CN115814327A - Aqueous film-forming foam extinguishing agent and preparation method thereof - Google Patents
Aqueous film-forming foam extinguishing agent and preparation method thereof Download PDFInfo
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- CN115814327A CN115814327A CN202111092778.6A CN202111092778A CN115814327A CN 115814327 A CN115814327 A CN 115814327A CN 202111092778 A CN202111092778 A CN 202111092778A CN 115814327 A CN115814327 A CN 115814327A
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- aqueous film
- forming foam
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- 239000006260 foam Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 58
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 54
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 46
- 125000002091 cationic group Chemical group 0.000 claims abstract description 23
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 21
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 16
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 16
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 16
- 239000003381 stabilizer Substances 0.000 claims abstract description 9
- 239000006184 cosolvent Substances 0.000 claims abstract description 7
- 239000003755 preservative agent Substances 0.000 claims abstract description 7
- 230000002335 preservative effect Effects 0.000 claims abstract description 7
- PBVZTJDHQVIHFR-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoroprop-1-ene Chemical compound FC(F)=C(F)C(F)(F)F.FC(F)=C(F)C(F)(F)F PBVZTJDHQVIHFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 5
- 238000007710 freezing Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 18
- 239000004202 carbamide Substances 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical group [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 12
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 11
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical group O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 11
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 claims description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229940125782 compound 2 Drugs 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 4
- 229940125904 compound 1 Drugs 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000007798 antifreeze agent Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- PQJJJMRNHATNKG-UHFFFAOYSA-N ethyl bromoacetate Chemical compound CCOC(=O)CBr PQJJJMRNHATNKG-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- HVTICUPFWKNHNG-UHFFFAOYSA-N iodoethane Chemical compound CCI HVTICUPFWKNHNG-UHFFFAOYSA-N 0.000 claims description 2
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- 239000011698 potassium fluoride Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- WFRKJMRGXGWHBM-UHFFFAOYSA-M sodium;octyl sulfate Chemical compound [Na+].CCCCCCCCOS([O-])(=O)=O WFRKJMRGXGWHBM-UHFFFAOYSA-M 0.000 claims description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 2
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009044 synergistic interaction Effects 0.000 abstract 1
- 230000001988 toxicity Effects 0.000 abstract 1
- 231100000419 toxicity Toxicity 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 24
- 238000005303 weighing Methods 0.000 description 22
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical group [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 11
- 235000010234 sodium benzoate Nutrition 0.000 description 11
- 239000004299 sodium benzoate Substances 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YLIMHFXLIKETBC-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCC[Na] YLIMHFXLIKETBC-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229920004449 Halon® Polymers 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- -1 fluorocarbon quaternary ammonium salt Chemical class 0.000 description 4
- 239000004302 potassium sorbate Substances 0.000 description 4
- 235000010241 potassium sorbate Nutrition 0.000 description 4
- 229940069338 potassium sorbate Drugs 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 235000013373 food additive Nutrition 0.000 description 3
- 239000002778 food additive Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- HWMMCEJITBPQBR-UHFFFAOYSA-N CCCCCCCC[Na] Chemical compound CCCCCCCC[Na] HWMMCEJITBPQBR-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- BHFJBHMTEDLICO-UHFFFAOYSA-N Perfluorooctylsulfonyl fluoride Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)S(F)(=O)=O BHFJBHMTEDLICO-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000254 damaging effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention discloses an aqueous film-forming foam extinguishing agent and a preparation method thereof, wherein the product consists of a fluorocarbon surfactant, a hydrocarbon surfactant, a foam stabilizer, a cosolvent, an anti-burning agent, an anti-freezing agent and a preservative, wherein the fluorocarbon surfactant is a perfluorinated branched short-chain cationic surfactant prepared by taking an industrialized hexafluoropropylene dimer as an initial raw material. The fire extinguishing agent disclosed by the invention contains the perfluorinated branched short-chain environment-friendly quaternary ammonium salt cationic fluorocarbon surfactant, is low in toxicity, good in biodegradability and high in surface activity, and obviously shows excellent performance through synergistic interaction when being compounded with the hydrocarbon surfactant, so that the use cost of the aqueous film forming foam fire extinguishing agent can be reduced, and the fire extinguishing agent has the characteristics of high fire extinguishing speed, high fire extinguishing efficiency and the like.
