CN118416438A - Composition for fire extinguishing agent, fire extinguishing agent and preparation method and application thereof - Google Patents
Composition for fire extinguishing agent, fire extinguishing agent and preparation method and application thereof Download PDFInfo
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- CN118416438A CN118416438A CN202410329420.8A CN202410329420A CN118416438A CN 118416438 A CN118416438 A CN 118416438A CN 202410329420 A CN202410329420 A CN 202410329420A CN 118416438 A CN118416438 A CN 118416438A
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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
- A62D1/0028—Liquid extinguishing substances
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/20—Mountings; Secondary casings or frames; Racks, modules or packs; Suspension devices; Shock absorbers; Transport or carrying devices; Holders
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- Fire-Extinguishing Compositions (AREA)
Abstract
The invention relates to the technical field of energy storage lithium ion battery safety, and discloses a composition for a fire extinguishing agent, the fire extinguishing agent, a preparation method and application thereof. The composition comprises 60-90wt% of perfluorinated compounds, 5-35wt% of halogenated olefins, 2-25wt% of polar flame retardant compounds and 1-5wt% of solubilizers; the content mass ratio of the olefin I to the olefin II in the halogenated olefin is 1:1-2; the alkene I is propylene substituted with at least 3 halogen atoms and/or butene substituted with at least 3 halogen atoms; and the halogen atoms in the alkene I include at least one Br and at least one F; the alkene II is propylene substituted with at least 4 halogen atoms; and the halogen atoms in the alkene II include at least one Cl and at least one F. The fire extinguishing agent provided by the invention has high fire extinguishing efficiency and low toxicity, and can be widely applied to energy storage lithium ion battery fire extinguishing systems.
Description
Technical Field
The invention relates to the technical field of energy storage lithium ion battery safety, in particular to a composition for a fire extinguishing agent, the fire extinguishing agent, a preparation method and application thereof.
Background
The lithium ion battery energy storage is an important energy storage system, according to the statistics of the Guanyu energy storage industry technology alliance in China, the installed scale of the energy storage lithium ion battery in 2022 breaks through 6GW, and is increased by 228% in comparison with 2021, and the installed scale is expected to reach 600GW in 2035.
However, under the induction of internal and external faults, the lithium ion battery is extremely easy to generate thermal runaway, release a large amount of flammable and explosive gases and cause fire and explosion; in addition, when the energy storage lithium ion battery system has a thermal runaway fault, electrolyte in the battery can volatilize to form flammable and explosive white fog, and the white fog is extremely easy to explode under the ignition of sparks and the like
With the increasing capacity of lithium ion battery energy storage power stations (hundreds of MWh to several GWh), safety problems such as fire explosion and the like have become key to restrict the development of the lithium ion battery energy storage industry.
Conventional energy storage lithium ion battery extinguishing media include water mist, heptafluoropropane and perfluoro hexanone.
However, the fine water mist is difficult to pass through the flame plume and the smoke plume to reach the root of the flame source in a short time, and the defect of long open flame extinguishing time exists; and when the battery is out of control, a large amount of lithium salt with strong electric conduction property can be sprayed out, and electrical equipment short circuit is easily caused when the lithium salt contacts with water mist, so that fire disaster is enlarged.
The heptafluoropropane has high boiling point, small vaporization latent heat and poor temperature reduction performance on thermal runaway, so that the fire extinguishing effect is poor.
The perfluoro-hexanone has large gasification latent heat and high fire extinguishing efficiency, but fluorine-based fire extinguishing agents including perfluoro-hexanone can generate a large amount of hydrogen fluoride gas which is poisonous and harmful to human bodies in the fire extinguishing process, so that the safety performance is poor.
In summary, there is a need to develop an energy storage lithium ion battery fire extinguishing medium with high fire extinguishing efficiency, low toxicity and reduced flammability of electrolyte.
