treat in the film behind the noresidue solvent that it is crosslinked to put it in the electric heating blast dry oven 90 ℃ of heating, takes out behind the reaction 5h, promptly obtains the crosslinking modified PVDF-HFP superfine fibre membrane by PEGDMA.
Claims (2)
1. cross-linking modified vinylidene fluoride-hexafluoropropylene copolymer superfine fibre film, it is characterized in that, the vinylidene fluoride-hexafluoropropylene copolymer superfine fibre film that this is cross-linking modified is that 10～35% polyethylene glycol dimethacrylate and mass content are that the diameter of 90～65% vinylidene fluoride-hexafluoropropylene copolymer is that the thickness that the superfine fibre of 50nm～500nm constitutes is the superfine fibre film of 10 μ m～60 μ m with mass content.
2. method for preparing the described cross-linking modified vinylidene fluoride-hexafluoropropylene copolymer superfine fibre film of claim 1, it is characterized in that comprising following process: it is characterized in that comprising following process: at N, dinethylformamide and acetone are (9～6) by volume: in the mixed solvent of (1～4), the mass ratio of pressing vinylidene fluoride-hexafluoropropylene copolymer and polyethylene glycol dimethacrylate is (6.5～9.0): (3.5～1.0), at first be that 480,000 vinylidene fluoride-hexafluoropropylene copolymer adds in the mixed solvent with relative molecular mass, under 40～55 ℃, be that 100～200rpm stirs to clarify solution with rotating speed, to add relative molecular mass be 330～875 polyethylene glycol dimethacrylate and add 0～2% azodiisobutyronitrile initator by the polyethylene glycol dimethacrylate quality to settled solution then, continue to stir and make the electrospinning solution that concentration is 0.10～0.25g/mL, this electrospinning solution is injected in the syringe in the electrostatic spinning apparatus, with receiving range 10cm～25cm, operating voltage 5kV～30kV, to spin by diameter be the film that the superfine fibre of 50nm～500nm forms to static under flow 0.1mL/h～0.5mL/h condition, afterwards, this superfine fibre film is placed vacuum drying oven, is the down dry 12～24h of 200Pa in 25～38 ℃ with vacuum, remove residual solvent in the superfine fibre film, again superfine fibre film is put into the electric heating blast dry oven in 80～135 ℃ of generation cross-linking reaction 0.5～15h, made cross-linking modified vinylidene fluoride-hexafluoropropylene copolymer superfine fibre film.
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| WO2009127170A3 (en) * | 2008-04-15 | 2009-12-03 | Elmarco S.R.O. | Method for production of nanofibres from fluorinated copolymers and terpolymers through electrostatic spinning, nanofibres and fabrics |
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| CN101805454B (en) * | 2009-02-13 | 2011-12-28 | 中国科学院理化技术研究所 | Polyvinylidene fluoride and vinylidene fluoride-hexafluoropropylene copolymer blended nanofibre polymer electrolyte membrane and preparation method thereof |
| CN102587040A (en) * | 2012-02-17 | 2012-07-18 | 浙江大东南集团有限公司 | Preparation method of nanofiber membrane for lithium ion battery diaphragm |
| CN102629679A (en) * | 2012-04-28 | 2012-08-08 | 中国科学院理化技术研究所 | Nanometer fiber lithium ion battery diaphragm material with composite structure and preparation method of nanometer fiber lithium ion battery diaphragm material |
| CN103700797A (en) * | 2012-09-27 | 2014-04-02 | 比亚迪股份有限公司 | Polymer electrolyte, its preparation method and battery comprising the same |
| CN104707490A (en) * | 2015-02-09 | 2015-06-17 | 杭州费尔过滤技术有限公司 | Method for preparing superfine polyolefin degassing membrane |
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| WO2009127170A3 (en) * | 2008-04-15 | 2009-12-03 | Elmarco S.R.O. | Method for production of nanofibres from fluorinated copolymers and terpolymers through electrostatic spinning, nanofibres and fabrics |
| CN101805454B (en) * | 2009-02-13 | 2011-12-28 | 中国科学院理化技术研究所 | Polyvinylidene fluoride and vinylidene fluoride-hexafluoropropylene copolymer blended nanofibre polymer electrolyte membrane and preparation method thereof |
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| CN102218871B (en) * | 2011-04-14 | 2014-08-27 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| CN102587040A (en) * | 2012-02-17 | 2012-07-18 | 浙江大东南集团有限公司 | Preparation method of nanofiber membrane for lithium ion battery diaphragm |
| CN102629679A (en) * | 2012-04-28 | 2012-08-08 | 中国科学院理化技术研究所 | Nanometer fiber lithium ion battery diaphragm material with composite structure and preparation method of nanometer fiber lithium ion battery diaphragm material |
| CN102629679B (en) * | 2012-04-28 | 2018-04-20 | 中国科学院理化技术研究所 | Nanofiber lithium ion battery separator material with composite construction and preparation method thereof |
| CN103700797A (en) * | 2012-09-27 | 2014-04-02 | 比亚迪股份有限公司 | Polymer electrolyte, its preparation method and battery comprising the same |
| CN103700797B (en) * | 2012-09-27 | 2016-04-27 | 比亚迪股份有限公司 | Polymer dielectric and preparation method thereof and the battery comprising this polymer dielectric |
| CN104707490A (en) * | 2015-02-09 | 2015-06-17 | 杭州费尔过滤技术有限公司 | Method for preparing superfine polyolefin degassing membrane |
| CN107331824A (en) * | 2017-07-04 | 2017-11-07 | 哈尔滨理工大学 | It is crosslinked blending and modifying EVOH SO3The method of Li electrospinning films |
| CN107174986A (en) * | 2017-07-18 | 2017-09-19 | 中国科学院生态环境研究中心 | A kind of preparation method of electrostatic spinning hydrophobic membrane |
| CN110106572A (en) * | 2019-04-25 | 2019-08-09 | 吉林大学 | A kind of preparation method of periodicity luminescent composite |
| CN110106572B (en) * | 2019-04-25 | 2021-08-31 | 吉林大学 | Preparation method of periodic luminous composite material |
| CN110124540A (en) * | 2019-05-27 | 2019-08-16 | 济南大学 | A kind of preparation method of Superhydrophilic polyvinylidene fluoride film |
| CN111416087A (en) * | 2020-03-18 | 2020-07-14 | 江苏厚生新能源科技有限公司 | Preparation method of novel thermal radiation cross-linked semi-solid lithium battery diaphragm |
| CN114496589A (en) * | 2022-02-25 | 2022-05-13 | 西安交通大学 | Porous gel electrolyte and preparation method and application thereof |
| CN114496589B (en) * | 2022-02-25 | 2022-12-09 | 西安交通大学 | Porous gel electrolyte and preparation method and application thereof |
| CN115652475A (en) * | 2022-10-26 | 2023-01-31 | 大连理工大学 | Method for preparing proton exchange membrane by electrostatic spinning in-situ densification |
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