CN110265715A - A kind of lithium battery semisolid electrolyte special gel agent and preparation method - Google Patents
A kind of lithium battery semisolid electrolyte special gel agent and preparation method Download PDFInfo
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- CN110265715A CN110265715A CN201910539993.2A CN201910539993A CN110265715A CN 110265715 A CN110265715 A CN 110265715A CN 201910539993 A CN201910539993 A CN 201910539993A CN 110265715 A CN110265715 A CN 110265715A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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- 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
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Abstract
The present invention proposes a kind of lithium battery semisolid electrolyte special gel agent and preparation method, the gelling agent is that polymeric matrix and hydroxypropyl methyl cellulose, fire retardant mixed grinding are first obtained composite particles, then it is sprayed after mixing Perhydropolysilazane, porous mineral with ammonium hydroxide on composite particles surface, be finally completely dispersed obtained cladded type composite particles and dispersing agent using airflow mixer and is made.Special gel agent addition provided by the invention will not generate gel at the initial stage of electrolyte, after greatly improving existing Electrolyte Gelization processing it is difficult to that the defect used is uniformly perfused, and chemical conversion is perfused can substantially uniformity infiltration diaphragm and electrode, increase electrolyte toughness, gel state is changed by liquid, improves the safety of electrolyte.
Description
Technical field
The present invention relates to lithium cell electrolyte technical fields, dedicated solidifying more particularly to a kind of lithium battery semisolid electrolyte
Jelly and preparation method.
Background technique
With the fast development of automobile industry and the strict control of environmental pollution, electric car, which has become, at present works as
One Developing mainstream of modern car industry.Mainstream technology of the lithium battery as current automobile power cell, market are gradually mature.Lithium electricity
Pond is mainly made of positive electrode, negative electrode material and electrolyte.Development with from lithium ion battery to ternary high-energy density, it is right
The requirement of electrolyte is higher and higher.The electrolyte of lithium ion battery is by organic solvent, electrolyte lithium salt and functional additive group
At.Electrolyte carry in the battery between positive and negative anodes transmit charge effect, to the specific capacity of battery, operating temperature range,
Cycle efficieny and security performance etc. play a crucial role.Liquid lithium ionic cell is generallyd use at present, mainly with six
Lithium fluophosphate is dissolved in solvent as electrolyte.Due to using the electrolyte of liquid, generally use the aluminum hull of hard into
Row packaging not only increases weight, and there are the hidden danger such as leakage, explosion.Electrolyte lithium battery energy density is big, but safety
Property, stable charge/discharge, service life always exist problem, become restrict its development bottleneck.
According to existing lithium battery current situation, for lithium battery tertiary cathode unstability, graphite cathode easy peelability, with
And electrolyte itself is inflammable, the problems such as being also easy to produce gas flatulence, it is main at present to be solved by addition additive in the electrolytic solution
Certainly, but limitation is solved.For especially ternary lithium battery there are many defects, safety problem is very troubling.Ternary material
All it is very easy to fever.If heat is conducted cannot in time, battery just has the risk of explosion.However at this stage, in electricity
In the safety in pond, reliability, it is difficult to rely on electrolyte and additive is added solves.New-energy automobile is close to power battery energy
The requirement of degree is all very high.Under the system of prior art route, Yao Tigao energy density can only improve ternary nickel material, but high
The thermal stability of nickel is very poor.So once traditional ternary lithium battery energy density improves, also imply that the decline of stability,
Inside battery thermal response can very acutely, and safety is just at very big problem.
