CN109568869A - A kind of insulated type flame-retarding fire-extinguishing material and preparation method thereof - Google Patents
A kind of insulated type flame-retarding fire-extinguishing material and preparation method thereof Download PDFInfo
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- CN109568869A CN109568869A CN201810935026.3A CN201810935026A CN109568869A CN 109568869 A CN109568869 A CN 109568869A CN 201810935026 A CN201810935026 A CN 201810935026A CN 109568869 A CN109568869 A CN 109568869A
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0007—Solid extinguishing substances
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0064—Gels; Film-forming compositions
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/06—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires containing gas-producing, chemically-reactive components
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Abstract
The invention discloses a kind of insulated type flame-retarding fire-extinguishing material and preparation method thereof, include the following steps: to prepare PEO (polyethylene glycol oxide) base extinguishment additive agent；By the product filtration treatment of step 1), unreacted silane coupling agent is disposed, is reacted under the protection of nitrogen after leaving the silane coupled object of product PEG- with nano silica hydrosol, reaction product centrifugal treating；It is fabricated to mixture paste；Frozen drying processing, followed by break process are screened at granular material, the granular size by sieve pore；Ac impedance measurement, tensile property test, vertical burn test, limit oxygen index test are carried out respectively, obtain boundary's test structure；Product passes through electron microscope observation result situation, and product reaction uniformity is fine, and dispersibility and mobility all reach standard, and reaction effect is ideal.
Description
Technical field
The present invention relates to the invention belongs to field of new materials, and in particular to a kind of insulated type flame-retarding fire-extinguishing material and its preparation
Method.
Background technique
Currently on the market, common extinguishing chemical has dry powder fire extinguishing agent, foaming extinguishing chemical and aqua extinguishing chemical, and point is to inhale
Heat, cooling, closing fire source and starvation, based on physics extinguishing method, the disadvantage is that blow-off velocity rate is low, and aqua goes out
Fiery process is also easy to produce water-gas explosion at high temperature, to easily cause major accident.In addition the tree with flame retardant property used
Rouge or addition fire retardant, have cooperated the material of fire retardant in burning, the toxic and harmful gas and cigarette of generation in actual use
Dirt greatly affected people flee from, succour, the measures such as fire-fighting.
Therefore, a kind of highly efficient fire extinguishing, fire extinguishing material utensil safe and reliable simultaneously, are forced to be essential in fire-fighting domain
It asks.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of insulated type flame-retarding fire-extinguishing materials and preparation method thereof, effectively mention
Rise safety of the fire extinguishing appliance in use process, high efficiency.(fire extinguishing material contains apparatus)
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of insulated type flame-retarding fire-extinguishing material and its
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, is fabricated to mixture paste；
4) slurry obtained by step 3) and polymer precursor material are mixed evenly by mass fraction ratio；
5) product is put on a workstation, and step 4) product is subjected to fast low temperature freeze-drying process, followed by
Break process is screened at granular material, the granular size by sieve pore.
6) by step 3) products obtained therefrom, ac impedance measurement, tensile property test, vertical burn test, pole are carried out respectively
Limited oxygen index test obtains boundary's test structure；Product passes through electron microscope observation result situation, and product reacts uniformity very
Good, dispersibility and mobility all reach standard, and 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).
As an improvement slot size is 1000 mesh in the step 5).
It is had received widespread attention in recent years using gel derived fire extinguishing material, silica gel is that one kind has in conjunction with potassium carbonate
The fire retardant of fire protecting performance is widely used in various Common Polymers (mass fraction be only total additive 10%), and such as poly- third
Alkene, nylon, polymethyl methacrylate, polyvinyl alcohol, cellulose and a small amount of polystyrene and styrene-acrylonitrile,
In combustion process, its advantage is that water absorption is big, the water conservation time is long, Fire resistances are high, adhesive force is strong, gel fire retardant, not
In the case where dramatically increasing smog or carbon monoxide content, highest release heat reduces 60%.Mostly at 200 DEG C~300 DEG C
Lower decomposition delays or terminates the chain reaction burnt by capturing the free radical of Degradation of Polymer Materials reaction when decomposition, play resistance
Every the effect of surface flammable explosive gas, the scene of a fire can not only be made to cool down rapidly, can also body surface formed gel overlay layer every
Exhausted air inhibits toxic and harmful gas diffusion, and cooling object consumes big calorimetric, to reach control fire spread and quickly have
Imitate the purpose of fire extinguishing.Therefore we have invented gel fire-retardant film fire extinguishing materials.