Description
Technical Field
The invention belongs to the field of fire-fighting and fire-extinguishing materials, and particularly relates to an aqueous film-forming foam extinguishing agent, and more particularly relates to an efficient and environment-friendly aqueous film-forming foam extinguishing agent based on a perfluoro-branched short-chain fluorocarbon quaternary ammonium salt cationic surfactant and a preparation method thereof.
Background
The Halon fire extinguishing agent is widely applied and researched due to the excellent fire extinguishing performance of the Halon fire extinguishing agent. However, since the first death of people from carbon tetrachloride in 1919, and the discovery in 1974 that chlorofluorocarbons (CFCs) and halons have a long life in the atmosphere and a strong damaging effect on the ozone layer, alternatives to halons have been sought.
In the report of the Harong technical selection Committee, 5 kinds of fire extinguishers are recommended as substitutes for the Harong 1211 hand fire extinguisher according to fire extinguishing objects, wherein the aqueous film-forming foam fire extinguishing agent has the best fire extinguishing effect due to the double fire extinguishing action of the aqueous film and the foam, and more than 97% of the components in the aqueous film-forming foam fire extinguishing agent are water, so that the aqueous film-forming foam fire extinguishing agent is taken as an ideal substitute for the Harong fire extinguishing agent in the international 'Harong elimination action' and becomes a fire extinguishing agent with key development in the world. At present, perfluorooctane sulfonyl compounds (PFOS) are mostly used as fluorocarbon surfactants in aqueous film-forming foam extinguishing agents on the market, and the water-forming foam extinguishing agents not only have hydrophobic and oleophobic properties, but also have extremely strong durability, so that the fire extinguishing agents can be guaranteed to have high stability in various environments; however, PFOS has very poor degradation performance and is an organic pollutant which is relatively difficult to decompose. Furthermore, our country has gradually increased control over perfluorooctylsulfonic acid and its salt products, and perfluorooctylsulfonyl fluoride products (PF 0S-type products), which have been listed in the list of persistent organic pollutants, and is gradually under phase-out.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an aqueous film-forming foam extinguishing agent from the perspective of high efficiency and environmental protection.
In order to achieve the above purpose of the present invention, the present invention provides the following technical solutions:
an aqueous film-forming foam extinguishing agent is composed of a cationic fluorocarbon surfactant, a hydrocarbon surfactant, a foam stabilizer, a cosolvent, an anti-burning agent, an anti-freezing agent, a preservative and water, and the mass percentages of the components are as follows:
preferably, the fluorocarbon surfactant is a perfluoro-branched short-chain fluorocarbon cationic surfactant with a linear fluorocarbon atom of 5.
Specifically, the fluorocarbon surfactant is a quaternary ammonium salt cationic fluorocarbon surfactant, and has the following structure:
preferably, the hydrocarbon surfactant is one or two of sodium n-octyl sulfate and dodecyl betaine.
Preferably, the cosolvent is diethylene glycol monobutyl ether.
Preferably, the anti-burning agent is urea.
Preferably, the foam stabilizer is sodium carboxymethylcellulose.
Preferably, the antifreeze agent is ethylene glycol.
Preferably, the water is deionized water or industrial soft water.
Preferably, the preservative is sodium benzoate or potassium sorbate.
The method for preparing the aqueous film-forming foam extinguishing agent comprises the following steps: weighing fluorocarbon surfactant and hydrocarbon surfactant according to the proportion of the components, mixing and stirring to form a component A, weighing foam stabilizer, cosolvent and water, mixing to form a component B, finally weighing anti-burning agent, anti-freezing agent and preservative, mixing uniformly to form a component C, adding B into A, mixing, slowly adding C, and stirring uniformly to prepare the fire extinguishing agent concentrated solution.
According to the aqueous film-forming foam extinguishing agent, when in use, the concentrated solution of the extinguishing agent is mixed with water according to the volume ratio of 3.
Compared with the prior art, the invention has the advantages that:
(1) The invention can be stored and used for a long time and is not easy to decay. The main components of the fire extinguishing agent and the added additive are nontoxic and pollution-free, and belong to environment-friendly products.
(2) The preparation method of the invention does not need heating and filtering, does not generate three wastes, is environment-friendly and energy-saving, and has high production efficiency.
(3) The foam prepared by the invention has good stability and high fire extinguishing efficiency, belongs to a high-efficiency environment-friendly product, and can be widely applied to fire-proof key units such as oil fields, oil depots, ships, submarines, petrochemical products, hangars, airports and the like.