CN117531162a discloses a fire extinguishing composition. The composition comprises perfluoro-hexanone, a fluorine-containing surfactant and a fluorinated solution; and the proportion of the perfluorinated hexanone in the fire-extinguishing composition is not less than 55wt%; the fluorinated liquid comprises at least one of perfluorobutyl methyl ether, perfluorobutyl ethyl ether, 1,2,3,4, 5-decafluoro-3-methoxy-4- (trifluoromethyl) -pentane and 3-ethoxy-1,1,1,2,3,4,4,5,5,6,6,6-dodecafluoro-2-trifluoromethyl-hexane. The fire extinguishing composition has good fire extinguishing performance and high storage retention rate at normal temperature. However, the composition can generate a large amount of poisonous gas of hydrogen fluoride during fire extinguishment, and has high toxicity.
CN113209536a discloses a perfluoro-hexanone emulsion fire-extinguishing agent of composite fire retardant. The fire extinguishing agent comprises oil system perfluorinated hexanone as a liquid phase component, a solid flame retardant synergist as a solid phase component and coated with a nonionic flame retardant, and an emulsifier for mixing and connecting the liquid phase component and the solid phase component; the nonionic flame retardant is one or a mixture of a plurality of phosphorus flame retardants, brominated flame retardants and halogenated phosphate mixed flame retardants; the mass ratio of the oil system perfluorinated hexanone to the solid flame retardant synergist to the emulsifier is (10-50) 1:10. The composite fire extinguishing agent has low cost, good environmental protection and excellent effect of inhibiting fire of the lithium ion battery. However, after the fire extinguishing agent is used for extinguishing a fire, a flame-retardant layer with electric conduction capacity is formed on the surface of a fire object, and for extinguishing a fire of electrified equipment such as a battery, the electric conduction flame-retardant layer can cause short circuit of the battery or the electric equipment, so that secondary disasters are easy to cause. In addition, when the fire extinguishing agent is used for extinguishing fire of the battery, once the fire extinguishing agent is sprayed by mistake under normal conditions, a large amount of solid and liquid conductive flame retardant can be remained on the surface of the battery, so that the safety of the battery is threatened.
Disclosure of Invention
The invention aims to solve the problems of low fire extinguishing efficiency and large amount of toxic gas generated in the fire extinguishing process when an energy storage lithium ion battery is in fire in the prior art.
In order to achieve the above object, a first aspect of the present invention provides a composition for a fire extinguishing agent, which contains 60 to 90wt% of a perfluoro compound, 5 to 35wt% of a halogenated olefin, 2 to 25wt% of a polar flame retardant compound, and 1 to 5wt% of a solubilizing agent;
The content mass ratio of the olefin I to the olefin II in the halogenated olefin is 1:1-2;
the alkene I is propylene substituted with at least 3 halogen atoms and/or butene substituted with at least 3 halogen atoms; and the halogen atoms in the alkene I include at least one Br and at least one F;
the alkene II is propylene substituted with at least 4 halogen atoms; and the halogen atoms in the alkene II include at least one Cl and at least one F.
Preferably, the composition contains 65-75wt% of a perfluorinated compound, 15-20wt% of a halogenated olefin, 5-15wt% of a polar flame retardant compound and 2-4wt% of a solubilizing agent.
Preferably, the alkene I is propylene substituted with 1 Br and 2F and/or butene substituted with 1 Br and 2F.
Preferably, the olefin II is selected from at least one of propylene substituted with 1 Cl and 3F, propylene substituted with 2 Cl and 2F, propylene substituted with 3 Cl and 1F, and propylene substituted with 4 Cl and 1F.
Preferably, the olefin I is 2-bromo-3, 3-trifluoropropene; the olefin II is 2-chloro-3, 3-trifluoropropene.
Preferably, the perfluorinated compound is selected from at least one of perfluoroethane, perfluoropropane, perfluorobutane, perfluoropentane, perfluorocyclopentane and perfluorohexanone.