Based on the safety problem of existing electrolyte lithium battery, become the direction of development using solid electrolyte.Solid electrolytic
Electrolyte cell since Solid-state battery electrode and electrolyte are all made of solid matter, solid electrolyte is non-combustible, it is corrosion-free, do not wave
Hair, no leakage, while Li dendrite phenomenon is also overcomed, even if being heated to very high temperature, will not catch fire, thus safety
Property is higher.The maximum difference of solid-state lithium electricity and current lithium battery is solid electrolyte, solid-state lithium electricity use solid electrolyte with
Afterwards, the voltage platform of battery on the one hand can be promoted, the energy density of battery is further promoted；On the other hand, in solid-solid reaction
In reduce the discharge of gas, improve the security performance of battery.Although solid state lithium battery is compared to current mainstream electrolyte lithium
Battery has many advantages, but solid state lithium battery technology is low by solid electrolyte technology conductivity, interface impedance is excessive, cycle-index
Low technological difficulties are difficult quick industrialization in a short time.For this purpose, gel state, semisolid, quasi- solid state battery are technically relatively
It easily realizes, becomes the mainstream of development.
Chinese invention patent application number 201810593201.5 discloses a kind of lithium battery gel-form solid polymer electrolyte, including
Complex polymer, plasticizer and lithium salts electrolyte are constituted, during the preparation process, first will be polyacrylonitrile hydrolyzed, then will be after hydrolysis
Polyacrylonitrile is acidified with strong acid, and after being then acidified polyacrylonitrile dissolution, thionyl chloride is added, after heating reaction, recycling design,
Obtain modified hydrolyzed polyacrylonitrile；It is in mass ratio again 3:1-5:1 compounding by modified hydrolyzed polyacrylonitrile and more aldehyde sodium alginates,
Obtain Complex polymer；After then mixing Complex polymer and plasticizer, heating stirring reaction adds lithium salts electrolyte, stirs
It mixes after mixing, is film-made to get lithium battery gel-form solid polymer electrolyte.Chinese invention patent application number 201811221369.X
Disclose a kind of preparation method of lithium battery gel electrolyte, comprising the following steps: (1) under the conditions of being protected from light, to lithium salt electrolyte
Middle addition urethane acrylate and reactive diluent, and be uniformly mixed, prepare electrolyte slurry；(2) into electrolyte slurry
The phase-change material micro-capsule of 10-15wt% is added and is uniformly mixed；(3) again into electrolyte slurry 3% photoinitiator, by ultraviolet
Light irradiates gelled electrolyte.
In order to solve lithium battery gel state electrolyte at this stage in use, since gel state is different from electrolyte, exist
The defect of poor fluidity, so that the method using the existing gel directly prepared in perfusion leads to gel electrolyte and diaphragm, electricity
The problem of pole wellability is deteriorated, it is necessary to propose a kind of novel lithium battery electrolyte gelling agent, and then improve improvement gel electricity
The wellability of Xie Zhiyu diaphragm, electrode.
Summary of the invention
It is inconvenient for use for current lithium battery gel electrolyte, insufficient defect is infiltrated with diaphragm, electrode, and fill
React the problem to form gel process complexity after note again, the present invention propose a kind of lithium battery semisolid electrolyte special gel agent and
Preparation method so that gel electrolyte and diaphragm, electrode can substantially uniformity infiltrate, while improving the safety of electrolyte
Property.
To solve the above problems, the invention adopts the following technical scheme:
A kind of preparation method of lithium battery semisolid electrolyte special gel agent, it is specific the preparation method is as follows:
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent.
Preferably, the polymeric matrix is polymethyl methacrylate, in polyethylene glycol oxide, polyamide, polyacrylonitrile
A combination of one or more.
Preferably, the fire retardant is polyphosphazene.
Preferably, the porous mineral is one kind of nanoscale zeolite powder, alumina aerogels, silica aerogel
Or two or more combination.
Preferably, the pressure of high-pressure atomization described in step (1) is 10-30bar, mist flow 1.2-3L/min.
