CN108841229A - A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof - Google Patents

A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof Download PDF

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Publication number
CN108841229A
CN108841229A CN201810760474.4A CN201810760474A CN108841229A CN 108841229 A CN108841229 A CN 108841229A CN 201810760474 A CN201810760474 A CN 201810760474A CN 108841229 A CN108841229 A CN 108841229A
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parts
graphene
water
fireproof coating
type low
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车春玲
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Shandong Jiaxing Environmental Protection Technology Co Ltd
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Shandong Jiaxing Environmental Protection Technology Co Ltd
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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
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C09D5/185—Intumescent paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Fireproofing Substances (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to a kind of graphene expansion type low-smoke fireproof coating, are made of the raw material of following weight parts：200-300 parts of water-base resin, 150-250 parts of 2 chloroethyl phosphoric acid ester, 20-30 parts of fluorinated graphene, 10-15 parts of graphene oxide, 20-40 parts of carbon fiber powder, 10-15 parts of boric acid melamine, 3-5 parts of dipentaerythritol, 1-2 parts of alkali formula copper molybdate, 5-15 parts of perlite, 3-5 parts of octamethylcy-clotetrasiloxane, 3-5 parts of alkyl phenol polyoxyethylene ether, 1-2 parts of foaming agent, 250-400 parts of water.Fireproof coating prepared by the present invention can improve the intensity of charring layer, improve fire resistance；Graphene and carbon fiber can cooperate with the generation for inhibiting volatile degradation products, form a kind of reticular structure that efficient anti-seepage is saturating, resist the release for decomposing the pernicious gas generated.