Preferably, the polar flame retardant compound is pentafluoro (phenoxy) cyclotriphosphazene and/or ethoxy (pentafluoro) cyclotriphosphazene.
Preferably, the solubilizer is at least one selected from the group consisting of sodium perfluorononenoxybenzenesulfonate, sodium perfluorooctanoate and perfluoropolyether-based surfactant.
In a second aspect, the present invention provides a method of preparing a fire extinguishing agent, the method comprising: the fire extinguishing agent is obtained by mixing the components in the composition for fire extinguishing agent according to the first aspect.
A third aspect of the present invention provides a fire extinguishing agent prepared by the method of the second aspect described above.
A fourth aspect of the present invention provides the use of the fire extinguishing agent of the third aspect in a fluorine-based high-efficiency safety fire extinguishing system for an energy storage lithium ion battery.
The invention has at least the following beneficial effects:
The perfluorinated compounds, the halogenated olefins, the polar flame retardant compounds and the solubilizer in the composition for the fire extinguishing agent can be fully mutually dissolved, can be sprayed through the same fire extinguishing system and the same pipeline, and is beneficial to improving the convenience of application and the convenience of application.
The fire extinguishing agent provided by the invention can realize high-efficiency open fire extinguishing, can obviously reduce the content of toxic gas (HF) generated during fire extinguishing, can effectively prevent the re-combustion of electrolyte smoke, and solves the safety problem when the energy storage lithium ion battery is out of control.
Drawings
FIG. 1 is a schematic diagram of a fire extinguishing process in which a fire extinguishing agent is applied to a fluorine-based high-efficiency safe fire extinguishing system of an energy storage lithium ion battery;
FIG. 2 is a schematic diagram of a fluorine-based high-efficiency and safe fire extinguishing system for an energy storage lithium ion battery in a test example of the invention.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As previously described, a first aspect of the present invention provides a composition for a fire extinguishing agent, the composition comprising 60 to 90wt% of a perfluorinated compound, 5 to 35wt% of a halogenated olefin, 2 to 25wt% of a polar flame retardant compound, and 1 to 5wt% of a solubilizing agent;
The content mass ratio of the olefin I to the olefin II in the halogenated olefin is 1:1-2;
the alkene I is propylene substituted with at least 3 halogen atoms and/or butene substituted with at least 3 halogen atoms; and the halogen atoms in the alkene I include at least one Br and at least one F;
the alkene II is propylene substituted with at least 4 halogen atoms; and the halogen atoms in the alkene II include at least one Cl and at least one F.
Preferably, the composition contains 65-75wt% of a perfluorinated compound, 15-20wt% of a halogenated olefin, 5-15wt% of a polar flame retardant compound and 2-4wt% of a solubilizing agent. The inventors of the present invention found that in this preferred case, the fire extinguishing efficiency of the resulting fire extinguishing agent is higher.
Preferably, the alkene I is propylene substituted with 1 Br and 2F and/or butene substituted with 1 Br and 2F.
Preferably, the olefin II is selected from at least one of propylene substituted with 1 Cl and 3F, propylene substituted with 2 Cl and 2F, propylene substituted with 3 Cl and 1F, and propylene substituted with 4 Cl and 1F.
Preferably, the olefin I is 2-bromo-3, 3-trifluoropropene; the olefin II is 2-chloro-3, 3-trifluoropropene.
Preferably, the perfluorinated compound is selected from at least one of perfluoroethane, perfluoropropane, perfluorobutane, perfluoropentane, perfluorocyclopentane and perfluorohexanone.
Preferably, the polar flame retardant compound is pentafluoro (phenoxy) cyclotriphosphazene and/or ethoxy (pentafluoro) cyclotriphosphazene. The inventors of the present invention found that in this preferred case, the fire extinguishing efficiency of the resulting fire extinguishing agent is higher.
