CN109244329A - The preparation method of fiber base lithium ion battery separator - Google Patents
The preparation method of fiber base lithium ion battery separator Download PDFInfo
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- CN109244329A CN109244329A CN201811120172.7A CN201811120172A CN109244329A CN 109244329 A CN109244329 A CN 109244329A CN 201811120172 A CN201811120172 A CN 201811120172A CN 109244329 A CN109244329 A CN 109244329A
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- cellulose
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- lithium ion
- ion battery
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
-
- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention proposes a kind of preparation methods of fiber base lithium ion battery separator, comprising the following steps: 1) prepares nano-cellulose suspension；2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, after dispersion liquid is warming up to 60~80 DEG C, silane coupling agent is added and carries out reacting 1~3h with sodium alginate；3) spinning: by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2), mixed liquor is subjected to vacuum defoamation, spinning solution is obtained after deaeration, spinning solution is added in syringe, carry out electrostatic spinning, cellulose basement membrane is formed, then gained cellulose basement membrane is dried.Not only porosity is high for the diaphragm that this method is prepared, but also heat insulation and lithium ion conductivity are good.
Description
Technical field
The invention belongs to battery diaphragm technical fields, and in particular to a kind of preparation side of fiber base lithium ion battery separator
Method.
Background technique
Cellulose is a kind of renewable resource of rich reserves in nature, is had using the material that cellulose is produced as raw material
Many good characteristics, if dielectric constant is high, puncture is strong, chemical stability is good, thermostabilization is good, degradable etc., in papermaking, electricity
The fields such as sub- product, industrial processes, medicine are widely used.In recent years, many membrane material researchers were devoted to research and develop
Inexpensive, reproducible cellulosic material prepares High-performance diaphragm, especially based on cellulose, modification and the cellulose of enhancing
The lithium ion battery separator of body raw material, and and polyalkene diaphragm in heat resistance, puncture, intensity, resistance sizes, high voltage withstanding
Property etc. is compared research.In cellulosic molecule, intermolecular hydrogen bonding and under the action of Van der Waals force, cellulose divides greatly
Subchain flocks together the cellulose primitive fibril formd with cellulose Ⅰ crystalline structure.But cellulose in nature
Aggregation is not a kind of perfect crystal structure, and there is also a large amount of amorphous domains.It can be by way of physics, chemistry
Cellulose primitive fibril effectively, is completely stripped out from native cellulose state of aggregation.
Lithium ion battery has that energy density is high, specific power is big, cycle performance as a kind of high-energy green secondary cell
Good, memory-less effect, it is pollution-free the features such as, be widely used to Intelligent mobile equipment, hybrid vehicle, electric vehicle, the sun
The new energy fields such as energy electricity generation system, quickly grow.These fields do not require nothing more than battery with high-energy, power density, to electricity
The security requirement in pond is also higher and higher.And diaphragm is influence and determine lithium ion battery chemical property and safety important
Factor.Currently, the diaphragm material of commercial lithium-ion batteries mainly still uses polyethylene, microporous polypropylene membrane.But poly- second
Alkene, polypropylene diaphragm are poor to electrolyte compatibility, there are imbibition rate and protect the low deficiency of liquid rate, electrolyte is easy to happen side
Leakage, there are hidden danger for the safety of battery.In addition, diaphragm currently on the market it is all simple play simple buffer action, in phase
Under same aperture, not any help of the raising to lithium ion conductivity.
Summary of the invention
The present invention proposes a kind of preparation method of fiber base lithium ion battery separator, and the diaphragm that this method is prepared is not only
Porosity is high, and heat insulation and lithium ion conductivity are good.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of fiber base lithium ion battery separator, comprising the following steps:
1) it prepares nano-cellulose suspension: cellulose or cellulose derivative is added in TEMPO catalyst system,
It adjusts pH to 9.0~10.0 to be reacted, obtains nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, by dispersion liquid liter
Temperature adds silane coupling agent and carries out reacting 1~3h with sodium alginate to after 60~80 DEG C；
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carries out vacuum defoamation, and spinning solution is obtained after deaeration, spinning solution is added in syringe, carries out electrostatic spinning, is formed fine
Plain basement membrane is tieed up, then gained cellulose basement membrane is dried.
Preferably, the cellulose derivative used in the step 1) is cellulose nitrate, cellulose ethanoate, fiber
Plain acetate butyrate, cellulose sulfonate, methylcellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, cyanogen
One of ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose are a variety of.
Preferably, the mass ratio of the nano aluminium oxide in the step 2) and the emulsion acrylic resin is 10
~20:100, the mass ratio of the nano aluminium oxide and the silane coupling agent are 100:4~8, the nano aluminium oxide with
The mass ratio of the sodium alginate is 100:1~3.
Preferably, the silane coupling agent is KH550 or KH560.