The invention is prepared using gel fire-retardant film, prepares film, fire-retardant machine with polymer gel film
Reason is the fracture of polymer high temperature segment, generates PO free radical, it is free that PO free radical can capture H free radical and OH in High Temperature Gas compound
Base forms very stable carbide on the surface of high molecular material, so that material be made to have completely cut off oxygen, and then plays fire-retardant work
With battery without gas evolution in storage and discharge process, safety is good, and fire extinguishing material is made and is with a wide range of applications, has
There is very huge socioeconomic value.
The technical solution adopted by the present invention, the beneficial effect is that: fire extinguishing material prepared by the invention this method
Have following performance: 1, flame retardant type gel film material not only has good flame retardant effect, but also greatly improves its extinguishing property；
2, the satisfactory mechanical property of the film facilitates storage to transport；3, the gel film also has good chemical property, can make battery
Security performance greatly improve.
Detailed description of the invention:
Fig. 1 electrochemical impedance test chart；
Fig. 2 limit oxygen index comparison diagram.
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 insulated type flame-retarding fire-extinguishing material and preparation method thereof, this method includes following step
It is rapid:
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 such as Fig. 1 and Fig. 2；
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:
It is put out a fire using novel methyl-phosphoric acid dimethyl ester film, this method comprises:
1) according to the ratio precise methyl-phosphoric acid dimethyl ester and PPG of mass ratio 2:1, chloroform is used to dissolve first as solvent
Simultaneously proper catalyst is added in base dimethyl phosphate and PPG, reacts under the protection of nitrogen after the two mixing, chloroform and methyl acid phosphate
Dimethyl ester and PPG three's mass ratio are 10:2:1.The product of previous step is mixed with PEG, proper catalyst is added in nitrogen
Protection under react.Finally the PEG of the product of previous step and silanization is reacted, acquired solution is poured on Teflon mould
On, fast freezing low-temperature treatment, followed by break process are carried out, screening sieve leakage controls granular size size, symbol can be obtained
Close desired gel smother material.
2) performance test: product is placed on the test of the combustion characteristics such as work station enterprising limit by row oxygen index (OI), tensile property is surveyed
Examination, limit oxygen index and excellent fireproof performance, especially mechanical performance is good, is a kind of good fire extinguishing filler material.
Embodiment three:
With embodiment one, two the difference is that: select physical doping methyl-phosphoric acid dimethyl ester extinguishment additive agent for, should
Method includes:
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, be rapidly frozen at low temperature
Reason, followed by break process, screening sieve leakage, control granular size size, satisfactory physical doping methyl can be obtained
Dimethyl phosphate film fire extinguishing material.
2) combustion testing, tensile property test, limit oxygen index test performance test: are carried out.
In above-mentioned each group embodiment, it is successfully prepared polyethylene glycol groups fire extinguishing material, the fire extinguishing of novel methyl-phosphoric acid dimethyl ester
Material possesses good mechanical performance and safety, and can apply to physical doping methyl-phosphoric acid dimethyl ester fire extinguishing material
Lithium battery.Interface impedance test is carried out with physical doping methyl-phosphoric acid dimethyl ester fire extinguishing material and tensile property test burning is surveyed
Examination, the results showed that the methyl-phosphoric acid dimethyl ester film fire extinguishing material combustion time is short, good mechanical property, and electrochemical impedance is good.