Preferably, the polar flame retardant compound is pentafluoro (phenoxy) cyclotriphosphazene.
Preferably, the solubilizing agent is selected from at least one of sodium perfluorononenoxybenzenesulfonate, sodium perfluorooctanoate and perfluoropolyether-based surfactant.
Preferably, the solubilizing agent is a perfluoropolyether-based surfactant.
In the invention, the principle of synchronously extinguishing fire and reducing the content of toxic gas (HF) by using the perfluorinated compounds and the halogenated olefin is as follows:
The CF 3 groups in the perfluorinated compounds extinguish the fire by capturing chain-borne free radicals; cl and Br in the halogenated olefin inhibit fire hazard through catalytic reforming cyclic reaction; the Cl free radicals and the Br free radicals can absorb a large amount of H free radicals, so that the combination of the H free radicals and the F free radicals to generate a large amount of HF is avoided; the specific reaction formula is as follows:
CF3+H·→CF2·+HF (1)
CF3+OH·→CF2O·+HF (2)
Cl·+H·→HCl (3)
Br·+H·→HBr (4)
HCl+OH·→Cl·+H2O (5)
HBr+OH·→Br·+H2O (6)
Cl·+H·→HCl (7)
Br·+H·→HBr (8)
As previously described, a second aspect of the present invention provides a method of preparing a fire extinguishing agent, the method comprising: the fire extinguishing agent is obtained by mixing the components in the composition for fire extinguishing agent according to the first aspect.
Preferably, the mixing conditions include: the temperature is 10-30 ℃.
As previously mentioned, a third aspect of the present invention provides a fire extinguishing agent prepared by the method of the second aspect described above.
As previously mentioned, a fourth aspect of the present invention provides the use of the fire extinguishing agent of the third aspect in a fluorine-based high-efficiency safety fire extinguishing system for energy storage lithium ion batteries.
According to a particularly preferred embodiment, the energy storage lithium ion battery fluorine-based high-efficiency and safe fire extinguishing system comprises: the device comprises a thermal runaway monitoring module, a control module, a fire extinguishing agent conveying pipeline and atomizing nozzles arranged on the periphery of each energy storage battery pack;
The fire extinguishing module comprises the fire extinguishing agent and a storage component; the storage assembly comprises a fire extinguishing agent storage tank and a control valve for controlling the fire extinguishing agent storage tank;
the fire extinguishing agent conveying pipeline comprises a main pipeline and a branch pipeline;
the thermal runaway monitoring module and the fluorine-based efficient safe fire extinguishing module are respectively connected with the control module;
the fire extinguishing agent holding vessel with the entry of trunk line links to each other, the export of trunk line with each the entry of branch pipeline links to each other, each the export of branch pipeline with atomizing nozzle links to each other.
Preferably, the pressure in the fire extinguishing agent storage tank is 4-10MPa, and the pressure source is nitrogen.
In the invention, the thermal runaway monitoring module is used for monitoring the thermal runaway characteristic gases (H2 and CO) and fire conditions of the energy storage battery compartment in real time and sending out thermal runaway gas exceeding standard and fire occurrence position signals.
In the invention, the control module is used for regulating and controlling the control valve of the fire extinguishing agent storage tank.
According to a preferred embodiment, as shown in fig. 1, the invention provides a method for extinguishing fire by using the fluorine-based efficient and safe fire extinguishing system of the energy storage lithium ion battery, which comprises the following steps:
The thermal runaway monitoring module is used for monitoring thermal runaway characteristic gas, when a fire signal occurs in the energy storage battery compartment, the thermal runaway monitoring module determines the position, and the control module is used for starting the high-efficiency safe fire extinguishing system, so that the fire extinguishing agent is atomized in the space above the battery or the space above the battery cluster, and meanwhile, high-efficiency safe fire extinguishing and electrolyte smoke re-combustion prevention are realized; if no fire signal occurs in the energy storage battery compartment, the high-efficiency safe fire extinguishing system is not started.
