CN106544786A - A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium - Google Patents
A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium Download PDFInfo
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- CN106544786A CN106544786A CN201610978758.1A CN201610978758A CN106544786A CN 106544786 A CN106544786 A CN 106544786A CN 201610978758 A CN201610978758 A CN 201610978758A CN 106544786 A CN106544786 A CN 106544786A
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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
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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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/52—Separators
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/04—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons
- D10B2321/042—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons polymers of fluorinated hydrocarbons, e.g. polytetrafluoroethene [PTFE]
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/08—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated carboxylic acids or unsaturated organic esters, e.g. polyacrylic esters, polyvinyl acetate
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Cell Separators (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium, is prepared by the raw materials in：Kynoar 80 83, polymethyl methacrylate 20 22, appropriate DMF, nm boehmite 23, Silane coupling agent KH550 0.8 1, appropriate deionized water, lanthanum sesquioxide 1.5 2, lithium carbonate 1.5 2, titanium dioxide 23, polyimides 89, appropriate dehydrated alcohol.Lanthanum sesquioxide, lithium carbonate, titanium dioxide compounding are made the alloy with certain conductivity by certain chemical technology by the present invention, it is added in the preparation of diaphragm material, the mechanical performance of electrolyte is strengthened but also electrical conductivity can be made also significantly to improve；Diaphragm material made by the present invention has connective preferably threadiness pore passage structure, preferable electrolyte absorbent properties and preferable chemical property, and technique is easy to industrialized production, is adapted to ultracapacitor and uses.
Description
Technical field
The present invention relates to supercapacitor technologies field, more particularly to a kind of titanium doped modified Static Spinning super capacitor of lanthanum lithium
Device diaphragm material.
Background technology
Ultracapacitor is a kind of accumulator of the great market competitiveness, as it can realize quick charge, high current
Electric discharge, and with the charge lifetimes of more than 100,000 times, occupy critical role in some needs applications of high-multiplying power discharge in short-term.
The requirement of hybrid vehicle and electric automobile to electrical source of power also result in worldwide that this is new to ultracapacitor
The extensive attention of type energy storage device.In the composition of ultracapacitor, the property of electrode, electrolyte and diaphragm paper to ultracapacitor
Conclusive impact can be played.The electrode and electrolyte of ultracapacitor is the focus of research at present, but people are for barrier film
Research and attention rate it is 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 a part of isolation during repeated charge, prevent 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, and with good isolation performance, and its hole should as far as possible less than electricity
The minimum grain size of pole surfactant.The necessary aperture of the preferable diaphragm paper of isolation performance is little, can so make the circulation of electrolyte
Property decline, battery charging and discharging hydraulic performance decline；And electrolyte is impregnated with that rate is higher, ion by the good diaphragm material of property often hole compared with
It is big more, easily cause and between the two poles of the earth, contact the internal short-circuit for causing.The maximum advantage of ultracapacitor is charge/discharge rates
Hurry up, can with high power discharge, therefore, diaphragm material will be, porosity thinner towards thickness higher, aperture less and be more evenly distributed
Contour performance trend development.
Non-woven fabrics prepared by electrostatic spinning 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 prepares PAN/PVDF-HFP diaphragm of supercapacitor and its power
Learn performance evaluation》PAN/PVDF-HFP composite nano-fiber membranes are prepared by electrostatic spinning technique in one text, to PAN/
PVDF-HFP/PAN three-deckers composite membrane carries out hot-pressing processing, although the diaphragm material for obtaining than product film performance
Improve, but the shortcoming for yet suffering from low intensity, short life, yielding poorly, need further to carry out electrostatic spinning diaphragm material
It is modified, to improve heat stability, the mechanical property of barrier film.
The content of the invention
The object of the invention is exactly for the defect for making up prior art, there is provided a kind of titanium doped modified Static Spinning of lanthanum lithium is super
Capacitor diaphragm material.
The present invention is achieved by the following technical solutions：
A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium, is prepared by the raw materials in：Gather inclined fluorine
Ethylene 80-83, polymethyl methacrylate 20-22, appropriate DMF, nm boehmite 2-3, Silane coupling agent KH550 0.8-1, go
Ion appropriate amount of water, lanthanum sesquioxide 1.5-2, lithium carbonate 1.5-2, titanium dioxide 2-3, polyimides 8-9, appropriate dehydrated alcohol.
