CN106367895A - Composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane - Google Patents
Composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane Download PDFInfo
- Publication number
- CN106367895A CN106367895A CN201610978791.4A CN201610978791A CN106367895A CN 106367895 A CN106367895 A CN 106367895A CN 201610978791 A CN201610978791 A CN 201610978791A CN 106367895 A CN106367895 A CN 106367895A
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- CN
- China
- Prior art keywords
- polyurethane
- electrostatic spinning
- diaphragm material
- parts
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- 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
- D04H1/40—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
- D04H1/42—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 characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- 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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane. The composite electrostatic spinning fiber diaphragm material is prepared from, by weight parts, 80-83 parts of polyvinylidene difluoride, 20-22 parts of polymethyl methacrylate, an appropriate amount of DMF, 2-3 parts of nano boehmite, 0.8-1 part of silane coupling agent KH550, an appropriate amount of deionized water, 2-3 parts of graphite oxide, 2-3 parts of nano zirconia, 3-4 parts of polyethylene glycol, 0.8-1 part of polyvinylpyrrolidone and 2-3 parts of polyurethane. Nano zirconia, graphite oxide and polyurethane and the like are compounded and added into spinning solution, a fiber membrane is obtained through electrostatic spinning, the composite electrostatic spinning fiber diaphragm material has good breaking strength and electrochemical stability, and the hydrophilicity and permeability of the fiber membrane are greatly improved. The fiber membrane can serve as a capacitor diaphragm material, is safe and hydrophilic, has wettability, is high in liquid absorption rate, can meet the high-performance capacitor requirements, and is good in stability.
Description
Technical field
The present invention relates to supercapacitor technologies field, more particularly, to a kind of doped zirconia compounds the compound quiet of polyurethane
Electrospinning fibre diaphragm material.
Background technology
Ultracapacitor is a kind of accumulator of the great market competitiveness, because it can realize quick charge, high current
Electric discharge, and there are the charge lifetimes of more than 100,000 times, need to occupy critical role in the application of high-multiplying power discharge in short-term at some.
The requirement to electrical source of power of hybrid vehicle and electric automobile also result in that in worldwide, this is new to ultracapacitor
The extensive attention of type energy storage device.In the composition of ultracapacitor, electrode, the electrolyte and diaphragm paper property to ultracapacitor
Conclusive impact can be played.The electrode of ultracapacitor and electrolyte are the focuses studied at present, but people are for barrier film
Research and attention rate not high.
The diaphragm paper of ultracapacitor is located between two porous carbon electrodes, and complete wetting is in electrolyte together with electrode
In, play the effect of isolation during repeated charge, stop electronics conduction, prevent between the two poles of the earth, contacting the inside caused short
Road.This requires that diaphragm material is the insulator of electronics, has good isolation performance, and its hole should be less than electricity as far as possible
The minimum grain size of pole surfactant.The necessary aperture of the preferable diaphragm paper of isolation performance is little, so can make the circulation of electrolyte
Property decline, battery charging and discharging hydraulic performance decline；And electrolyte is impregnated with that rate is higher, ion passes through the good diaphragm material of property, and often hole is relatively
More greatly, easily cause and between the two poles of the earth, contact the internal short-circuit causing.The maximum advantage of ultracapacitor is charge/discharge rates
Hurry up, can with high power discharge, therefore, diaphragm material will thinner towards thickness, porosity is higher, aperture is less and is more evenly distributed
Contour performance trend development.
The non-woven fabrics of electrostatic spinning preparation have the advantages that three-dimensional micropore structure, specific surface area be big, porosity is high, in lithium electricity
There is preferable application prospect in pond barrier film field." method of electrostatic spinning preparation pan/pvdf-hfp diaphragm of supercapacitor and its power
Learn performance evaluation " in a literary composition by electrostatic spinning technique preparation pan/pvdf-hfp composite nano-fiber membrane, to pan/
Pvdf-hfp/pan three-decker composite membrane carries out hot-pressing processing, although the diaphragm material obtaining than product film performance
Improve, but yet suffer from low intensity, short life, the shortcoming yielding poorly, need further electrostatic spinning diaphragm material to be carried out
Modification, to improve heat stability, the mechanical property of barrier film.