Description

A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof
Technical field
The invention belongs to technical field of coatings, and in particular to a kind of graphene expansion type low-smoke fireproof coating and its preparation Method.
Background technique
It is organic that traditional fireproof coating is mainly based upon macromolecule matrix, including propylene acid esters, epoxy resin, esters of silicon acis etc. Resin.And their main application technology is spraying, brushing, roller coating etc., another method is exactly that material surface is directly soaked Stain in coating, make its infiltrate through in material achieve the effect that it is fire-retardant.However these technologies are there are problems, for example method It is too cumbersome, serious pollution, and duplicate brushing are caused to environment, the adhesion strength that will cause between coating is not strong, is easy de- The problem of falling.
Expanding fire-proof paint is made of matrix, flame-retardant system, additive and various auxiliary agents.In the effect of thermal-flame Under, dope layer melting, foaming, expansion form cellular bag-like charring layer structure, and release fire retardant gas, play fire insulation Heat-insulated effect.At present there is charring layer intensity difference mostly, be easy to fall off from substrate surface in expanding fire-proof paint.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene expansion type low-smoke fireproof coating and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is：A kind of graphene expansion type low-smoke fireproof painting Material, is made of the raw material of following weight parts：
200-300 parts of water-base resin,
150-250 parts of 2 chloroethyl phosphoric acid ester,
20-30 parts of fluorinated graphene,
10-15 parts of graphene oxide,
20-40 parts of carbon fiber powder,
10-15 parts of boric acid melamine,
3-5 parts of dipentaerythritol,
1-2 parts of alkali formula copper molybdate,
5-15 parts of perlite,
3-5 parts of octamethylcy-clotetrasiloxane,
3-5 parts of alkyl phenol polyoxyethylene ether,
1-2 parts of foaming agent,
250-400 parts of water.
Specifically, the preparation method of the fluorinated graphene is as follows：It adds graphene oxide into deionized water, at ultrasound Reason 2-3h obtains graphene oxide water solution；Graphene oxide water solution is added in the water heating kettle with polytetrafluoroethyllining lining, so After fluorization agent is added, 100-200 DEG C of reaction 20-25h is cooled to room temperature after reaction, filtering, filter cake is washed with deionized water To neutrality, dry to get fluorinated graphene.
Specifically, the water-base resin is one of aqueous polyurethane, aqueous epoxy resins or water-based acrylic resin.
Specifically, the foaming agent is double cyanogen ammoniums or phosphorus ammonium based compound.
The preparation method of above-mentioned graphene expansion type low-smoke fireproof coating, specific step is as follows：
1）Fluorinated graphene and graphene oxide are added to the water, 2-3h is ultrasonically treated, obtains finely dispersed graphene mixed liquor；
2）By 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 1000-2000rpm disperses 1-2h, then 1500rpm grinds 30-60min in grinder, and then water-base resin and foaming agent are added, and stirring 30-60min keeps dispersion equal It is even, it is sieved to get graphene expansion type low-smoke fireproof coating.
Fire retardant mechanism of the graphene in fireproof coating is the superposition of following several fire retardations：（1）The two dimension of graphene Lamellar structure can be layering in coating, form fine and close physical isolation layer, improve flame retardant property.（2）Graphene can be with Resin be crosslinked compound in coating, is further formed one layer of fine and close protective film, plays the role of obstructing air, to play Fire-retardant effect.（3）Graphene coating burns generate carbon dioxide and water at high temperature, and generate finer and close, continuous carbon Layer, barrier action are stronger.
The invention has the advantages that：Fireproof coating prepared by the present invention can improve the intensity of charring layer, improve Fire resistance；Graphene and carbon fiber can cooperate with the generation for inhibiting volatile degradation products, and it is saturating to form a kind of efficient anti-seepage Reticular structure resists the release for decomposing the pernicious gas generated.
Specific embodiment
The following is specific embodiments of the present invention, is described further to technical solution of the present invention, but of the invention Protection scope is not limited to these examples.It is all to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute Protection scope within.
Embodiment 1
A kind of graphene expansion type low-smoke fireproof coating, is made of the raw material of following weight parts：270 parts of aqueous polyurethane, 2- 200 parts of chloroethyl phosphonate, 30 parts of fluorinated graphene, 12 parts of graphene oxide, 30 parts of carbon fiber powder, boric acid melamine 10 Part, 3 parts of dipentaerythritol, 1.5 parts of alkali formula copper molybdate, 10 parts of perlite, 5 parts of octamethylcy-clotetrasiloxane, alkyl phenol polyoxy second 3 parts of alkene ether, 2 parts of double cyanogen ammoniums, 300 parts of water.
Fluorinated graphene is prepared first, and steps are as follows：It adds graphene oxide into deionized water, ultrasonic treatment 2h obtains oxygen Graphite aqueous solution；Graphene oxide water solution is added in the water heating kettle with polytetrafluoroethyllining lining, fluorination is then added Agent, 150 DEG C of reaction 25h, is cooled to room temperature after reaction, filtering, and filter cake is washed till neutrality with deionized water, drying to get Fluorinated graphene.
The preparation method of graphene expansion type low-smoke fireproof coating, specific step is as follows：
1）Fluorinated graphene and graphene oxide are added to the water, 2h is ultrasonically treated, obtains finely dispersed graphene mixed liquor；
2）By 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 1500rpm disperses 1h, are then grinding 1500rpm grinds 40min in machine, and then aqueous polyurethane and double cyanogen ammoniums are added, and stirring 50min makes to be uniformly dispersed, and is sieved, i.e., Obtain graphene expansion type low-smoke fireproof coating.
Embodiment 2
A kind of graphene expansion type low-smoke fireproof coating, is made of the raw material of following weight parts：250 parts of aqueous epoxy resins, 150 parts of 2 chloroethyl phosphoric acid ester, 20 parts of fluorinated graphene, 15 parts of graphene oxide, 20 parts of carbon fiber powder, boric acid melamine 15 parts, 4 parts of dipentaerythritol, 1.8 parts of alkali formula copper molybdate, 5 parts of perlite, 4 parts of octamethylcy-clotetrasiloxane, alkyl phenol polyoxy second 4 parts of alkene ether, 1.5 parts of phosphorus ammonium based compound, 250 parts of water.
Fluorinated graphene is prepared first, and steps are as follows：It adds graphene oxide into deionized water, ultrasonic treatment 2h obtains oxygen Graphite aqueous solution；Graphene oxide water solution is added in the water heating kettle with polytetrafluoroethyllining lining, fluorination is then added Agent, 100 DEG C of reaction 23h, is cooled to room temperature after reaction, filtering, and filter cake is washed till neutrality with deionized water, drying to get Fluorinated graphene.
The preparation method of graphene expansion type low-smoke fireproof coating, specific step is as follows：
1）Fluorinated graphene and graphene oxide are added to the water, 3h is ultrasonically treated, obtains finely dispersed graphene mixed liquor；
2）By 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 1800rpm disperses 1.5h, are then grinding 1500rpm grinds 50min in grinding machine, and then aqueous epoxy resins and phosphorus ammonium based compound are added, and stirring 30min keeps dispersion equal It is even, it is sieved to get graphene expansion type low-smoke fireproof coating.
Embodiment 3
A kind of graphene expansion type low-smoke fireproof coating, is made of the raw material of following weight parts：Water-based acrylic resin 200 Part, 250 parts of 2 chloroethyl phosphoric acid ester, 25 parts of fluorinated graphene, 13 parts of graphene oxide, 40 parts of carbon fiber powder, boric acid trimerization 13 parts of cyanamide, 5 parts of dipentaerythritol, 2 parts of alkali formula copper molybdate, 15 parts of perlite, 5 parts of octamethylcy-clotetrasiloxane, alkyl phenol is poly- 5 parts of ethylene oxide ether, 2 parts of phosphorus ammonium based compound, 400 parts of water.
Fluorinated graphene is prepared first, and steps are as follows：It adds graphene oxide into deionized water, ultrasonic treatment 3h obtains oxygen Graphite aqueous solution；Graphene oxide water solution is added in the water heating kettle with polytetrafluoroethyllining lining, fluorination is then added Agent, 200 DEG C of reaction 22h, is cooled to room temperature after reaction, filtering, and filter cake is washed till neutrality with deionized water, drying to get Fluorinated graphene.
The preparation method of graphene expansion type low-smoke fireproof coating, specific step is as follows：
1）Fluorinated graphene and graphene oxide are added to the water, 2.5h is ultrasonically treated, obtains finely dispersed graphene mixed liquor；
2）By 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 1000rpm disperses 2h, are then grinding 1500rpm grinds 30min in machine, and then water-based acrylic resin and phosphorus ammonium based compound are added, and stirring 60min keeps dispersion equal It is even, it is sieved to get graphene expansion type low-smoke fireproof coating.
Embodiment 4
A kind of graphene expansion type low-smoke fireproof coating, is made of the raw material of following weight parts：Water-based acrylic resin 300 Part, 220 parts of 2 chloroethyl phosphoric acid ester, 28 parts of fluorinated graphene, 10 parts of graphene oxide, 35 parts of carbon fiber powder, boric acid trimerization 12 parts of cyanamide, 4 parts of dipentaerythritol, 1 part of alkali formula copper molybdate, 12 parts of perlite, 3 parts of octamethylcy-clotetrasiloxane, alkyl phenol is poly- 4 parts of ethylene oxide ether, 1 part of double cyanogen ammoniums, 350 parts of water.
Fluorinated graphene is prepared first, and steps are as follows：It adds graphene oxide into deionized water, ultrasonic treatment 2.5h is obtained Graphene oxide water solution；Graphene oxide water solution is added in the water heating kettle with polytetrafluoroethyllining lining, fluorine is then added Agent, 130 DEG C of reaction 20h, is cooled to room temperature after reaction, and filter cake is washed till neutrality with deionized water by filtering, dries, i.e., Obtain fluorinated graphene.
The preparation method of graphene expansion type low-smoke fireproof coating, specific step is as follows：
1）Fluorinated graphene and graphene oxide are added to the water, 2h is ultrasonically treated, obtains finely dispersed graphene mixed liquor；
2）By 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 2000rpm disperses 1h, are then grinding 1500rpm grinds 60min in machine, and then water-based acrylic resin and double cyanogen ammoniums are added, and stirring 40min makes to be uniformly dispersed, mistake Sieve is to get graphene expansion type low-smoke fireproof coating.