Hydroxypropyl methyl cellulose belongs to a kind in nonionic cellulose compound ether, be it is a kind of it is semi-synthetic,
Sluggish, viscoelasticity polymer can be used as dispersion suspension, thickening, emulsification and adhesive and use.Hydroxypropyl methyl cellulose is real
Border is a kind of methylcellulose through epoxy pronane modification, water-insoluble with the cold-water-soluble and heat similar with methylcellulose
Characteristic, when environment temperature is more than certain temperature, cellulose ether can be precipitated from water, lose water-retaining property, realize gelation.Due to
It is modified containing hydroxypropyl, greatly improve the temperature of its gelation in the hot water compared with methylcellulose.Therefore, the present invention passes through
Hydroxypropyl methyl cellulose dixie cup gelling agent is added, not only can effectively assist gel-forming, and when electrolyte generates water, easily
In aquation occurs, so that fixed water, avoids electrolyte from deteriorating, improves the safety of electrolyte.
Preferably, polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, Perhydropolysilazane, porous in step (1)
Inorganic matter, ammonium hydroxide mass ratio be 100:15-25:2-5:8-15:10-20:30-60.Ammonium hydroxide selects the ammonia of commercially available 20wt%
Water.
Preferably, the dispersing agent is 12- hydroxy stearic acid.
Preferably, it in airflow mixer described in step (2), is mixed using compressed air, the pressure of compressed air
For 0.8-1.5MPa, 4-8min is mixed.
Preferably, in step (2), cladded type composite particles, dispersing agent mass ratio be 100:1-3.
A kind of lithium battery semisolid electrolyte being prepared the present invention also provides a kind of above-mentioned preparation method is dedicated solidifying
Jelly, the gelling agent are that polymeric matrix and hydroxypropyl methyl cellulose, fire retardant mixed grinding are first obtained composite particles,
Then it is sprayed after mixing Perhydropolysilazane, porous mineral with ammonium hydroxide on composite particles surface, finally by obtained cladded type
Composite particles and dispersing agent are completely dispersed using airflow mixer and are made.
Further, the present invention passes through polymeric matrix is micro- for nanoscale with hydroxypropyl methyl cellulose freeze grinding
Grain, the property of silica mocromembrane is hydrolyzed to using Perhydropolysilazane in ammonia-water systems, and porous mineral is adhered to and is coated
On composite particles surface, the composite particles are as gelling agent in use, directly addition in the electrolytic solution, has excellent particle point
Property is dissipated, but not forms gel, fluid injection can be carried out in a manner of the fluid injection of traditional electrolyte, there is excellent mobility, Neng Gouchong
Sub-dip moistens electrode, diaphragm；After fluid injection, gelling agent surface coating layer has inorganic microporous, when heating chemical conversion, the solvent of electrolyte
It is slowly immersed in gelling agent, polymeric matrix material and inorganic microporous material form gel frame, be conducive to lithium salts in electrolyte
The quick transmitting of dissociation and lithium ion.
Existing lithium battery gel electrolyte infiltrates insufficient defect there are inconvenient for use, with diaphragm, electrode, and will fill
It reacts to form the complex of gel process again after gel-filled electrolyte perfusion, limit its application.In consideration of it, the present invention proposes
A kind of lithium battery semisolid electrolyte special gel agent and preparation method, by polymeric matrix and hydroxypropyl methyl cellulose, resistance
It fires agent and obtains composite particles in freeze grinding, then disperse ammonium hydroxide for Perhydropolysilazane, porous mineral, pass through high pressure mist
Change equipment to spray on composite particles surface, it is dry, obtain cladded type composite particles；By cladded type composite particles and dispersant
Uniformly, through airflow mixer, dispersed by air blast and hit, be completely dispersed composite particles, lithium battery semisolid electricity is made
Solve the agent of matter special gel.Special gel agent addition provided by the invention will not generate gel at the initial stage of electrolyte, greatly improve
Be difficult to the defect used uniformly be perfused after existing Electrolyte Gelization processing, and be perfused chemical conversion can substantially uniformity infiltrate diaphragm with
Electrode, increases electrolyte toughness, is changed into gel state by liquid, improves the safety of electrolyte.