Content of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of doped zirconia to compound answering of polyurethane
Close electrostatic spinning fiber diaphragm material.
The present invention is achieved by the following technical solutions:
The Combined Electrostatic that a kind of doped zirconia compounds polyurethane spins fibre diaphragm material, is prepared by the raw materials in:
Kynoar 80-83, polymethyl methacrylate 20-22, appropriate dmf, nm boehmite 2-3, silane coupler
Kh5500.8-1, appropriate deionized water, graphite oxide 2-3, nano zircite 2-3, Polyethylene Glycol 3-4, Polyvinylpyrrolidone
0.8-1, polyurethane 2-3.
The Combined Electrostatic that a kind of described doped zirconia compounds polyurethane spins fibre diaphragm material, by following concrete grammar system
Standby form:
(1) after nm boehmite being completely dried inside vacuum drying oven be dissolved in the silane coupled of 4-5 times amount deionized water
Agent kh550 mixes, and after ultrasonic disperse 30-40 minute, terminates anti-after being heated to 140-150 DEG C of backflow 90-120 minute while stirring
Should, centrifugation standing, solid deionized water is cleaned 2-3 time, is then put in vacuum drying oven solid with 60-70 DEG C of temperature
It is dried 12 hours, obtain the boehmite of modification；
(2) graphite oxide is washed with deionized clean post-drying, is subsequently adding in the deionized water of 5-6 times amount, continue to add
Enter nano zircite, suspension is formed with 300-400 rev/min of speed stirring, adds the poly- second being dissolved in 2-3 times amount deionized water
Alkene pyrrolidone, is spray-dried after continuing ultrasonic 60 minutes, obtains modified filler；
(3) at normal temperatures by Kynoar, polymethyl methacrylate, polyurethane mixing, add the dmf of total amount 8-9 times amount,
Add step (1), the product that obtains of step (2) and its surplus to stir under 400-500 rev/min of speed to after be completely dissolved
Remaining composition, continues ultrasonic disperse 40-50 minute after stirring 120-150 minute, obtains spinning liquid；
(4) spinning liquid is carried out electrostatic spinning, control and push away liquid speed degree 0.002mm/s, receiving range 18cm, the condition of voltage 22kv
Lower electrostatic spinning 2 hours, after the completion of spinning, after the fiber membrane collected is dried 12 hours in 60-70 DEG C of vacuum drying oven
Take out, push down in vacuum drying oven hot pressing 90-120 minute at 120 DEG C with clean glass is smooth, take out after natural cooling
Obtain final product.
The invention has the advantage that the present invention is by carrying out to boehmite being added to Kynoar, poly- first after surface modification
Base acrylic acid methyl ester. compounds in spinning liquid, obtains composite fibre diaphragm material by electrostatic spinning technique, intensity after hot-pressing processing
Strengthened, be there is good pick up simultaneously；Cooperation boehmite interpolation, due to boehmite particles surface polar group with
Polymer polarity Interaction of substituents, on the one hand can improve the heat stability of barrier film, mechanical strength, pore-size stability,
On the other hand the compatibility to electrolyte for the barrier film can be improved；In addition boehmite has excellent heat conductivility, can improve electricity
Container barrier film Heat Conduction Problems；The diaphragm material heat stability that the present invention makes is good, mechanical strength is improved, pick up high,
Electrochemical stability is good, have preferable high magnification capacity and good cyclic reversibility, is highly suitable for ultracapacitor
In.
The present invention is added to spinning by a series of PROCESS FOR TREATMENT by compounding to nano zircite, graphite oxide, polyurethane etc.
In silk stock solution, fibrous membrane is obtained by electrostatic spinning, there is good fracture strength, electrochemical stability, and greatly change
It has been apt to hydrophilic and the permeability of fibrous membrane；Fibrous membrane of the present invention can serve as capacitor diaphragm material, safe, hydrophilic, profit
Moist good, pick up is high, disclosure satisfy that the demand of high performance capacitors, the ultracapacitor stability made is good.