Drawings
FIG. 1 is a nuclear magnetic resonance hydrogen spectrum of the quaternary ammonium salt cationic fluorocarbon surfactant.
FIG. 2 is a FNMR map of the quaternary ammonium salt cationic fluorocarbon surfactant of the present invention.
FIG. 3 is a fire extinguishing diagram of an aqueous film forming foam fire extinguishing agent according to example 1 of the present invention.
FIG. 4 is a graph showing the burning resistance of the aqueous film-forming fire foam of example 1 of the present invention.
Detailed Description
The following examples are provided to further illustrate the essence of the present invention, but are not intended to limit the present invention.
According to the invention, from the perspective of high efficiency and environmental protection, the perfluorinated branched short-chain quaternary ammonium salt cationic fluorocarbon surfactant is prepared, and the cationic fluorocarbon surfactant and the hydrocarbon surfactant are compounded, so that the cationic fluorocarbon surfactant and the hydrocarbon surfactant are compounded to generate an excellent synergistic effect, and the addition of the hydrocarbon surfactant can obviously reduce the surface tension of an aqueous solution of the fluorocarbon surfactant and can also obviously reduce the use concentration of the fluorocarbon surfactant.
The fluorocarbon surfactant used in the invention is a quaternary ammonium salt cationic fluorocarbon surfactant synthesized by taking hexafluoropropylene dimer as a raw material, can reduce the surface tension of water to be less than 21mN/m, and is superior to hydrocarbon surfactants. In addition, the water-soluble foam oil has little environmental pollution, is a green and environment-friendly surfactant, has high thermal stability and chemical stability, and has the function of reducing the surface tension of water, so that the foam solution can form a water film on the oil surface and quickly spread to seal the oil surface, thereby achieving the purpose of quickly extinguishing fire.
The fluorocarbon surfactant used in the invention is a perfluoro branched short-chain quaternary ammonium salt cationic fluorocarbon surfactant, and the synthetic route is as follows:
the following provides the synthesis process and structural characterization of the perfluoro branched short-chain quaternary ammonium salt cationic fluorocarbon surfactant.
1g of hexafluoropropylene dimer (D2) and 0.6123g of ethyl bromoacetate were slowly added dropwise to a stirred solution of 3.33mL of dry N-N dimethylacetamide (DMAc), 0.0167g of tetrabutylammonium bromide and 0.236g of potassium fluoride under an argon atmosphere. The reaction was then heated at 80 ℃ for 24 hours, cooled to room temperature, poured into ether, washed with water and brine. Finally, the organic solvent is dried by anhydrous sodium sulfate, filtered, concentrated under reduced pressure and purified by column chromatography (petroleum ether: ethyl acetate = 20).
Compound 1 and 5mL n, n-dimethylethylenediamine were added to a 25mL sealed tube, and after sealing, the mixture was placed in a 130 ℃ oil bath and stirred for reaction for 34 hours, cooled to room temperature, concentrated by spin drying, and purified by column chromatography (dichloromethane: methanol = 20) to obtain compound 2.
After purging three times with 50mL of a sealed tube, 0.37g of iodoethane, 0.65g of Compound 2, and 7.0mL of anhydrous acetonitrile were added in that order under argon. The whole was then stirred at 80 ℃ for 3 hours. And finally, moving to room temperature, removing the solvent, washing the solid with acetone, filtering, dissolving with methanol, and carrying out reduced pressure rotary evaporation to remove the solvent to obtain the quaternary ammonium salt cationic fluorocarbon surfactant. The hydrogen spectrum and FNMR map are shown in FIG. 1 and FIG. 2, respectively.
1 HNMR(300MHz,CD 3 OD)δ3.64(t,J=7.1Hz,2H),3.47(q,J=7.3Hz,2H),3.38(t,2H),3.25(s,2H),3.13(s,6H),1.40(t,J=7.3Hz,3H);
19 FNMR(282MHz,CD 3 OD)δ-67.37to-68.45(m,6F),-85.14to-85.99(m,3F),-111.28to-112.85(m,2F),-127.20to-127.88(m,2F);
LRMS(ESI)m/z:477.1([M-I]+).。
The hydrocarbon surfactant used in the invention is n-octyl sodium sulfate and dodecyl betaine, has excellent foaming performance, and can reduce the interfacial tension between the foam solution and the oil surface. The following are quaternary ammonium salt cation fluorocarbon surfactant and different hydrocarbon surfactants, and the compound ratio is 1: surface tension and critical micelle concentration at 1, data are shown in table 1 below.