The invention will be described in detail below by way of examples. In the following examples, unless otherwise specified, the instruments, reagents, materials and the like referred to are conventional instruments, reagents, materials and the like, and are commercially available. Wherein, unless otherwise indicated, all reagents used were commercially available analytically pure products.
Perfluorinated compounds:
perfluoro hexanone: purchased from the company of Hemsleyak, inc. under the trade name FK-5-1-12.
Perfluorobutane: CAS number 355-25-9.
Halogenated olefins:
olefin I: 2-bromo-3, 3-trifluoropropene was purchased from Zhongshan chemical company under the designation CSSC-FA.
Olefin II: 2-chloro-3, 3-trifluoropropene, available from 3M company under CAS number 2730-62-3.
Polar flame retardant compound:
Pentafluoro (phenoxy) cyclotriphosphazene available from Whank biomedical technologies Co., ltd., CAS number 33027-68-8.
Nonpolar flame retardant compounds:
hexachlorobenzene, available from Hubei Korea chemical Co., ltd., CAS number 118-74-1.
Solubilizer:
the perfluoro polyether based surfactant has CAS number 107852-51-7.
Sodium dodecyl sulfonate, available from Shandong Ming chemical company under the trade designation K12.
In the following examples of the invention, different raw material formulations were used, the raw materials were used in parts by weight and each part by weight represents 100g unless otherwise specified.
Example 1
This example illustrates the formulation of the fire extinguishing agent composition of the present invention according to Table 1, and the fire extinguishing agent is prepared as follows.
The method for preparing the fire extinguishing agent comprises the following steps:
Mixing a perfluorinated compound, halogenated olefins (olefins I and II), a polar flame retardant compound and a solubilizer to obtain a fire extinguishing agent;
mixing conditions: the temperature was 20 ℃.
Example 2
This example was performed in a similar manner to example 1, except that the formulation was different, with specific reference to table 1.
Example 3
This example was performed in a similar manner to example 1, except that the formulation was different, with specific reference to table 1.
Example 4
This example was conducted in a similar manner to example 1 except that the perfluoropolyether-based surfactant of example 1 was replaced with equal parts by weight of sodium dodecyl sulfate, and the remainder was conducted in the same manner as in example 1 to obtain a fire extinguishing agent, see specifically Table 1.
Comparative example 1
This comparative example was carried out in a similar manner to example 1, except that the formulation was different, with the formulation being specifically referred to in Table 1.
Comparative example 2
This comparative example was carried out in a similar manner to example 1, except that the formulation was different, with the formulation being specifically referred to in Table 1.
Comparative example 3
This comparative example was carried out in a similar manner to example 1, except that the formulation was different, with the formulation being specifically referred to in Table 1.
Comparative example 4
This comparative example was conducted in a similar manner to example 1 except that the present example was conducted by substituting equal parts by weight of hexachlorobenzene for the pentafluoro (phenoxy) cyclotriphosphazene in example 1, and the remaining same as example 1, to obtain a fire extinguishing agent.
Comparative example 5
This comparative example was carried out in a similar manner to example 1, except that the formulation was different, with the formulation being specifically referred to in Table 1.
Comparative example 6
This comparative example was carried out in a similar manner to example 1, except that the formulation was different, with the formulation being specifically referred to in Table 1.
TABLE 1
Table 1, below
Test case
The fire disaster of the 280Ah energy storage lithium iron phosphate battery compartment is simulated, and the fire extinguishing performance test is carried out on the fire extinguishing agent prepared in the example by adopting the energy storage lithium ion battery fluorine-based high-efficiency safe fire extinguishing system shown in figure 2.
