CN109054866A - A kind of lithium battery fire extinguishing packing material addictive preparation method - Google Patents
A kind of lithium battery fire extinguishing packing material addictive preparation method Download PDFInfo
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- CN109054866A CN109054866A CN201810779839.8A CN201810779839A CN109054866A CN 109054866 A CN109054866 A CN 109054866A CN 201810779839 A CN201810779839 A CN 201810779839A CN 109054866 A CN109054866 A CN 109054866A
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- product
- peg
- lithium battery
- packing material
- fire
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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 discloses a kind of lithium battery fire extinguishing packing material addictive preparation methods; the preparation of PEO base extinguishment additive agent: according to the ratio precise PEG and silane coupling agent of mass ratio 5:1; it uses appropriate THF to dissolve PEG and silane coupling agent as solvent, is reacted under the protection of nitrogen after the two mixing.It will be reacted under the protection of nitrogen after the product filtration treatment of previous step with nano silica hydrosol, reaction product centrifugal treating.Finally the product of previous step and PPG are reacted.Product finds out that product reaction uniformity is fine by electron microscope observation result, and dispersibility and mobility all reach standard.This novel high fire-retardance extinguishment additive agent is readily synthesized, and easy to use, low waste provides better choice for toxic halogen fire retardant.
Description
Technical field
The present invention relates to the invention belongs to field of new materials, and in particular to a kind of lithium battery fire extinguishing packing material additive system
Preparation Method.
Background technique
Lithium battery can spontaneous combustion, can then explode because of overheat.The reason of generating overheat includes electric short circuit, quickly
Electric discharge, overcharges, manufacturing defect, designs bad or mechanical failure etc..Overheat will lead to " thermal runaway " and process generation,
Be exactly inside battery exothermic reaction will lead to internal temperature of battery and pressure with rate quickly rising, thus by energy dissipation
Fall.
Once some battery unit enters thermal runaway state, it can generate enough heats, so that adjacent battery unit
Also enter thermal runaway state.As each battery unit ruptures in turn and discharge its content, one kind will be generated and burnt repeatedly
Flame.This results in the flammable electrolyte in battery and leaks, if can also discharge can using disposable lithium cell
The lithium metal of burning.Then will lead to the problem of one it is huge, these fire cannot be treated as " normal " fire, be needed
Carry out targetedly training, prevention and control planning rationally stores and establish fire extinguishing system etc..These reality there are the problem of, it is potential
Risk needs to reduce or avoid as far as possible, gives effectively to solve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithium battery fire extinguishing packing material addictive preparation methods, effectively
Lithium ion battery is promoted in the safety of use process.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of lithium battery fire extinguishing packing material addition
Agent preparation method, includes the following steps:
1) prepare PEO (polyethylene glycol oxide) base extinguishment additive agent: according to mass ratio precise PEG (polyethylene glycol) and
The mass ratio of silane coupling agent, the PEG and silane coupling agent is 5:1, is made with the THF (tetrahydrofuran) that mass concentration is 20%
PEG and silane coupling agent are dissolved for solvent, is reacted under the protection of nitrogen after the two mixing, is reacted 4 hours, stir in a kettle
Mixing good fortune mixing speed is 70 revs/min, and the reaction time 4 hours, reaction temperature was controlled at 60 degrees Celsius；
2) by the product filtration treatment of step 1), unreacted silane coupling agent is disposed, leaves product PEG- silane
It is reacted under the protection of nitrogen after conjugate with nano silica hydrosol, reaction product centrifugal treating；
3) step 2) products obtained therefrom and polypropylene glycol are reacted, the two is stirred to react 2 hours in a kettle, the stirring
Good fortune mixing speed is 70 revs/min；
4) step 3) acquired solution and methyl-phosphoric acid dimethyl ester are mixed evenly by 25% mass fraction ratio；
5) product performance test: is placed on progress ac impedance measurement, vertical burn test, limit oxygen index on work station
Test obtains boundary's test structure；
6) product passes through electron microscope observation result situation, and product reaction uniformity is fine, and dispersibility and mobility are all
Reach standard, reaction effect is ideal.
As an improvement in the step 2) after the silane coupled object of PEG- and the liquid bulk of nano silica hydrosol
Product is than being 20:1.
As an improvement it is Teflon mould that product, which is placed on work station main device, in the step 5).
Being prepared using phosphoric acid ester extinguishment additive agent can be such that full property greatly improves, no leakage, high-flexibility, high physics
Chemical stability, can be with large-scale popularization application；Cell safety is reliable: making polymer while not influencing mechanical properties of polymer
With fire retardation, fire-retardant mechanism is segment fracture after polymer combustion, generates PO free radical, PO free radical can capture H
Free radical and OH free radical form very stable carbide on the surface of high molecular material, so that material is made to have completely cut off oxygen, into
And fire-retardant action battery is played in storage and discharge process without gas evolution, safety is good；This novel high fire-retardance fire extinguishing
Additive is readily synthesized, easy to use, low waste, provides better choice for toxic halogen fire retardant.