A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium, prepared by following concrete grammar and
Into：
（1）After nm boehmite is completely dried inside vacuum drying oven be dissolved in 4-5 times and measure the silane coupled of deionized water
Agent KH550 mixes, and after ultrasonic disperse 30-40 minutes, terminates anti-after being heated to 140-150 DEG C of backflow 90-120 minute while stirring
Should, centrifugation stands, and solid deionized water is cleaned 2-3 time, and solid is put in vacuum drying oven the temperature with 60-70 DEG C then
It is dried 12 hours, obtains modified boehmite；
（2）Lanthanum sesquioxide, lithium carbonate, titania powder respectively in Muffle furnace with 550-600 DEG C under the conditions of calcine 2-3 it is little
When to remove the impurity in raw material, then mix homogeneously is put into the dehydrated alcohol of total amount equivalent, ball milling 60-90 minutes, then at
5-6 hours are calcined at 900-950 DEG C, mixed powder is obtained；
（3）At normal temperatures by Kynoar, polymethyl methacrylate, polyimides mixing, add what total amount 8-9 times was measured
DMF, adds step to stir under 400-500 rev/min of speed to after being completely dissolved（1）, step（2）The product for obtaining, continues
Ultrasonic disperse 40-50 minutes after stirring 120-150 minutes, obtain spinning liquid；
（4）Spinning liquid is carried out into electrostatic spinning, control pushes away liquid speed degree 0.002mm/s, receives apart from 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, the hot pressing 90-120 minutes at 120 DEG C are pushed down in vacuum drying oven with clean glass is smooth, taken out after natural cooling
Obtain final product.
It is an advantage of the invention that：By carrying out to boehmite, surface is modified to be added to Kynoar, poly- first to the present invention
In base acrylic acid methyl ester. compounding spinning liquid, composite fibre diaphragm material is obtained by electrostatic spinning technique, intensity after hot-pressing processing
Strengthened, while with good pick up；Coordinate boehmite addition, 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 of the barrier film to electrolyte can be improved；In addition boehmite has excellent heat conductivility, can improve electricity
Container barrier film Heat Conduction Problems；Diaphragm material heat stability made by the present invention is good, mechanical strength is improved, pick up high,
Electrochemical stability is good, with preferable high magnification capacity and good cyclic reversibility, be highly suitable for ultracapacitor
In.
The present invention is made lanthanum sesquioxide, lithium carbonate, titanium dioxide compounding with certain by certain chemical technology
The alloy of conductivity, is added in the preparation of diaphragm material, and the mechanical performance of electrolyte can not only strengthened but also can be with
Electrical conductivity is made also significantly to improve；Diaphragm material made by the present invention has connective preferably threadiness pore passage structure, preferably
Electrolyte absorbent properties and preferable chemical property, technique is easy to industrialized production, is adapted to ultracapacitor and uses.
Specific embodiment
The titanium doped modified Static Spinning diaphragm of supercapacitor material of a kind of lanthanum lithium, by following weight portion（Kilogram）Raw material system
Into：Kynoar 80, polymethyl methacrylate 20, appropriate DMF, nm boehmite 2, Silane coupling agent KH550 0.8, go
Ion appropriate amount of water, lanthanum sesquioxide 1.5, lithium carbonate 1.5, titanium dioxide 2, polyimides 8, appropriate dehydrated alcohol.
The titanium doped modified Static Spinning diaphragm of supercapacitor material of a kind of lanthanum lithium according to claims 1, by following
Concrete grammar is prepared from：
（1）With the silane coupler for being dissolved in 4 times of amount deionized waters after nm boehmite is completely dried inside vacuum drying oven
KH550 mixes, and ultrasonic disperse terminated reaction after 30 minutes after being heated to 140 DEG C of backflows while stirring 90 minutes, centrifugation stands,
Solid deionized water is cleaned 2 times, then solid is put in vacuum drying oven and is dried 12 hours with 60 DEG C of temperature, changed
The boehmite of property；
（2）Lanthanum sesquioxide, lithium carbonate, titania powder are respectively in Muffle furnace calcining 2 hours removing under the conditions of 550 DEG C
The impurity gone in raw material, then mix homogeneously, is put into the dehydrated alcohol of total amount equivalent, and ball milling 60 minutes is calcined at 900 DEG C
5 hours, obtain mixed powder；
（3）At normal temperatures by Kynoar, polymethyl methacrylate, polyimides mixing, the DMF of 8 times of amounts of total amount is added,
Step is added to stir under 400 revs/min of speed to after being completely dissolved（1）, step（2）The product for obtaining, continues 120 points of stirring
After clock, ultrasonic disperse 40 minutes, obtain spinning liquid；
（4）Spinning liquid is carried out into electrostatic spinning, control pushes away liquid speed degree 0.002mm/s, receives apart from 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, hot pressing 90 minutes at 120 DEG C are pushed down in vacuum drying oven with clean glass is smooth, take out and obtain final product after natural cooling.