TABLE 1
According to the invention, by compounding the fluorocarbon surfactant and the hydrocarbon surfactant, lower surface tension and good spreading performance can be ensured.
The cosolvent of the invention uses diethylene glycol monobutyl ether. Not only has the function of helping dissolution, but also can strengthen the stability of the foam.
The anti-burning agent is preferably urea. Besides the anti-burning effect, the urea can further increase the stability of the foam and has a certain dissolution assisting effect.
The foam stabilizer of the invention is preferably sodium carboxymethylcellulose. The sodium carboxymethyl cellulose has better foam stability as a foam stabilizer.
The preservative of the invention uses one or two of sodium benzoate and potassium sorbate. Sodium benzoate and potassium sorbate as food additive have high sterilizing and antiseptic effect and no environmental pollution.
The fire extinguishing agent components prepared in the following examples and comparative examples are all commercial products except that the quaternary ammonium salt cationic fluorocarbon surfactant is self-prepared.
Example 1:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfate and 3.4kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 3kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; 3kg of urea and 20kg of glycol are weighed and evenly mixed, slowly added into the A, 5kg of sodium benzoate is added, finally water is added for diluting to 100kg, and the mixture is evenly stirred to obtain 100kg of foam extinguishing agent concentrated solution.
Example 2:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfate and 6kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 3kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; weighing 3kg of urea and 20kg of ethylene glycol, uniformly mixing, slowly adding the urea and the ethylene glycol into the mixture A, adding 5kg of sodium benzoate, finally adding water to dilute the mixture to 100kg, and uniformly stirring to obtain 100kg of foam extinguishing agent concentrated solution.
Example 3:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfate and 6kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 6kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; weighing 3kg of urea and 20kg of ethylene glycol, uniformly mixing, slowly adding the urea and the ethylene glycol into the mixture A, adding 5kg of sodium benzoate, finally adding water to dilute the mixture to 100kg, and uniformly stirring to obtain 100kg of foam extinguishing agent concentrated solution.
Example 4:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfate and 6kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 6kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; weighing 5kg of urea and 20kg of ethylene glycol, uniformly mixing, slowly adding the urea and the ethylene glycol into the mixture A, adding 5kg of sodium benzoate, finally adding water to dilute the mixture to 100kg, and uniformly stirring to obtain 100kg of foam extinguishing agent concentrated solution.
Example 5:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfate and 4kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 3kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; 3kg of urea and 20kg of glycol are weighed and evenly mixed, slowly added into the A, 5kg of sodium benzoate is added, finally water is added for diluting to 100kg, and the mixture is evenly stirred to obtain 100kg of foam extinguishing agent concentrated solution.
Comparative example 1:
weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant as a compound A; weighing 5kg of diethylene glycol monobutyl ether, 3kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; weighing 3kg of urea and 20kg of ethylene glycol, uniformly mixing, slowly adding the urea and the ethylene glycol into the mixture A, adding 5kg of sodium benzoate, finally adding water to 100kg, and uniformly stirring to obtain 100kg of foam extinguishing agent concentrated solution.
Comparative example 2:
respectively weighing 10kg of quaternary ammonium salt cationic fluorocarbon surfactant, 1.9kg of n-octyl sodium sulfonate and 3.4kg of dodecyl betaine, and uniformly mixing to form a mixture A; weighing 5kg of diethylene glycol monobutyl ether, 3kg of sodium carboxymethylcellulose and 30kg of water, and uniformly mixing to form a mixture B; adding B into A and stirring; weighing 3kg of urea and 20kg of ethylene glycol, uniformly mixing, slowly adding the urea and the ethylene glycol into the mixture A, adding 5kg of sodium benzoate, finally adding water to dilute the mixture to 100kg, and uniformly stirring to obtain 100kg of foam extinguishing agent concentrated solution.
The solution prepared by mixing the concentrated solution product of the comparative example 1 and water according to the volume ratio of 3.
The aqueous film-forming foam fire extinguishing agent concentrates prepared in examples 1 to 5 and comparative example 2 and the fire extinguishing agent concentrates prepared in comparative example have the specific compositions shown in table 2 below.