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 (4)
1. a kind of insulated type flame-retarding fire-extinguishing material and preparation method thereof, characterized by the following steps: 1), prepare PEO
(polyethylene glycol oxide) base extinguishment additive agent: described according to mass ratio precise PEG (polyethylene glycol) and silane coupling agent
The mass ratio of PEG and silane coupling agent be 5:1, use mass concentration be 20% THF (tetrahydrofuran) as solvent dissolve PEG with
Silane coupling agent is reacted under the protection of nitrogen after the two mixing, is reacted 4 hours in a kettle, and stirring good fortune mixing speed is
70 revs/min, the reaction time 4 hours, reaction temperature was controlled at 60 degrees Celsius；2), by the product filtration treatment of step 1), not
The silane coupling agent of reaction is disposed, leave after the silane coupled object of product PEG- and nano silica hydrosol nitrogen guarantor
The lower reaction of shield, reaction product centrifugal treating；3), step 2) products obtained therefrom and polypropylene glycol are reacted, the two is stirred in a kettle
Reaction 2 hours is mixed, the stirring good fortune mixing speed is 70 revs/min, is fabricated to mixture paste；4) it, will be starched obtained by step 3)
Material and polymer precursor material are mixed evenly by mass fraction ratio；5), product is put on a workstation, and step 4) is produced
Object carries out fast low temperature freeze-drying process, and followed by break process passes through sieve pore at granular material, the granular size
Screening；6), by step 3) products obtained therefrom, ac impedance measurement, tensile property test, vertical burn test, the limit are carried out respectively
Oxygen index (OI) test obtains boundary's test structure；Product passes through electron microscope observation result situation, and product reaction uniformity is fine,
Dispersibility and mobility all reach standard, and reaction effect is ideal.
2. a kind of insulated type flame-retarding fire-extinguishing material according to claim 1 and preparation method thereof, it is characterised in that: the step
It is rapid 2) in after the silane coupled object of PEG- and the liquid volume ratio of nano silica hydrosol is 20:1.
3. a kind of insulated type flame-retarding fire-extinguishing material according to claim 1 and preparation method thereof, it is characterised in that: the step
It is rapid 5) in by product be placed on work station main device be Teflon mould.
4. a kind of insulated type flame-retarding fire-extinguishing material according to claim 1 and preparation method thereof, it is characterised in that: the step
It is rapid 5) in slot size be 1000 mesh.
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| CN201810935026.3A CN109568869A (en) | 2018-08-16 | 2018-08-16 | A kind of insulated type flame-retarding fire-extinguishing material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220387837A1 (en) * | 2021-06-03 | 2022-12-08 | Huazhong University Of Science And Technology | Method for preparing non-corrosive fire extinguishing agent |
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| CN103897122A (en) * | 2012-12-28 | 2014-07-02 | 青岛鑫垚保水高新材料有限公司 | Method for preparing super absorbent polymer (potassium chloride) fire extinguishing agent |
| 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 |
| CN108054405A (en) * | 2017-11-10 | 2018-05-18 | 江汉大学 | Solid electrolyte and preparation method thereof and the one-shot battery based on the solid electrolyte |
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2018
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| CN1736516A (en) * | 2005-09-12 | 2006-02-22 | 福建师范大学 | Method for preparing compound fire-extinguishing particulate material |
| CN103897122A (en) * | 2012-12-28 | 2014-07-02 | 青岛鑫垚保水高新材料有限公司 | Method for preparing super absorbent polymer (potassium chloride) fire extinguishing agent |
| CN108054405A (en) * | 2017-11-10 | 2018-05-18 | 江汉大学 | Solid electrolyte and preparation method thereof and the one-shot battery based on the solid electrolyte |
| 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 (4)
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| H.F.XIANG ET AL: "Dimethyl methylphosphonate (DMMP) as an efficient flame retardant additive for the lithium-ion battery electrolytes", 《JOURNAL OF POWER SOURCES》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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