CN104157815B - A kind of Bacterial cellulose porous membrane and preparation method thereof - Google Patents

A kind of Bacterial cellulose porous membrane and preparation method thereof Download PDF

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Publication number
CN104157815B
CN104157815B CN201410416648.7A CN201410416648A CN104157815B CN 104157815 B CN104157815 B CN 104157815B CN 201410416648 A CN201410416648 A CN 201410416648A CN 104157815 B CN104157815 B CN 104157815B
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bacterial cellulose
porous membrane
film
cellulose porous
lithium ion
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CN201410416648.7A
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Chinese (zh)
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CN104157815A (en
Inventor
蒋峰景
钟春燕
章俊良
余晴春
钟宇光
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海南光宇生物科技有限公司
上海交通大学
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409Separators, membranes or diaphragms characterised by the material
    • H01M50/411Organic material
    • H01M50/429Natural polymers
    • H01M50/4295Natural cotton, cellulose or wood
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409Separators, membranes or diaphragms characterised by the material
    • H01M50/44Fibrous material
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403Manufacturing processes of separators, membranes or diaphragms
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides a kind of Bacterial cellulose porous membrane for lithium ion battery separator, be that hot repressing obtains after drying by after the water organic solvent displacement in bacterial cellulose wet-coating.The thickness of described Bacterial cellulose porous membrane is less than 40 microns, and porosity is more than 50%.The present invention still further provides its preparation method.The lithium ion battery separator using the Bacterial cellulose porous membrane of the present invention to prepare has the feature that porosity is high and ionic conductivity is high, the beneficially industrialization process of propulsion power lithium ion battery separator.The preparation method of Bacterial cellulose porous membrane of the present invention, has preparation technology simple, and process cycle is short, is suitable for the feature of large-scale production.

