CN106299469B - A kind of adding method of lithium-ion battery electrolytes organic solid additive - Google Patents
A kind of adding method of lithium-ion battery electrolytes organic solid additive Download PDFInfo
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- CN106299469B CN106299469B CN201510243351.XA CN201510243351A CN106299469B CN 106299469 B CN106299469 B CN 106299469B CN 201510243351 A CN201510243351 A CN 201510243351A CN 106299469 B CN106299469 B CN 106299469B
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- organic solid
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- 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
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- 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
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Abstract
The purpose of the present invention is to provide a kind of lithium-ion battery electrolytes adding methods of organic solid additive, the electrolyte prepared using the method, it can effectively ensure product quality, a kind of adding method of lithium-ion battery electrolytes organic solid additive, it is characterised in that include the following steps process：Raw material selection, the miscible preparation of the miscible fluid of additive containing high concentration, refined, the metering addition of the miscible fluid of additive containing high concentration, the present invention is safe and environment-friendly, and energy saving, technique, equipment are simple and convenient to operate.Organic solid additive adding method of the present invention has significant advantage compared to after the high temperature melting in industry through utilidor conveying charging.At energy-saving aspect：The fusing of solvent dissolution mechanism higher temperatures has apparent power savings advantages；In addition, for the additive of opposite high added value, identical packaging wall built-up, conveyance conduit are remained after dissolved dilution, material loss residual value is low.
Description
Technical field
The present invention relates to material addition field more particularly to a kind of lithium-ion battery electrolytes organic solid additives
Adding method.
Background technology
As society is higher and higher to environmental protection, energy-saving requirement, lithium ion battery is with its excellent performance quilt
It is considered the choosing of the ideal of high power capacity, high power battery, makes a breakthrough application in industrial energy storage and field of vehicles, electrolysis
For liquid as one of four big critical material of lithium ion battery, the market demand will the lasting increasing with the development of ev industry
It is long.
The a small amount of non-energy storage material used in electrochmical power source, can significantly improve certain performances of battery, such as be electrolysed
Conductivity, positive and negative anodes matching performance, the capacity of battery, cycle efficieny, cycle life, reversible capacity and security performance of liquid etc.,
People to the selection of additive, use and optimize and done a large amount of exploration and trial, the type and quantity of additive also because
And rapid development is obtained.
From the substance classes of additive, the additives of lithium-ion battery electrolytes includes organic additive and inorganic adds
Add agent.Organic additive has many advantages, such as and lithium-ion battery electrolytes intersolubility is good, effect of optimization is good and easy to use, causes
People enough attention have simultaneously obtained rapid development.In contrast, the selection of inorganic additive is faced with larger limitation
Property.From room temperature existence form, additive is divided into additives gas, liquid additive and solid additive.Additives gas
Use so that inner pressure of battery is increased, it is unfavorable to the safety of battery, with electrolyte have preferable intersolubility liquid or solid add
Agent causes the interest of people's bigger.
Because there are several solid additives, it is crystalline solid or waxy solid under room temperature, does not have mobility, current electrolysis liquid
Manufacturing is to the common adding method of organic solid additive：After high temperature melting, warm pipeline is added.Technique now
Operation when energy consumption, dangerous, the organic solvent after fusing is once reveal, and toxic gas easily spreads, is inflammable and explosive at high temperature, matter
Measure it is unstable, lithium-ion battery electrolytes with organic solid additive be chronically under high temperature it is easy to change, decompose.
Invention content
The purpose of the present invention is to provide a kind of lithium-ion battery electrolytes adding method of organic solid additive, profits
The electrolyte prepared with the method, can effectively ensure product quality,
A kind of adding method of lithium-ion battery electrolytes organic solid additive, it is characterised in that include the following steps
Process：
(1) the manner of packing of change organic solid additive is unified：Closed, pressurize is changed to by non-closed, non-pressurize packaging
Packaging；
(2) the miscible preparation of the miscible fluid of additive containing high concentration：By the quick liquid injection port of pail pack, metering in proportion adds
Enter to prepare the basic organic solvent and organic solid additive of target electrolyte, shakes after dissolving each other that be configured to determine containing for component highly concentrated
The miscible fluid of degree additive, a concentration of the 10%~80% of additive；
(3) the miscible fluid of additive containing high concentration is refined：The miscible fluid of additive containing high concentration qualified after testing through de-
It is stored after water, accurate filter filtering for use；
(4) metering addition：Detected after refinement treatment the qualified additive containing high concentration miscible fluid is closed, metering plus
Enter to dissolve in the basic electrolyte after lithium salts, stirring, can packaging and storage after detection is qualified to dissolving each other completely.
The pail pack of the organic solid additive includes feed inlet, liquid injection port, gas vent, and the liquid injection port passes through silk
Button connection quick coupling, the gas vent are attached to automatic overvoltage decompression function.
The pail pack of the organic solid additive is pressure-resistant, corrosion-resistant, organic solvent-resistant material, and material is according to addition
Agent kind physical property difference can choose stainless steel, stainless steel lining tetrafluoroethene, stainless steel lining polyethylene.