Preferably, the electrostatic spinning in the step 3) specifically comprises the processes of: in voltage be 20~35kV, to receive distance be
10~20cm, flow be 2~4mL/h, spinning temperature be 40~60 DEG C, receive drum rotation speed be 10~25m/h under conditions of into
Row electrostatic spinning forms fiber basement membrane.
Preferably, dry specific steps are as follows: the fiber basement membrane that electrostatic spinning is formed is put into vacuum drying oven, 45~
Dry 10~12h at a temperature of 55 DEG C.
Beneficial effects of the present invention:
1) nano pulp of the invention is mainly by nano aluminium oxide, silane coupling agent and sodium alginate in acrylic resin
Reaction is prepared in lotion, not only makes nano aluminium oxide dispersibility more preferable, also solves nanometer alumina slurry and do not have
The problem of standby lithium ion conduction ability.
2) preparation method of fiber base lithium ion battery separator of the invention is that nano pulp and nano-cellulose suspend
Spinning is carried out after liquid mixing to be prepared, and not only there is very high heat-proof quality, also there is good porosity.
3) present invention is prepared fiber base lithium battery diaphragm and can apply in lithium battery, the lithium-ion electric of battery diaphragm
Conductance is 5.6~7.9 × 10-3Scm-1, at 1.0C, after 100 circulations, the lithium battery capacity conservation rate of battery diaphragm
95% or more, the porosity of battery diaphragm reaches 75% or more.
Specific embodiment
Embodiment 1
A kind of preparation method of fiber base lithium ion battery separator, comprising the following steps:
1) it prepares nano-cellulose suspension: cellulose is added to TEMPO (tetramethyl piperidine nitrogen oxides) catalytic body
In system, adjusts pH to 9.6 and reacted, obtain nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, by dispersion liquid liter
Temperature adds silane coupling agent KH560 and carries out reacting 2h with sodium alginate to after 70 DEG C；Nano aluminium oxide and acrylic acid
The mass ratio of resin emulsion is 16:100, and the mass ratio of nano aluminium oxide and silane coupling agent is 100:6, nano aluminium oxide
Mass ratio with sodium alginate is 100:2.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 25kV, receive away from
From for 16cm, flow 3mL/h, spinning temperature is 50 DEG C, receives under conditions of drum rotation speed is 15m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, cellulose basement membrane is formed, then gained cellulose basement membrane is put into vacuum drying oven, dries at 50 °C
10h.
The lithium ion conductivity of the battery diaphragm of the present embodiment is 6.6 × 10-3Scm-1, at 1.0C, 100 circulations
Afterwards, the lithium battery capacity conservation rate 96% of battery diaphragm, the porosity of battery diaphragm reach 82%.
Embodiment 2
A kind of preparation method of fiber base lithium ion battery separator, comprising the following steps:
1) it prepares nano-cellulose suspension: cellulose nitrate is added to TEMPO (tetramethyl piperidine nitrogen oxides)
In catalyst system, adjusts pH to 9.0 and reacted, obtain nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, by dispersion liquid liter
Temperature adds Silane coupling agent KH550 and carries out reacting 3h with sodium alginate to after 60 DEG C；Nano aluminium oxide and acrylic acid
The mass ratio of resin emulsion is 10:100, and the mass ratio of nano aluminium oxide and silane coupling agent is 100:8, nano aluminium oxide
Mass ratio with sodium alginate is 100:1.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 20kV, receive away from
From for 10cm, flow 2mL/h, spinning temperature is 60 DEG C, receives under conditions of drum rotation speed is 10m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, forms cellulose basement membrane, then gained cellulose basement membrane is put into vacuum drying oven, it is dry at a temperature of 45 DEG C
12h.
The lithium ion conductivity of the battery diaphragm of the present embodiment is 5.6 × 10-3Scm-1, at 1.0C, 100 circulations
Afterwards, the lithium battery capacity conservation rate 95% of battery diaphragm, the porosity of battery diaphragm reach 76%.
Embodiment 3
A kind of preparation method of fiber base lithium ion battery separator, comprising the following steps:
1) it prepares nano-cellulose suspension: carboxymethyl cellulose is added to TEMPO (tetramethyl piperidine nitrogen oxides)
In catalyst system, adjusts pH to 9.6 and reacted, obtain nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, by dispersion liquid liter
Temperature adds silane coupling agent KH560 and carries out reacting 1h with sodium alginate to after 80 DEG C；Nano aluminium oxide and acrylic acid
The mass ratio of resin emulsion is 20:100, and the mass ratio of nano aluminium oxide and silane coupling agent is 100:4, nano aluminium oxide
Mass ratio with sodium alginate is 100:3.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 35kV, receive away from
From for 20cm, flow 4mL/h, spinning temperature is 40 DEG C, receives under conditions of drum rotation speed is 25m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, forms cellulose basement membrane, then gained cellulose basement membrane is put into vacuum drying oven, it is dry at a temperature of 55 DEG C
10h.
The lithium ion conductivity of the battery diaphragm of the present embodiment is 7.9 × 10-3Scm-1, at 1.0C, 100 circulations
Afterwards, 97% or more the lithium battery capacity conservation rate of battery diaphragm, the porosity of battery diaphragm reaches 85%.