Description

A kind of Bacterial cellulose porous membrane and preparation method thereof
Technical field
The present invention relates to lithium ion battery preparing technical field, especially relate to a kind of thin for lithium ion battery separator Fungin porous membrane and preparation method thereof.
Background technology
Barrier film is the core component of lithium ion battery, has been largely fixed the performance of lithium ion battery, safety, has made By important performance indexes such as life-spans.Novel lithium ion power battery working environment compared with conventional lithium ion battery is more complicated, needs Want more powerful discharge and recharge, higher safety and longer service life.Traditional lithium ion battery separator cannot meet The performance requirement of electrokinetic cell.Therefore, develop high performance new type power lithium-ion membrane have become as current American, Europe, The key areas of the auto industry developed countries and regions technology competitions such as Japan.Diaphragm of power lithium ion battery technology will be to the world The competition situation of new-energy automobile produces important impact.
At present, in lithium rechargeable battery industry, wide variety of micro-pore septum almost all uses polyolefin micropore Film, the method mainly obtains hemicrystalline thin polymer film by melt extruding, then stretches it, in order at thin film The a lot of micropore of middle generation, its manufacture process need not solvent, and throughput rate is higher, and high material used is polypropylene (PP) and gathers Ethylene (PE), belongs to one of the most cheap membrane material.But this kind of microporous membrane there is also a lot of shortcoming, as film aperture, crack up to 0.4 μm, the widest 0.04 μm, voidage is up to about 40%.Because liquid absorption is low, limit the raising of lithium ionic mobility, unfavorable Large current density in battery;Meanwhile, polypropylene ductility is poor, and surface can be low, belongs to hard bonding plastics, is unfavorable for positive and negative The bonding of pole piece, barrier film is combined with electrode interface not tight, affects the energy density of battery;Additionally, this method equipment is complicated, make Relatively costly, the most costly, the production cost of battery rises price the most accordingly.Additionally, the heat-shrinkable of conventional membrane is the tightest Weight, melt temperature is relatively low, and (PP is about 165oC), these features make conventional membrane cannot meet the requirement of electrokinetic cell safety.
In order to solve the problems referred to above, all competitively developing high-performance power battery barrier film with countries and regions such as U.S., days.Beautiful State have developed a kind of high performance lithium ion battery barrier film (Energain) based on nanofiber spining technology in 2007, specially Door is for power lithium-ion battery.After using this barrier film, the power of battery can improve 15%-30%, improves 20% service life, The safety of battery is greatly improved.EVONIC company of Germany has been developed over a High-performance diaphragm being specifically designed to electrokinetic cell (SEPARION®), the safe temperature of this film reaches 210oC, percent thermal shrinkage is less than 1% (200oC, 24h), wellability is obviously improved, There is outstanding heat stability and chemical stability.Di Ren technical products company limited under Di Ren group of Japan was in 2013 April 26 was announced, company develops the aramid nano-fiber that can be mass-produced first, and this fiber has higher quality, can carry For the most heat-resisting and antioxygenic property.This nanofiber uses the heat-resisting meta-aramid of Teijinconex that Di Ren company is proprietary Manufacturing, its size uniform, diameter is only hundreds of nanometer.It is reported, the form with non-woven sheet is applied to by aramid nano-fiber The manufacture of lithium ion battery (LIBs) barrier film, company will carry out commercially producing of this fiber in 2014.It is introduced, till now Till, the aramid nano-fiber of Di Ren company produces the most in the lab, and its sheet material produced can keep shape at 300 DEG C. Aramid nano-fiber is high temperature resistant, sludge proof performance can strengthen automobile lithium ion point and know and the safety of static electric power storage, Ensure that battery reduces the danger of fire in high power capacity, high-energy-density application, than traditional barrier film more advantage.Aramid fiber nanometer Fiber non-woven sheet material can be applicable to other features of battery diaphragm and includes: has high porosity and can promote that electrolyte flows smoothly Dynamic, thus have the output of higher electric power and quickly-chargeable ability;Surface area is big, has nanofiber feature, and high hole Rate, when ionic conductivity declines, still can make electrolyte the most effectively keep the performance of battery;As non-woven Sheet material, compared with traditional polyolefin-based separator, makes electrolyte absorption rapider, contributes to shortening and make electrolyte be poured into battery institute The time needed, thus reduce the production cost of high capacity cell.
Bacterial cellulose is the extracellular fiber element produced by microorganism (predominantly antibacterial), the earliest by British scientist Brown found in 1886.Compared with plant cellulose, bacterial fibers have many features, such as high water-holding capacity;Train in static state Under the conditions of Yanging, there is high Young's modulus, high-tensile and splendid shape and maintain ability;High-crystallinity;Ultra-fine (nanoscale) Fibrous reticular structure;The high-altitude fixed rate of interest (> 90%);High-purity (99 % are above cellulose);Higher biocompatibility and good Biodegradability;Physical property controllable etc. during biosynthesis.Because Bacterial cellulose is at purity, absorbency, physics and machine The aspects such as tool performance have above-mentioned premium properties, so people attach great importance to its applied research in every field, at lithium ion Battery diaphragm aspect also has commercial applications potentiality widely.
But, bacterial cellulose wet-coating is processed into lithium ion battery separator needs to overcome several key technical problem: (1) The thickness of cellulosic separator should be less than 40 microns;(2) cellulosic separator thickness is uniform;(3) Bacterial cellulose barrier film should have relatively High voidage.And the techniques such as traditional lyophilization, supercritical drying have a complex process, cost is high, arid cycle length etc. Shortcoming.The mode convection drying bacterial cellulose wet-coating barrier film using hot pressing then has that energy consumption is big, membrane porosity is little, ion guide The shortcoming that electricity rate is low.
Summary of the invention