The basic organic solvent for compounding high concentration additive miscible fluid can be the base for preparing target electrolyte
Plinth organic solvent：Dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), diethyl carbonate (DEC), ethylene carbonate (EC), carbon
Acid propylene ester (PC), methyl propyl carbonate (MPC), gamma-butyrolacton (GBL), ethyl acetate (EA), ethyl propionate (EP) therein one
Kind is a variety of.
The basic organic solvent for compounding high concentration additive miscible fluid is all high-purity, low after refined
Aqueous solvent, avoids introducing new impurity and moisture, the weight of the basic organic solvent purity >=99.98%, the basis
Organic solvent moisture is less than 7PPm.
The filter element of precision filter material is Kynoar or polytetrafluoroethylene (PTFE), and precision is 0.05~5 μm, to remove
The insoluble matter introduced in additive raw material and in dehydration process.
The method can be used for be under any room temperature solid organic solid additive adding method, the organic solid adds
It is 1,3-propane sultone (PS), succinonitrile (SN), biphenyl (BP), ethyl sulfate (DTD) to add agent.The method can be used for gel
The addition of the gelatinous gelling agent of electrolyte.
The method can be used for the addition of poor fluidity, environmentally sensitive solid additive.
The beneficial effects of the present invention are：The present invention is safe and environment-friendly, and energy saving, technique, equipment are simple and convenient to operate.This hair
Bright organic solid additive adding method is significantly excellent compared to having through utilidor conveying charging after the high temperature melting in industry
Gesture.In terms of stable quality：Easy decomposed metamorphic under organic materials hot soak condition, coloration increase, thus this method by
It is not related to heat temperature raising in material, whole process all operates at room temperature, more can guarantee the quality stability of product, and entirely have
The operation processing procedure of machine solid additive, material all flow under air-tight state, ensure that additive not by external environment because
The interference of element also ensures the stable quality of electrolysis liquid product.In terms of operating environment, safety, occupational health：After high temperature melting
Organic solvent once revealing, toxic gas, which is easily spread, endangers that worker health, organic gas is inflammable and explosive at high temperature, and our
Method whole process room temperature operation, it is comparatively safe reliable.At energy-saving aspect：The fusing of solvent dissolution mechanism higher temperatures has apparent section
It can advantage；For the additive of opposite high added value, identical packaging wall built-up, conveyance conduit are remained after dissolved dilution, material
It is low that residual value is lost.
Specific implementation mode
The present invention is described in further detail With reference to embodiment：
Note：Add additivated reference electrolyte each component content and each index is as follows：
Reference electrolyte：
Ethylene carbonate (EC):Methyl ethyl carbonate (EMC):Diethyl carbonate (DEC)=1:1:1(V)
Lithium hexafluoro phosphate (LiPF6) concentration：1.0mol/L
Coloration (APHA) index：≤50；(measured value：15)
Moisture (Karl_Fischer method) index：≤10PPm；(measured value：7PPm)
Conductivity indices：8.45±0.05ms/cm；(measured value：8.47ms/cm)
The additive amount of additive is：5%
Embodiment 1
1,3-propane sultone (PS) material for taking one barrel of non-airtight package of 10Kg, is put into and is set as the explosion-proof of 50 DEG C of constant temperature
In baking oven, after 72 hours after material completely melt after sample detection moisture content, coloration；Take 1, the 3- propane of one barrel of 10Kg airtight package
The closed methyl ethyl carbonate (EMC) that water content 5PPM is added of sultone (PS) material equivalent, vibration take after being completely dissolved processing
Sample detects moisture content, coloration.
Comparative example 1
Into the electrolyte quota kettle of a 100L it is closed be added 100Kg reference electrolytes, by 5% the close addition of additive amount
1,3-propane sultone (PS) after 5Kg thawings, opening stirring and dissolving sample detection after 2 hours：Moisture, coloration (APHA), electricity
Conductance.
Into the electrolyte quota kettle of a 100L it is closed be added 100Kg reference electrolytes, by 5% 1,3- propane sulphurs
The closed addition 10Kg1 of lactone (PS) content, 3- propane sultones (PS) and the miscible fluid of methyl ethyl carbonate (EMC) are (practical to be electrolysed
In liquid production process, it is molten to consider that equivalent subduction is introduced because adding additivated miscible fluid during preparing basic electrolyte
Dosage), opening stirring and dissolving sample detection after 2 hours：Moisture, coloration (APHA), conductivity.
Embodiment 2
Succinonitrile (SN) material of one barrel of non-airtight package of 10Kg is taken to be put into the explosion-proof baking oven for being set as 80 DEG C of constant temperature,
After 72 hours after material completely melt after sample detection moisture content, coloration；Take succinonitrile (SN) object of one barrel of 10Kg airtight package
Expect that the closed methyl ethyl carbonate (EMC) that water content 5PPM is added of equivalent, vibration are completely dissolved sample detection moisture content, color after processing
Degree.