The present invention proposes a kind of lithium battery semisolid electrolyte special gel agent and preparation method, compared with prior art,
Its feature protruded and excellent effect are:
1, for the present invention by preparing special gel agent, gelling agent addition will not generate gel at the initial stage of electrolyte, substantially change
After being apt to existing Electrolyte Gelization processing it is difficult to that the defect used is uniformly perfused.Greatly facilitate use.
2, special gel agent produced by the present invention be added electrolyte perfusion chemical conversion can substantially uniformity infiltration diaphragm and electrode,
Electrolyte toughness is increased, gel state is changed by liquid, improves the safety of electrolyte.Hydroxypropyl methyl therein is fine
Dimension element not only assists gel-forming, and when electrolyte generates water, it is prone to aquation, so that fixed water, avoids electricity
Solve liquid deterioration.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；Polymeric matrix is poly- first
Base methacrylate；Fire retardant is polyphosphazene；Porous mineral is nanoscale zeolite arogel；The pressure of high-pressure atomization is
220bar, mist flow 2.3L/min；Wherein, the poly- silicon nitrogen of polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, perhydro
Alkane, porous mineral, ammonium hydroxide mass ratio be 100:19:3:11:16:50；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent；Dispersing agent is 12- hydroxyl
Stearic acid；It in airflow mixer, is mixed using compressed air, the pressure of compressed air is 1.3MPa, mixes 6min；Its
In, cladded type composite particles, dispersing agent mass ratio be 100:2.5.
Test method:
The special gel agent that the present embodiment prepares is tested for the property, first at room temperature by gelling agent according to mass ratio
It is uniformly dispersed in the EC/DMC/EMC electrolyte of the 5% commercially available LiPF6 (1M) of addition, is electrolysed after standing 60min using viscosimeter test
The viscosity of liquid, then as 60min in 100 DEG C of water-bath, simulation chemical conversion temperature, so that Electrolyte Gel, test is electric again
The viscosity for solving liquid, obtains that the results are shown in Table 1.
Embodiment 2
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；Polymeric matrix is polyoxy
Change ethylene；Fire retardant is polyphosphazene；Porous mineral is alumina in Nano level aeroge；The pressure of high-pressure atomization is 10bar, spray
Spray amount is 1.2L/min；Wherein, polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, Perhydropolysilazane, porous nothing
Machine object, ammonium hydroxide mass ratio be 100:15:2:8:10:30；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent；Dispersing agent is 12- hydroxyl
Stearic acid；It in airflow mixer, is mixed using compressed air, the pressure of compressed air is 0.8MPa, mixes 8min；Its
In, cladded type composite particles, dispersing agent mass ratio be 100:1.
It is tested using the method for embodiment 1, test result is as shown in table 1.
Embodiment 3
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；Polymeric matrix is polyamides
Amine；Fire retardant is polyphosphazene；Porous mineral is nanoscale silica aerogel；The pressure of high-pressure atomization is 30bar, spraying
Flow is 3L/min；Wherein, polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, Perhydropolysilazane, porous mineral,
The mass ratio of ammonium hydroxide is 100:25:5:15:20:60；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent；Dispersing agent is 12- hydroxyl
Stearic acid；It in airflow mixer, is mixed using compressed air, the pressure of compressed air is 1.5MPa, mixes 8min；Its
In, cladded type composite particles, dispersing agent mass ratio be 100:3.
It is tested using the method for embodiment 1, test result is as shown in table 1.
Embodiment 4
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；Polymeric matrix is poly- third
Alkene nitrile；Fire retardant is polyphosphazene；Porous mineral is nanoscale zeolite powder；The pressure of high-pressure atomization is 20bar, mist flow
For 2L/min；Wherein, polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, Perhydropolysilazane, porous mineral, ammonium hydroxide
Mass ratio be 100:20:4:12:15:45；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent；Dispersing agent is 12- hydroxyl
Stearic acid；It in airflow mixer, is mixed using compressed air, the pressure of compressed air is 1.2MPa, mixes 6min；Its
In, cladded type composite particles, dispersing agent mass ratio be 100:2.