The energy storage lithium ion battery fluorine-based high-efficiency safe fire extinguishing system in fig. 2 comprises: a thermal runaway monitoring module, a control module, a fire extinguishing agent conveying pipeline, and an atomizing nozzle arranged at the periphery of each energy storage battery pack (illustratively, the energy storage battery packs comprise an energy storage battery pack 1, an energy storage battery pack 2, an energy storage battery pack 3, an energy storage battery pack 4 and … … and an energy storage battery pack X, wherein X is equal to 4); the fire extinguishing module comprises a fire extinguishing agent and a storage component; the storage component comprises a fire extinguishing agent storage tank (the fire extinguishing agent storage pressure is 4MPa, and the pressure source is nitrogen) and a control valve for controlling the fire extinguishing agent storage tank; the fire extinguishing agent conveying pipeline comprises a main pipeline and a branch pipeline; the thermal runaway monitoring module and the fluorine-based efficient safe fire extinguishing module are respectively connected with the control module; the fire extinguishing agent holding vessel with the entry of trunk line links to each other, the export of trunk line with each the entry of branch pipeline links to each other, each the export of branch pipeline with atomizing nozzle links to each other.
The fire extinguishing performance test specifically comprises the following steps:
(1) The energy storage battery cabin is internally provided with 16 energy storage battery packs connected in series, and the energy storage batteries Bao Re are triggered to run away in a heating mode (the size of a heating plate is 135mm multiplied by 220mm multiplied by 2mm, and the rated power is 900W); when the energy storage battery pack has thermal runaway smoke, the electronic igniter is used for ignition (the ignition energy of the electronic igniter is 20J, the ignition is performed in a pulse ignition mode, the time of one pulse ignition is 10ms, the interval is 10ms, and the electronic igniter is positioned 3cm above the battery safety valve);
(2) When a fire signal occurs in the energy storage battery compartment, the thermal runaway monitoring module determines the position of the fire, and the control valve of the fire extinguishing agent storage tank is opened through the control module, so that the fire extinguishing agent reaches the atomizing nozzle through the fire extinguishing agent conveying pipeline, and the fire extinguishing agent is sprayed to extinguish the fire.
In the fire extinguishing process, simultaneously testing the fire extinguishing time, the peak value of HF content in the fire extinguishing process and whether the electrolyte white fog in the battery module can be ignited;
The test method for whether the electrolyte white fog can be ignited is as follows:
after the fire disaster of the energy storage lithium iron phosphate battery compartment is extinguished, the electronic igniter is used for igniting the white fog above the battery to evaluate whether the white fog can be ignited or not (the ignition energy of the electronic igniter is 20J, the ignition is performed in a pulse ignition mode, the time of one pulse ignition is 10ms, the interval is 10ms, and the electronic igniter is positioned 3cm above a battery safety valve);
The fire extinguishing effect of the fire extinguishing agent prepared in the above example on the energy storage lithium ion battery is shown in table 2.
TABLE 2
| Fire extinguishing agent source | Extinguishing time/s | HF content/ppm | Whether or not the electrolyte mist is flammable |
| Example 1 | 2.5 | ＜200 | Whether or not |
| Example 2 | 3 | 245 | Whether or not |
| Example 3 | 4 | 210 | Whether or not |
| Example 4 | 3 | 280 | Whether or not |
| Comparative example 1 | 3.5 | 1520 | Whether or not |
| Comparative example 2 | 3 | 249 | Ignitable |
| Comparative example 3 | 3 | 1020 | Ignitable |
| Comparative example 4 | 4 | 320 | Ignitable |
| Comparative example 5 | 8 | 600 | Ignitable |
| Comparative example 6 | 7 | 300 | Ignitable |
As can be seen from the results in Table 2, the fire extinguishing agent provided by the invention is applied to the fluorine-based high-efficiency safe fire extinguishing system of the energy storage lithium ion battery, can obviously reduce the content of toxic gas generated in the fire extinguishing process while improving the fire extinguishing efficiency, and can effectively prevent the smoke of the electrolyte from re-burning.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
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