Claims (5)

1. a kind of graphene expansion type low-smoke fireproof coating, which is characterized in that be made of the raw material of following weight parts：
200-300 parts of water-base resin,
150-250 parts of 2 chloroethyl phosphoric acid ester,
20-30 parts of fluorinated graphene,
10-15 parts of graphene oxide,
20-40 parts of carbon fiber powder,
10-15 parts of boric acid melamine,
3-5 parts of dipentaerythritol,
1-2 parts of alkali formula copper molybdate,
5-15 parts of perlite,
3-5 parts of octamethylcy-clotetrasiloxane,
3-5 parts of alkyl phenol polyoxyethylene ether,
1-2 parts of foaming agent,
250-400 parts of water.
2. graphene expansion type low-smoke fireproof coating as described in claim 1, which is characterized in that the fluorinated graphene Preparation method is as follows：It adds graphene oxide into deionized water, ultrasonic treatment 2-3h obtains graphene oxide water solution；It will oxidation Graphene aqueous solution is added in the water heating kettle with polytetrafluoroethyllining lining, and fluorization agent, 100-200 DEG C of reaction 20- is then added 25h is cooled to room temperature after reaction, filtering, and filter cake is washed till neutrality with deionized water, is dried to get fluorinated graphene.
3. graphene expansion type low-smoke fireproof coating as described in claim 1, which is characterized in that the water-base resin is water One of property polyurethane, aqueous epoxy resins or water-based acrylic resin.
4. graphene expansion type low-smoke fireproof coating as described in claim 1, which is characterized in that the foaming agent is double cyanogen Ammonium or phosphorus ammonium based compound.
5. the preparation method of the graphene expansion type low-smoke fireproof coating as described in claim 1-4 is any, which is characterized in that Steps are as follows：
1) fluorinated graphene and graphene oxide are added to the water, are ultrasonically treated 2-3h, obtain finely dispersed graphene mixed liquor；
2) by 2 chloroethyl phosphoric acid ester, carbon fiber powder, boric acid melamine, dipentaerythritol, alkali formula copper molybdate, perlite, Octamethylcy-clotetrasiloxane, alkyl phenol polyoxyethylene ether are added in graphene mixed liquor, and 1000-2000rpm disperses 1-2h, then 1500rpm grinds 30-60min in grinder, and then water-base resin and foaming agent are added, and stirring 30-60min keeps dispersion equal It is even, it is sieved to get graphene expansion type low-smoke fireproof coating.
CN201810760474.4A 2018-07-12 2018-07-12 A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof Pending CN108841229A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430416A (en) * 2020-11-17 2021-03-02 福建南烽防火科技有限公司 Expansion heat-insulation anticorrosive paint and preparation method thereof
CN112473065A (en) * 2020-12-07 2021-03-12 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430416A (en) * 2020-11-17 2021-03-02 福建南烽防火科技有限公司 Expansion heat-insulation anticorrosive paint and preparation method thereof
CN112473065A (en) * 2020-12-07 2021-03-12 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof
CN112473065B (en) * 2020-12-07 2022-04-05 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof

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