Comparative example 2
Into the electrolyte quota kettle of a 100L it is closed be added 100Kg reference electrolytes, by 5% the close addition of additive amount
Succinonitrile (SN) after 5Kg thawings, opening stirring and dissolving sample detection after 2 hours：Moisture, coloration (APHA), conductivity.
Into the electrolyte quota kettle of a 100L it is closed be added 100Kg reference electrolytes, by 5% succinonitrile (SN)
Content is closed be added 10Kg succinonitrile (SN) and the miscible fluid of methyl ethyl carbonate (EMC) (in practical electrolyte production process, with
Consider that equivalent reduces the quantity of solvent introduced because adding additivated miscible fluid during basic electrolyte processed), it is molten to open stirring
Sample detection after solution 2 hours：Moisture, coloration (APHA), conductivity.
Contrasting detection data see the table below：
The result shows that preferable using the electrolyte technical indicator that the method for the present invention makes, each index and performance are completely full
The requirement of sufficient lithium ion battery.
The above is only a preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as this hair
Bright protection domain.
Claims (9)
1. a kind of lithium-ion battery electrolytes adding method of organic solid additive, it is characterised in that included the following steps
Journey：
(1) the manner of packing of change organic solid additive is unified：Closed, pressurize packet is changed to by non-closed, non-pressurize packaging
Dress；
(2) the miscible preparation of the miscible fluid of additive containing high concentration：It is metered in proportion to match by the quick liquid injection port of pail pack
The basic organic solvent and organic solid additive of target electrolyte processed, shake are configured to determine containing high concentration adding for component after dissolving each other
Add the miscible fluid of agent, a concentration of the 10%~80% of additive；
(3) the miscible fluid of additive containing high concentration is refined：The miscible fluid of additive containing high concentration qualified after testing through dehydration, essence
It is stored after close filter filtering for use；
(4) metering addition：The miscible fluid that the qualified additive containing high concentration is detected after refinement treatment is closed, metered molten
It solves in the basic electrolyte after lithium salts, stirring, can packaging and storage after detection is qualified to dissolving each other completely.
2. a kind of adding method of lithium-ion battery electrolytes organic solid additive as described in claim 1, feature exist
Include feed inlet, liquid injection port, gas vent in the pail pack of the organic solid additive, the liquid injection port passes through screwed connection
Quick coupling, the gas vent are attached to automatic overvoltage decompression function.
3. a kind of adding method of lithium-ion battery electrolytes organic solid additive as described in claim 1, feature exist
It is made of pressure-resistant, corrosion-resistant, organic solvent-resistant material in the pail pack of organic solid additive, material is according to additive kind
Physical property difference can choose stainless steel, stainless steel lining tetrafluoroethene, stainless steel lining polyethylene.
4. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
It is that the basic organic solvent for compounding high concentration additive miscible fluid is the basic organic solvent for preparing target electrolyte, base
Plinth organic solvent is dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), diethyl carbonate (DEC), ethylene carbonate (EC), carbon
Acid propylene ester (PC), methyl propyl carbonate (MPC), gamma-butyrolacton (GBL), ethyl acetate (EA), ethyl propionate (EP) therein one
Kind is a variety of.
5. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
It is that the basic organic solvent for compounding high concentration additive miscible fluid is high-purity, the low aqueous solvent after refined, avoids
Introduce new impurity and moisture, basic organic solvent purity >=99.98% for compounding high concentration additive miscible fluid
Weight, the basic organic solvent moisture ＜ 7PPm for compounding high concentration additive miscible fluid.
6. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
It is that filter element of precision filter material is Kynoar or polytetrafluoroethylene (PTFE), precision is 0.05~5 μm, to remove additive original
The insoluble matter introduced in material and in dehydration process.
7. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
Be the method can be used for be under any room temperature solid organic solid additive adding method, the organic solid additive
For 1,3-propane sultone (PS), succinonitrile (SN), biphenyl (BP), ethyl sulfate (DTD).
8. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
It is that the method can be used for addition of the gel electrolyte with gelatinous gelling agent.
9. a kind of lithium-ion battery electrolytes adding method of organic solid additive as described in claim 1, feature
It is that the method can be used for the addition of poor fluidity, environmentally sensitive solid additive.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101847752A (en) * | 2010-05-26 | 2010-09-29 | 惠州市德赛聚能电池有限公司 | Additive of electrolytic solution of lithium ion battery |
| CN103594735A (en) * | 2013-11-29 | 2014-02-19 | 湖南高远电池有限公司 | Preparation method for lithium titanate lithium ion battery |
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| US20140178770A1 (en) * | 2012-02-07 | 2014-06-26 | Battelle Memorial Institute | Electrolytes for dendrite-free energy storage devices having high coulombic effciency |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101847752A (en) * | 2010-05-26 | 2010-09-29 | 惠州市德赛聚能电池有限公司 | Additive of electrolytic solution of lithium ion battery |
| CN103594735A (en) * | 2013-11-29 | 2014-02-19 | 湖南高远电池有限公司 | Preparation method for lithium titanate lithium ion battery |
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