The problem existed for above-mentioned key technology, the invention provides one and has higher porosity and ionic conductivity The Bacterial cellulose porous membrane for lithium ion battery separator, with and preparation method thereof, described preparation method is simple, high Effect, the Bacterial cellulose porous membrane prepared has the advantages that porosity is high and ionic conductivity is high, can be used for preparing lithium Ion battery barrier film.
The technical scheme is that
A kind of Bacterial cellulose porous membrane for lithium ion battery separator, it is by the water in bacterial cellulose wet-coating After replacing with organic solvent, hot repressing obtains after drying.
Described organic solvent is preferably the combination of one or more in acetone, methanol, ethanol, isopropanol, oxolane.
Described bacterial cellulose wet-coating is that the Bacterial cellulose that fermentation obtains contains moisture film.
The preparation method of Bacterial cellulose porous membrane of the present invention, comprises the steps of
(1) bacterial cellulose wet-coating is placed on precommpression 2 ~ 30 seconds under 0.01 ~ 1.0 MPa pressure;
(2) bacteria cellulose film after precommpression is put into immersion 5 ~ 15 min in organic solvent, the water in film is replaced Out;
(3) bacteria cellulose film after being replaced by organic solvent carries out hot pressing under 0.01 ~ 1.0 MPa pressure dries 5 ~ 20 Min, heating-up temperature is 40 ~ 80oC。
Organic solvent in step (2) is preferably one or more in acetone, methanol, ethanol, isopropanol, oxolane Combination.
Bacterial cellulose wet-coating in step (1) is that the Bacterial cellulose that fermentation obtains contains moisture film.
The Bacterial cellulose porous membrane obtained according to said method, thickness is less than 40 microns, and porosity is more than 50%.Non- It is adapted to prepare lithium ion battery separator.Its resistance is much smaller than the resistance directly drying the film product obtained simultaneously so that use Its lithium ion battery separator prepared has the feature that porosity is high and ionic conductivity is high, beneficially propulsion power lithium-ion electric The industrialization process of pond barrier film.The preparation method of Bacterial cellulose porous membrane of the present invention, has preparation technology simple, Process cycle is short, is suitable for the feature of large-scale production.
Accompanying drawing explanation
Fig. 1 is the bacteria cellulose film that the Bacterial cellulose barrier film prepared by the present invention is prepared with traditional direct oven drying method Relatively, the membrane electrical resistance that wherein prepared by the present invention only has 2.5 Europe to resistance ratio in the electrolytic solution, and prepared by direct drying method every Membrane resistance has 9.5 Europe, and the electrical conductivity of Bacterial cellulose porous membrane prepared by the present invention is apparently higher than the direct stoving process of tradition The bacteria cellulose film of preparation;
Fig. 2 is the relation of the Bacterial cellulose barrier film prepared of present invention electrical conductivity in the electrolytic solution and temperature.
Detailed description of the invention
Below embodiments of the invention are elaborated.The present embodiment is lower real premised on technical solution of the present invention Execute, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment. It should be pointed out that, to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make Some deformation and improvement, these broadly fall into protection scope of the present invention.
Embodiment 1:
The bacterial cellulose wet-coating that 10 mm are thick is placed on precommpression 30 seconds under 0.01MPa pressure, by the antibacterial after precommpression Cellulose membrane is put into and is soaked 5 min in acetone, and the bacteria cellulose film after then being replaced by acetone enters under 0.01 MPa pressure 5 min are dried in row hot pressing, and heating-up temperature is 80oC.Obtain Bacterial cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 20 Rice, porosity is more than 50%, has high ion conductivity (as shown in Figure 2) in the electrolytic solution.
Embodiment 2:
The bacterial cellulose wet-coating that 15 mm are thick is placed on precommpression 15 seconds under 0.05MPa pressure, by the antibacterial after precommpression Cellulose membrane is put into and is soaked 10 min in methanol, is then entered under 0.05 MPa pressure by the bacteria cellulose film after methanol replacement 10 min are dried in row hot pressing, and heating-up temperature is 60oC.Obtain Bacterial cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 30 Rice, porosity is more than 50%, and ionic conductivity in the electrolytic solution is similar to Example 1.
Embodiment 3:
The bacterial cellulose wet-coating that 8 mm are thick is placed on precommpression 2 seconds under 0.1MPa pressure, the antibacterial after precommpression is fine Dimension element film is put into and is soaked 15 min in ethanol, is then carried out under 0.1 MPa pressure by the bacteria cellulose film after ethanol replacement 15 min are dried in hot pressing, and heating-up temperature is 40oC.Obtain Bacterial cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 20 Rice, porosity is more than 50%, and ionic conductivity in the electrolytic solution is similar to Example 1.
Embodiment 4:
The bacterial cellulose wet-coating that 16 mm are thick is placed on precommpression 10 seconds under 0.03MPa pressure, by the antibacterial after precommpression Cellulose membrane is put into and is soaked 20 min in isopropanol, and the bacteria cellulose film after then being replaced by isopropanol is at 0.06 MPa pressure Under carry out hot pressing and dry 20 min, heating-up temperature is 50oC.Obtain Bacterial cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 30 Rice, porosity is more than 50%, and ionic conductivity in the electrolytic solution is similar to Example 1.
Embodiment 5:
The bacterial cellulose wet-coating that 20 mm are thick is placed on precommpression 20 seconds under 0.08MPa pressure, by the antibacterial after precommpression Cellulose membrane is put into and is soaked 18 min in oxolane, and the bacteria cellulose film after then being replaced by oxolane is at 0.04 MPa Carrying out hot pressing under pressure and dry 12 min, heating-up temperature is 70oC.Obtain Bacterial cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 40 Rice, porosity is more than 50%, and ionic conductivity in the electrolytic solution is similar to Example 1.
Embodiment 6:
The bacterial cellulose wet-coating that 12 mm are thick is placed on precommpression 28 seconds under 0.02MPa pressure, by the antibacterial after precommpression Cellulose membrane puts into mixed solvent (mixed volume is than 1:1) middle immersion 13 min of methanol and oxolane, is then put by solvent Bacteria cellulose film after changing carries out hot pressing under 0.07MPa pressure dries 16 min, and heating-up temperature is 65oC.Obtain antibacterial Cellulose porous membrane.
The main chemical compositions of described Bacterial cellulose porous membrane is Bacterial cellulose, and film thickness is micro-less than 20 Rice, porosity is more than 50%, and ionic conductivity in the electrolytic solution is similar to Example 1.