Specific embodiment
The Combined Electrostatic that a kind of doped zirconia compounds polyurethane spins fibre diaphragm material, by following weight portion (kilogram)
Raw material is made: Kynoar 80, polymethyl methacrylate 20, appropriate dmf, nm boehmite 2, silane coupler
Kh5500.8, appropriate deionized water, graphite oxide 2, nano zircite 2, Polyethylene Glycol 3, Polyvinylpyrrolidone 0.8, poly- ammonia
Ester 2.
The Combined Electrostatic that a kind of described doped zirconia compounds polyurethane spins fibre diaphragm material, by following concrete grammar system
Standby form:
(1) with the silane coupler being dissolved in 4 times amount deionized waters after nm boehmite being completely dried inside vacuum drying oven
Kh550 mixes, and ultrasonic disperse, after 30 minutes, terminates reaction after being heated to 140 DEG C of backflows while stirring 90 minutes, is centrifuged standing,
Solid deionized water is cleaned 2 times, then puts into solid in vacuum drying oven and is dried 12 hours with 60 DEG C of temperature, is changed
The boehmite of property；
(2) graphite oxide is washed with deionized clean post-drying, is subsequently adding in the deionized water of 5 times amount, continuously adds
Nano zircite, forms suspension with 300 revs/min of speed stirring, adds the polyvinylpyrrolidine being dissolved in 2 times amount deionized waters
Ketone, is spray-dried after continuing ultrasonic 60 minutes, obtains modified filler；
(3) at normal temperatures by Kynoar, polymethyl methacrylate, polyurethane mixing, add the dmf of total amount 8 times amount, with
Stir under 400 revs/min of speed to after be completely dissolved and add step (1), the product that obtains of step (2) and remaining residue to become
Point, after continuing to stir 120 minutes, ultrasonic disperse 40 minutes, obtains spinning liquid；
(4) spinning liquid is carried out electrostatic spinning, control and push away liquid speed degree 0.002mm/s, receiving range 18cm, the condition of voltage 22kv
Lower electrostatic spinning 2 hours, after the completion of spinning, takes after the fiber membrane of collection is dried 12 hours in 60 DEG C of vacuum drying ovens
Go out, push down in vacuum drying oven hot pressing 90 minutes at 120 DEG C with clean glass is smooth, take out after natural cooling and obtain final product.
By testing to the present embodiment diaphragm material, porosity is 64.5%, and pick up is 595%, percentage elongation
75.45%, at 110 DEG C, percent thermal shrinkage is less than 1%, and at 150 DEG C, percent thermal shrinkage is less than 1%.
Claims (2)
1. a kind of doped zirconia compounds the Combined Electrostatic of polyurethane and spins fibre diaphragm material it is characterised in that by following weight
The raw material of part is made: Kynoar 80-83, polymethyl methacrylate 20-22, appropriate dmf, nm boehmite 2-3, silane
Coupling agent kh5500.8-1, appropriate deionized water, graphite oxide 2-3, nano zircite 2-3, Polyethylene Glycol 3-4, polyethylene pyrrole
Pyrrolidone 0.8-1, polyurethane 2-3.