The technical solution adopted by the present invention, the beneficial effect is that: lithium-ion electric prepared by the invention this method
Pond can effectively solve the safety problem of battery, excellent in view of its efficient anti-flammability and excellent thermal stability and low pollution etc.
Point, small molecule phosphate compounds can be used as flame retardant for Li-ion battery, and the phosphate of macromolecular is in lithium ion battery
Fire-retardant aspect also has preferable application, is with a wide range of applications in lithium-ion energy storage battery flame-retarding fire-extinguishing field.
Detailed description of the invention:
Fig. 1 is additive infrared test figure.
Specific embodiment
Embodiment one:
By taking the full extinguishment additive agent of PEO base as an example:
The embodiment of the invention provides a kind of lithium battery fire extinguishing packing material addictive preparation method, this method includes as follows
Step:
1) prepare PEO (polyethylene glycol oxide) base extinguishment additive agent: according to mass ratio precise PEG (polyethylene glycol) and
The mass ratio of silane coupling agent, the PEG and silane coupling agent is 5:1, is made with the THF (tetrahydrofuran) that mass concentration is 20%
PEG and silane coupling agent are dissolved for solvent, is reacted under the protection of nitrogen after the two mixing, is reacted 4 hours, stir in a kettle
Mixing good fortune mixing speed is 70 revs/min, and the reaction time 4 hours, reaction temperature was controlled at 60 degrees Celsius.
2) by the product filtration treatment of step 1), unreacted silane coupling agent is disposed, leaves product PEG- silane
It is reacted under the protection of nitrogen after conjugate with nano silica hydrosol, reaction product centrifugal treating.
3) step 2) products obtained therefrom and polypropylene glycol are reacted, the two is stirred to react 2 hours in a kettle, the stirring
Good fortune mixing speed is 70 revs/min；
4) step 3) acquired solution and methyl-phosphoric acid dimethyl ester are mixed evenly by 25% mass fraction ratio；
5) product performance test: is placed on progress ac impedance measurement, vertical burn test, limit oxygen index on work station
Test obtains boundary's test structure；
6) product passes through electron microscope observation result situation, and product reaction uniformity is fine, and dispersibility and mobility are all
Reach standard, reaction effect is ideal.
It is summarized as the preparation of PEO base extinguishment additive agent: according to the ratio precise PEG of mass ratio 5:1 and silane coupled
Agent is used appropriate THF to dissolve PEG and silane coupling agent as solvent, is reacted under the protection of nitrogen after the two mixing.By previous step
Product filtration treatment after and nano silica hydrosol reacted under the protection of nitrogen, reaction product centrifugal treating.Finally
The product of previous step and PPG are reacted.Product finds out that product reaction uniformity is fine by electron microscope observation result, point
It dissipates property and mobility all reaches standard.
Performance test: product is placed on work station and is tested.
Embodiment two:
With embodiment one the difference is that: select physical doping methyl-phosphoric acid dimethyl ester extinguishment additive agent for this method
Include:
1) according to the ratio precise PEG and silane coupling agent of mass ratio 5:1, appropriate THF is used to dissolve PEG as solvent
And silane coupling agent, it is reacted under the protection of nitrogen after the two mixing.It will be after the product filtration treatment of previous step and nano-silica
The SiClx hydrosol reacts under the protection of nitrogen, reaction product centrifugal treating.Finally the product of previous step and PPG are reacted, it will
Acquired solution is mixed evenly with methyl-phosphoric acid dimethyl ester (25%), is poured on PTFE mold, and physical doping first can be obtained
Base dimethyl phosphate polymer dielectric.
2) product performance test: is placed on progress characteristic infrared absorption test, the result is shown in Figure 1 on work station, it can be seen that
The characteristic infrared absorption peak of methyl-phosphoric acid dimethyl ester is obvious, such as has apparent absorption peak 1006,734 etc..
Embodiment three:
With embodiment one, two the difference is that:
Using novel methyl-phosphoric acid dimethyl ester extinguishment additive agent, this method comprises:
1) according to the ratio precise methyl-phosphoric acid dimethyl ester and PPG of mass ratio 2:1, use appropriate chloroform molten as solvent
Simultaneously proper catalyst is added in solution methyl-phosphoric acid dimethyl ester and PPG, reacts under the protection of nitrogen after the two mixing.By previous step
Product is mixed with PEG, and proper catalyst is added and reacts under the protection of nitrogen.Finally by the product of previous step and silanization
PEG reaction, acquired solution is poured on PTFE mold, phosphate composite electrolyte can be obtained.