Claims (9)

1. the Bacterial cellulose porous membrane for lithium ion battery separator, it is characterised in that: it is by Bacterial cellulose After water in wet film is replaced with organic solvent, hot repressing obtains after drying.
Bacterial cellulose porous membrane the most according to claim 1, it is characterised in that: described organic solvent is acetone, first The combination of one or more in alcohol, ethanol, isopropanol, oxolane.
Bacterial cellulose porous membrane the most according to claim 1, it is characterised in that: described bacterial cellulose wet-coating is for sending out The Bacterial cellulose that ferment obtains contains moisture film.
Bacterial cellulose porous membrane the most according to claim 1, it is characterised in that: described Bacterial cellulose porous membrane Thickness less than 40 microns, porosity is more than 50%.
5. the preparation method of the Bacterial cellulose porous membrane described in claim 1, it is characterised in that comprise the steps of
(1) bacterial cellulose wet-coating is placed on precommpression 2 ~ 30 seconds under 0.01 ~ 1.0 MPa pressure;
(2) bacteria cellulose film after precommpression is put into immersion 5 ~ 15 min in organic solvent, the water in film is cemented out;
(3) bacteria cellulose film after being replaced by organic solvent carries out hot pressing under 0.01 ~ 1.0 MPa pressure dries 5 ~ 20 Min, heating-up temperature is 40 ~ 80oC。
Preparation method the most according to claim 5, it is characterised in that: the organic solvent in step (2) be acetone, methanol, The combination of one or more in ethanol, isopropanol, oxolane.
Preparation method the most according to claim 5, it is characterised in that: the bacterial cellulose wet-coating in step (1) is fermentation The Bacterial cellulose obtained contains moisture film.
8. the Bacterial cellulose porous membrane that the preparation method described in any one of claim 5-7 prepares, it is characterised in that: The thickness of described Bacterial cellulose porous membrane is less than 40 microns, and porosity is more than 50%.
9. the Bacterial cellulose porous membrane described in claim 8 is used for preparing lithium ion battery separator.
CN201410416648.7A 2014-08-22 2014-08-22 A kind of Bacterial cellulose porous membrane and preparation method thereof CN104157815B (en)

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CN106299213B (en) * 2015-05-26 2019-02-19 中国科学院金属研究所 A kind of bacteria cellulose-base microporous compound film and its preparation method and application
CN106299212B (en) * 2015-05-26 2019-03-29 中国科学院金属研究所 A kind of lithium electricity composite diaphragm and preparation method thereof with three-dimensional net structure
CN106450115B (en) * 2015-08-07 2019-08-09 海南椰国食品有限公司 Inorganic coating bacteria cellulose porous membrane and preparation method thereof
CN106531929A (en) * 2015-09-15 2017-03-22 海南椰国食品有限公司 Drying process of ceramic coated bacterial cellulose porous thin film
CN106549127A (en) * 2015-09-18 2017-03-29 海南椰国食品有限公司 For preparing the drying means of the bacteria cellulose material of lithium ion battery separator
CN106129311B (en) * 2016-08-31 2019-04-19 合肥国轩高科动力能源有限公司 A kind of preparation method of lithium ion battery separator material
CN106531931B (en) * 2016-11-10 2018-11-20 武汉纺织大学 A kind of preparation method of metal oxide-cellulose composite diaphragm
CN106601990B (en) * 2016-12-26 2019-06-21 南京理工大学 It is a kind of based on the N doping carbonization anode of bacteria cellulose, lithium-sulfur cell and preparation method thereof
CN106654122A (en) * 2017-01-18 2017-05-10 山东纳美德生物科技有限公司 Preparation method of power lithium ion battery diaphragm
CN109841899B (en) * 2017-11-28 2020-12-11 中国科学院上海硅酸盐研究所 Preparation method of three-dimensional network polymer gel electrolyte membrane based on bacterial cellulose
CN108448028B (en) * 2017-12-29 2021-03-02 深圳中兴新材技术股份有限公司 Lithium ion battery diaphragm and preparation method thereof
CN108126248A (en) * 2018-03-05 2018-06-08 涂青山 A kind of preparation method of porous bacteria cellulose membrane material
CN109037556A (en) * 2018-07-04 2018-12-18 东华大学 Functional lithium-sulfur cell diaphragm and preparation method thereof

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US20080220333A1 (en) * 2004-08-30 2008-09-11 Shoichiro Yano Lithium Ion Conductive Material Utilizing Bacterial Cellulose Organogel, Lithium Ion Battery Utilizing the Same and Bacterial Cellulose Aerogel
CN102170021A (en) * 2011-03-16 2011-08-31 海南椰国热带水果食品加工有限公司 Gel electrolyte film of lithium battery and preparation method of gel electrolyte film
CN102522515A (en) * 2011-12-22 2012-06-27 中国科学院青岛生物能源与过程研究所 Cellulose/polymer fiber composite diaphragm material for lithium secondary battery and preparation method thereof

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