It is tested using the method for embodiment 1, test result is as shown in table 1.
Comparative example 1
Comparative example 1 compared with Example 1, is not used Perhydropolysilazane and protects composite particles, special gel agent obtained is adding
It can be thickened in a short time after entering electrolyte, influence the perfusion of electrolyte.It is tested, is tested using the method for embodiment 1
The results are shown in Table 1.
Table 1:
Claims (10)
1. a kind of preparation method of lithium battery semisolid electrolyte special gel agent, which is characterized in that it is specific the preparation method is as follows:
(1) freeze grinding after mixing polymeric matrix with hydroxypropyl methyl cellulose, fire retardant obtains partial size at 10 μm or less
Composite particles, then Perhydropolysilazane, porous mineral are dispersed in ammonium hydroxide, then lead to obtained dispersion liquid
It crosses high pressure atomization plant to spray in composite particles surface, finally dry, obtain cladded type composite particles；
(2) cladded type composite particles and dispersant are uniform, then be added airflow mixer in, by air blast dispersion and
It hits, is completely dispersed composite particles, discharge to get lithium battery semisolid electrolyte special gel agent.
2. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In the polymeric matrix is one or both of polymethyl methacrylate, polyethylene glycol oxide, polyamide, polyacrylonitrile
Above combination.
3. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In the fire retardant is polyphosphazene.
4. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In the porous mineral is the one or more of nanoscale zeolite powder, alumina aerogels, silica aerogel
Combination.
5. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In the pressure of high-pressure atomization described in step (1) is 10-30bar, mist flow 1.2-3L/min.
6. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In, in step (1), polymeric matrix, hydroxypropyl methyl cellulose, fire retardant, Perhydropolysilazane, porous mineral, ammonium hydroxide
Mass ratio be 100:15-25:2-5:8-15:10-20:30-60.
7. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In the dispersing agent is 12- hydroxy stearic acid.
8. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In, in airflow mixer described in step (2), being mixed using compressed air, the pressure of compressed air is 0.8-1.5MPa,
Mix 4-8min.
9. a kind of preparation method of lithium battery semisolid electrolyte special gel agent according to claim 1, feature exist
In, in step (2), cladded type composite particles, dispersing agent mass ratio be 100:1-3.
10. a kind of lithium battery semisolid electrolyte that the preparation method as described in claim 1-9 any claim is prepared is dedicated
Gelling agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110854428A (en) * | 2019-11-28 | 2020-02-28 | 成都新柯力化工科技有限公司 | Semi-solid lithium battery electrolyte and preparation method thereof |
| CN113346128A (en) * | 2020-07-30 | 2021-09-03 | 道克特斯(天津)新能源科技有限公司 | Semi-solid/solid battery prepared by electrochemical oxidation-reduction method and method |
| WO2022052425A1 (en) | 2020-09-09 | 2022-03-17 | 蜂巢能源科技股份有限公司 | Electrolyte material, preparation method therefor and use thereof |
-
2019
- 2019-06-21 CN CN201910539993.2A patent/CN110265715A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110854428A (en) * | 2019-11-28 | 2020-02-28 | 成都新柯力化工科技有限公司 | Semi-solid lithium battery electrolyte and preparation method thereof |
| CN113346128A (en) * | 2020-07-30 | 2021-09-03 | 道克特斯(天津)新能源科技有限公司 | Semi-solid/solid battery prepared by electrochemical oxidation-reduction method and method |
| WO2022052425A1 (en) | 2020-09-09 | 2022-03-17 | 蜂巢能源科技股份有限公司 | Electrolyte material, preparation method therefor and use thereof |
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