By testing to the present embodiment diaphragm material, porosity is 60.6%, and pick up is 604%, percentage elongation
74.7%, 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. the titanium doped modified Static Spinning diaphragm of supercapacitor material of a kind of lanthanum lithium, it is characterised in that by the original of following weight portion
Material is made：Kynoar 80-83, polymethyl methacrylate 20-22, appropriate DMF, nm boehmite 2-3, silane coupler
KH5500.8-1, appropriate deionized water, lanthanum sesquioxide 1.5-2, lithium carbonate 1.5-2, titanium dioxide 2-3, polyimides 8-9,
Appropriate dehydrated alcohol.
2. the titanium doped modified Static Spinning diaphragm of supercapacitor material of a kind of lanthanum lithium according to claims 1, its feature exist
In being prepared from by following concrete grammar：
（1）After nm boehmite is completely dried inside vacuum drying oven be dissolved in 4-5 times and measure the silane coupled of deionized water
Agent KH550 mixes, and after ultrasonic disperse 30-40 minutes, terminates anti-after being heated to 140-150 DEG C of backflow 90-120 minute while stirring
Should, centrifugation stands, and solid deionized water is cleaned 2-3 time, and solid is put in vacuum drying oven the temperature with 60-70 DEG C then
It is dried 12 hours, obtains modified boehmite；
（2）Lanthanum sesquioxide, lithium carbonate, titania powder respectively in Muffle furnace with 550-600 DEG C under the conditions of calcine 2-3 it is little
When to remove the impurity in raw material, then mix homogeneously is put into the dehydrated alcohol of total amount equivalent, ball milling 60-90 minutes, then at
5-6 hours are calcined at 900-950 DEG C, mixed powder is obtained；
（3）At normal temperatures by Kynoar, polymethyl methacrylate, polyimides mixing, add what total amount 8-9 times was measured
DMF, adds step to stir under 400-500 rev/min of speed to after being completely dissolved（1）, step（2）The product for obtaining, continues
Ultrasonic disperse 40-50 minutes after stirring 120-150 minutes, obtain spinning liquid；
（4）Spinning liquid is carried out into electrostatic spinning, control pushes away liquid speed degree 0.002mm/s, receives apart from 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, the hot pressing 90-120 minutes at 120 DEG C are pushed down in vacuum drying oven with clean glass is smooth, taken out after natural cooling
Obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610978758.1A CN106544786A (en) | 2016-11-08 | 2016-11-08 | A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium |
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| CN201610978758.1A CN106544786A (en) | 2016-11-08 | 2016-11-08 | A kind of titanium doped modified Static Spinning diaphragm of supercapacitor material of lanthanum lithium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984194A (en) * | 2017-04-25 | 2017-07-28 | 浙江大学 | A kind of modifying super hydrophobicity nano fibrous membrane and its preparation method and application |
| CN109056194A (en) * | 2018-07-12 | 2018-12-21 | 东华大学 | A kind of flexibility Li-La-Ti oxygen ceramic nanofibers membrane material and preparation method thereof |
| CN113493958A (en) * | 2020-04-05 | 2021-10-12 | 北京化工大学 | Polyimide nanofiber membrane coaxially coated with boehmite and preparation method thereof |
| CN117153576A (en) * | 2023-07-26 | 2023-12-01 | 哈尔滨理工大学 | A preparation method for solid-state lithium-ion capacitors based on double-doped activated carbon |
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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 |
| CN105990039A (en) * | 2016-01-27 | 2016-10-05 | 安徽旭峰电容器有限公司 | Wear-resistant flexible composite separator material used for supercapacitor |
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| CN101707241A (en) * | 2009-11-27 | 2010-05-12 | 青岛生物能源与过程研究所 | Diaphragm for lithium-air battery and preparation method thereof |
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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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984194A (en) * | 2017-04-25 | 2017-07-28 | 浙江大学 | A kind of modifying super hydrophobicity nano fibrous membrane and its preparation method and application |
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| CN109056194A (en) * | 2018-07-12 | 2018-12-21 | 东华大学 | A kind of flexibility Li-La-Ti oxygen ceramic nanofibers membrane material and preparation method thereof |
| CN113493958A (en) * | 2020-04-05 | 2021-10-12 | 北京化工大学 | Polyimide nanofiber membrane coaxially coated with boehmite and preparation method thereof |
| CN117153576A (en) * | 2023-07-26 | 2023-12-01 | 哈尔滨理工大学 | A preparation method for solid-state lithium-ion capacitors based on double-doped activated carbon |
| CN117153576B (en) * | 2023-07-26 | 2024-04-05 | 哈尔滨理工大学 | A method for preparing a solid-state lithium ion capacitor based on double-doped activated carbon |
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