2) performance test: being placed on the test of the combustion characteristics such as work station enterprising limit by row oxygen index (OI) for product, the results are shown in Table 1,
As can be seen that the limit oxygen index and excellent fireproof performance of methyl-phosphoric acid dimethyl ester, are a kind of good fire extinguishing filler materials.
The limit oxygen index comparison diagram of the different flame-retardant additives of table 1
In addition to above preferred embodiment, there are other embodiments of the invention, and those skilled in the art can be according to this
Various changes and variants are made in invention, and as long as it does not depart from the spirit of the invention, should belong to appended claims of the present invention and determines
The range of justice.
Claims (3)
- The packing material addictive preparation method 1. a kind of lithium battery is put out a fire, include the following steps: 1), preparation PEO (polyoxyethylene Alkene) base extinguishment additive agent: according to mass ratio precise PEG (polyethylene glycol) and silane coupling agent, the PEG and silane are even The mass ratio for joining agent is 5:1, and the THF (tetrahydrofuran) that mass concentration is 20% is used to dissolve PEG and silane coupling agent as solvent, It reacts under the protection of nitrogen after the two mixing, reacts 4 hours in a kettle, stirring good fortune mixing speed is 70 revs/min, instead 4 hours between seasonable, reaction temperature is controlled at 60 degrees Celsius；2), by the product filtration treatment of step 1), unreacted silane is even Connection agent is disposed, and is reacted under the protection of nitrogen after leaving the silane coupled object of product PEG- with nano silica hydrosol, instead Answer product centrifugal treating；3), step 2) products obtained therefrom and polypropylene glycol to be reacted, the two is stirred to react 2 hours in a kettle, The stirring good fortune mixing speed is 70 revs/min；4), step 3) acquired solution and methyl-phosphoric acid dimethyl ester are pressed to 25% quality Score ratio is mixed evenly；5), performance test: product is placed on work station and carries out ac impedance measurement, vertical combustion is surveyed Examination, limit oxygen index test obtain boundary's test structure；6), product passes through electron microscope observation result situation, and product reaction is equal Even property is fine, and dispersibility and mobility all reach standard, and reaction effect is ideal.
- The packing material addictive preparation method 2. a kind of lithium battery according to claim 1 is put out a fire, it is characterised in that: described In step 2) after the silane coupled object of PEG- and the liquid volume ratio of nano silica hydrosol be 20:1.
- The packing material addictive preparation method 3. a kind of lithium battery according to claim 1 is put out a fire, it is characterised in that: described It is Teflon mould that product, which is placed on work station main device, in step 5).
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| CN201810779839.8A CN109054866A (en) | 2018-07-16 | 2018-07-16 | A kind of lithium battery fire extinguishing packing material addictive preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115335125A (en) * | 2020-01-22 | 2022-11-11 | 雅托普罗德克株式会社 | Fire extinguishing sheet |
| US20220387837A1 (en) * | 2021-06-03 | 2022-12-08 | Huazhong University Of Science And Technology | Method for preparing non-corrosive fire extinguishing agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450394A (en) * | 2016-11-24 | 2017-02-22 | 东莞理工学院 | PVDF-PEO solid composite polymer electrolyte and preparation method thereof |
| CN107863555A (en) * | 2017-10-31 | 2018-03-30 | 江汉大学 | A kind of fire-retardant type solid polymer electrolyte and its application in solid secondary batteries |
| CN107910481A (en) * | 2017-12-06 | 2018-04-13 | 江汉大学 | A kind of preparation method of PEO based polyalcohols membrane and its preparation method of one-shot battery |
-
2018
- 2018-07-16 CN CN201810779839.8A patent/CN109054866A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450394A (en) * | 2016-11-24 | 2017-02-22 | 东莞理工学院 | PVDF-PEO solid composite polymer electrolyte and preparation method thereof |
| CN107863555A (en) * | 2017-10-31 | 2018-03-30 | 江汉大学 | A kind of fire-retardant type solid polymer electrolyte and its application in solid secondary batteries |
| CN107910481A (en) * | 2017-12-06 | 2018-04-13 | 江汉大学 | A kind of preparation method of PEO based polyalcohols membrane and its preparation method of one-shot battery |
Non-Patent Citations (1)
| Title |
|---|
| H.F. XIANG ET AL.,: "Dimethyl methylphosphonate (DMMP) as an efficient flame", 《JOURNAL OF POWER SOURCES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115335125A (en) * | 2020-01-22 | 2022-11-11 | 雅托普罗德克株式会社 | Fire extinguishing sheet |
| US20220387837A1 (en) * | 2021-06-03 | 2022-12-08 | Huazhong University Of Science And Technology | Method for preparing non-corrosive fire extinguishing agent |
| US11617909B2 (en) * | 2021-06-03 | 2023-04-04 | Huazhong University Of Science And Technology | Method for preparing non-corrosive fire extinguishing agent |
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Application publication date: 20181221 |