2. a kind of doped zirconia according to claims 1 compounds the Combined Electrostatic spinning fibre diaphragm material of polyurethane, its
It is characterised by, be prepared from by following concrete grammar:
(1) after nm boehmite being completely dried inside vacuum drying oven be dissolved in the silane coupled of 4-5 times amount deionized water
Agent kh550 mixes, and after ultrasonic disperse 30-40 minute, terminates anti-after being heated to 140-150 DEG C of backflow 90-120 minute while stirring
Should, centrifugation standing, solid deionized water is cleaned 2-3 time, is then put in vacuum drying oven solid with 60-70 DEG C of temperature
It is dried 12 hours, obtain the boehmite of modification；
(2) graphite oxide is washed with deionized clean post-drying, is subsequently adding in the deionized water of 5-6 times amount, continue to add
Enter nano zircite, suspension is formed with 300-400 rev/min of speed stirring, adds the poly- second being dissolved in 2-3 times amount deionized water
Alkene pyrrolidone, is spray-dried after continuing ultrasonic 60 minutes, obtains modified filler；
(3) at normal temperatures by Kynoar, polymethyl methacrylate, polyurethane mixing, add the dmf of total amount 8-9 times amount,
Add step (1), the product that obtains of step (2) and its surplus to stir under 400-500 rev/min of speed to after be completely dissolved
Remaining composition, continues ultrasonic disperse 40-50 minute after stirring 120-150 minute, obtains spinning liquid；
(4) spinning liquid is carried out electrostatic spinning, control and push away liquid speed degree 0.002mm/s, receiving range 18cm, the condition of voltage 22kv
Lower electrostatic spinning 2 hours, after the completion of spinning, after the fiber membrane collected is dried 12 hours in 60-70 DEG C of vacuum drying oven
Take out, push down in vacuum drying oven hot pressing 90-120 minute at 120 DEG C with clean glass is smooth, take out after natural cooling
Obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610978791.4A CN106367895A (en) | 2016-11-08 | 2016-11-08 | Composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610978791.4A CN106367895A (en) | 2016-11-08 | 2016-11-08 | Composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane |
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|---|---|
| CN106367895A true CN106367895A (en) | 2017-02-01 |
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| CN201610978791.4A Pending CN106367895A (en) | 2016-11-08 | 2016-11-08 | Composite electrostatic spinning fiber diaphragm material with doped zirconia and compounded polyurethane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114197116A (en) * | 2021-11-09 | 2022-03-18 | 宁德卓高新材料科技有限公司 | Electrostatic spinning film, manufacturing method thereof, battery with electrostatic spinning film and object with electrostatic spinning film |
| CN114497721A (en) * | 2022-01-07 | 2022-05-13 | 哈尔滨工业大学 | Composite electrolyte film, preparation method thereof and application thereof in solid-state lithium battery |
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| CN104289042A (en) * | 2014-09-05 | 2015-01-21 | 东华大学 | Electrospinning nano-fiber electret filtering material and its preparation method |
| CN105428572A (en) * | 2015-11-27 | 2016-03-23 | 厦门大学 | Preparation method of electrospun composite membrane for lithium ion battery |
| CN105542625A (en) * | 2016-03-11 | 2016-05-04 | 吴伦 | Polymer fire retardant coating for steel plate and preparation method of coating |
| CN105778156A (en) * | 2016-03-27 | 2016-07-20 | 华南理工大学 | Novel rubber compound stuffing preparing method based on mercapto-alkene chemical reaction |
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2016
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285424A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Three-dimensional fiber-based aerogel tissue engineering scaffold and preparation method thereof |
| CN104124418A (en) * | 2014-07-25 | 2014-10-29 | 佛山市盈博莱科技有限公司 | Lithium ion battery diaphragm and preparation method thereof |
| CN104289042A (en) * | 2014-09-05 | 2015-01-21 | 东华大学 | Electrospinning nano-fiber electret filtering material and its preparation method |
| CN105428572A (en) * | 2015-11-27 | 2016-03-23 | 厦门大学 | Preparation method of electrospun composite membrane for lithium ion battery |
| CN105542625A (en) * | 2016-03-11 | 2016-05-04 | 吴伦 | Polymer fire retardant coating for steel plate and preparation method of coating |
| CN105778156A (en) * | 2016-03-27 | 2016-07-20 | 华南理工大学 | Novel rubber compound stuffing preparing method based on mercapto-alkene chemical reaction |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114197116A (en) * | 2021-11-09 | 2022-03-18 | 宁德卓高新材料科技有限公司 | Electrostatic spinning film, manufacturing method thereof, battery with electrostatic spinning film and object with electrostatic spinning film |
| CN114497721A (en) * | 2022-01-07 | 2022-05-13 | 哈尔滨工业大学 | Composite electrolyte film, preparation method thereof and application thereof in solid-state lithium battery |
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Application publication date: 20170201 |