Comparative example 1
A kind of preparation method of fiber base lithium ion battery separator, comprising the following steps:
1) it prepares nano-cellulose suspension: cellulose is added to TEMPO (tetramethyl piperidine nitrogen oxides) catalytic body
In system, adjusts pH to 9.6 and reacted, obtain nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, by dispersion liquid liter
Temperature adds silane coupling agent KH560 and carries out reaction 2h to after 70 DEG C；Nano aluminium oxide and emulsion acrylic resin
Mass ratio is 16:100, and the mass ratio of nano aluminium oxide and silane coupling agent is 100:6.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 25kV, receive away from
From for 16cm, flow 3mL/h, spinning temperature is 50 DEG C, receives under conditions of drum rotation speed is 15m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, cellulose basement membrane is formed, then gained cellulose basement membrane is put into vacuum drying oven, dries at 50 °C
10h.
The lithium ion conductivity of the battery diaphragm of the present embodiment is 2.6 × 10-4Scm-1, at 1.0C, 100 circulations
Afterwards, the lithium battery capacity conservation rate 94% of battery diaphragm, the porosity of battery diaphragm reach 73%.
Fiber base lithium ion battery separator is prepared at 200 DEG C in embodiment 1-3 and comparative example 1 and heats 6h, according to
The change in size of heating front and back diaphragm vertical and horizontal, calculates the shrinking percentage of diaphragm vertical and horizontal, the results are shown in Table 1.
Table 1
| Diaphragm sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Lateral percent thermal shrinkage (%) | 0.2 | 0.3 | 0.2 | 0.6 |
| Longitudinal percent thermal shrinkage (%) | 0.2 | 0.4 | 0.3 | 0.7 |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of fiber base lithium ion battery separator, which comprises the following steps:
1) it prepares nano-cellulose suspension: cellulose or cellulose derivative is added in TEMPO catalyst system, adjust
PH to 9.0~10.0 is reacted, and obtains nano-cellulose suspension after reaction；
2) prepared by nano pulp: nano aluminium oxide being put into emulsion acrylic resin and is dispersed, dispersion liquid is warming up to
After 60~80 DEG C, adds silane coupling agent and carry out reacting 1~3h with sodium alginate；
3) spinning: the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2) will mix
Liquid carries out vacuum defoamation, and spinning solution is obtained after deaeration, spinning solution is added in syringe, carries out electrostatic spinning, forms cellulose
Basement membrane, then gained cellulose basement membrane is dried.
2. the preparation method of fiber base lithium ion battery separator according to claim 1, which is characterized in that the step 1)
In cellulose derivative used be cellulose nitrate, cellulose ethanoate, cellulose acetate butyrate, cellulose sulfonic acid
Ester, methylcellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, cyanethyl cellulose, hydroxypropyl cellulose,
One of hydroxypropyl methyl cellulose is a variety of.
3. the preparation method of fiber base lithium ion battery separator according to claim 1, which is characterized in that the step 2)
In the nano aluminium oxide and the emulsion acrylic resin mass ratio be 10~20:100, the nano aluminium oxide with
The mass ratio of the silane coupling agent is 100:4~8, and the mass ratio of the nano aluminium oxide and the sodium alginate is 100:
1~3.
4. the preparation method of fiber base lithium ion battery separator according to claim 3, which is characterized in that the silane is even
Connection agent is KH550 or KH560.
5. the preparation method of fiber base lithium ion battery separator according to claim 1, which is characterized in that the step 3)
In electrostatic spinning specifically comprises the processes of: in voltage be 20~35kV, receiving distance is 10~20cm, and flow is 2~4mL/h,
Spinning temperature is 40~60 DEG C, receives under conditions of drum rotation speed is 10~25m/h and carries out electrostatic spinning, forms fiber basement membrane.
6. the preparation method of fiber base lithium ion battery separator according to claim 1, which is characterized in that dry is specific
Step are as follows: the fiber basement membrane that electrostatic spinning is formed is put into vacuum drying oven, dry 10~12h at a temperature of 45~55 DEG C, i.e.,
It can.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110299497A (en) * | 2019-07-03 | 2019-10-01 | 新乡芯蕴新能源有限公司 | A kind of electrostatic spinning lithium battery diaphragm material and No. 5, No. 7 rechargeable lithium batteries |
| CN112397849A (en) * | 2020-10-28 | 2021-02-23 | 中国地质大学（北京） | High-temperature-resistant flame-retardant battery diaphragm and preparation method and application thereof |
| CN113794034A (en) * | 2021-08-03 | 2021-12-14 | 惠州锂威新能源科技有限公司 | Self-supporting diaphragm and preparation method thereof, composite pole piece and secondary battery |
| CN116111275A (en) * | 2023-01-11 | 2023-05-12 | 河北光兴半导体技术有限公司 | Composite diaphragm and preparation method and application thereof |
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