TABLE 2
The solution prepared by mixing the fire extinguishing agent concentrated solution obtained in the above examples 1-5 and water according to the volume ratio of 3. The product self-inspection is tested according to national standard GB15308-2006, and each technical index is shown in the following table 3, wherein the fire extinguishing effect and the anti-burning effect of the fire extinguishing agent of the example 1 are respectively shown in fig. 3 and fig. 4.
TABLE 3
As is clear from the above results, the present invention has the following features:
(1) The synthetic route of the fluorocarbon surfactant takes industrialized hexafluoropropylene dimer as an initial raw material, is easy to operate under mild reaction conditions, has low cost and is easy to industrially amplify.
(2) The product of the invention generates synergistic effect by compounding with the hydrocarbon surfactant, greatly reduces the usage amount of the fluorocarbon surfactant and can further reduce the cost of the aqueous film-forming foam extinguishing agent. High fire extinguishing efficiency and strong burning resistance. Is green and environment-friendly.
(3) The used hydrocarbon surfactant has little toxic and side effect on the environment and is a green and environment-friendly substance; the fluorocarbon surfactant belongs to a novel perfluoro branched short-chain fluorocarbon cationic surfactant, has low toxicity and good biodegradability, and has less environmental pollution; diethylene glycol monobutyl ether and ethylene glycol are widely used in organic compounds of various chemical industries, and have small environmental pollution; urea is one of the most common organic fertilizers, and has negligible harm to the environment as the anti-burning agent of the invention; sodium carboxymethylcellulose is a common food additive, is used as the foam stabilizer of the invention, has no toxic or side effect on the ecological environment, and the preservative adopts potassium sorbate or sodium benzoate, both of which are common food additives, and has no toxic or side effect. Therefore, the product of the invention is an environment-friendly product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
2. The aqueous film-forming foam fire suppressant of claim 1 wherein said fluorocarbon surfactant is a perfluoro-branched short-chain fluorocarbon cationic surfactant having a linear fluorocarbon atom of 5.
4. the aqueous film-forming foam fire suppressant of claim 3 wherein the quaternary ammonium salt cationic fluorocarbon surfactant is prepared by the steps of:
(1) Slowly and dropwise adding hexafluoropropylene dimer and ethyl bromoacetate into a mixed solution of N-N dimethylacetamide, tetrabutylammonium bromide and potassium fluoride under an argon atmosphere, heating the reaction system at 80 ℃ for 24 hours, cooling to room temperature, and carrying out aftertreatment to obtain a compound 1;
(2) Adding the compound 1 and N, N-dimethylethylenediamine into a sealed tube, sealing, placing the sealed tube in an oil bath kettle at 130 ℃, stirring for reaction for 34 hours, cooling to room temperature, and performing post-treatment to obtain a compound 2;
(3) And (3) pumping the sealed tube for three times, sequentially adding ethyl iodide, a compound 2 and anhydrous acetonitrile under the protection of argon, stirring the whole system at 80 ℃ for reaction for 3 hours, and performing aftertreatment to obtain the quaternary ammonium salt cationic fluorocarbon surfactant.
5. The aqueous film-forming foam fire suppressant of claim 1 wherein the hydrocarbon surfactant is one or both of sodium n-octyl sulfate and dodecyl betaine.
6. The aqueous film-forming foam fire extinguishing agent according to claim 1, wherein the cosolvent is diethylene glycol monobutyl ether.
7. The aqueous film-forming foam fire suppressant of claim 1 wherein the fire suppressant is urea.
8. The aqueous film-forming foam fire extinguishing agent according to claim 1, wherein the foam stabilizer is sodium carboxymethylcellulose.
9. The aqueous film-forming foam fire suppressant of claim 1 wherein the anti-freeze agent is ethylene glycol.
10. The method for preparing the aqueous film-forming foam fire extinguishing agent according to any one of claims 1 to 9, characterized in that the fluorocarbon surfactant and the hydrocarbon surfactant are weighed according to the proportion of the components to be mixed and stirred to form a component A, the foam stabilizer, the cosolvent and the water are weighed to be mixed to form a component B, finally the anti-burning agent, the anti-freezing agent and the preservative are weighed to be uniformly mixed to form a component C, the component B is added into the component A to be mixed, the component C is slowly added, and the mixture is uniformly stirred to form the concentrated solution of the aqueous film-forming foam fire extinguishing agent.
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