CN112386856B - Preparation method of core-shell type cooling flame-retardant lithium battery extinguishing agent - Google Patents
Preparation method of core-shell type cooling flame-retardant lithium battery extinguishing agent Download PDFInfo
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- A—HUMAN NECESSITIES
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- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
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Abstract
The invention discloses a preparation method of a core-shell type cooling and flame-retardant lithium battery fire extinguishing agent, which relates to the technical field of lithium battery fire extinguishing agent preparation and comprises the following preparation steps: 1) dissolving a coating agent in pyrrolidone to prepare a coating solution; 2) dispersing perfluorohexanone in the coating solution through spraying, and stirring to prepare a mixed solution after spraying is finished; 3) heating and curing the mixed solution, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent; the fire extinguishing agent with the core-shell structure is prepared by coating the perfluorohexanone with the coating agent and combining the flame retardance of the shell material and the cooling function of the core material, so that the fire extinguishing agent with the dual functions of cooling and fire extinguishing can effectively prevent the fire of the lithium battery, can quickly reduce the temperature of the battery, can effectively inhibit secondary or repeated re-combustion of the fire of the lithium battery, and is suitable for extinguishing the fire of the lithium battery.
Description
Technical Field
The invention relates to the technical field of preparation of lithium battery extinguishing agents, in particular to a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent.
Background
The lithium battery energy storage is more and more emphasized by the energy storage field due to flexibility, simplicity and convenience and large volumetric specific energy density, and the application range of the lithium battery energy storage is increasingly common. However, the recent frequent fire hazard of lithium batteries at home and abroad arouses the wide worry of people about the energy storage safety of the lithium batteries. The existing fire extinguishing agent adopted for lithium battery fire is gas, such as heptafluoropropane, and the fire extinguishing agent can only block general electrical fire, cannot effectively inhibit secondary or repeated re-combustion of lithium battery fire, does not have the dual functions of cooling and fire extinguishing, and does not have applicability to lithium battery fire. Therefore, specific fire extinguishing agents must be developed for fire fighting of lithium batteries, especially large energy storage lithium batteries.
For example, a "heptafluoropropane-based high-efficiency fire extinguishing agent" disclosed in chinese patent literature, which publication No. CN106621158A, discloses a heptafluoropropane-based high-efficiency fire extinguishing agent comprising, in terms of weight percent, as raw materials: 35-45% of heptafluoropropane, 10-14% of dry ice, 6-10% of sodium dihydrogen phosphate, 8-12% of sodium carbonate, 6-10% of sodium acetate trihydrate, 8-12% of sodium chloride, 1-3% of carbamide and 8-12% of water. However, the fire extinguishing agent can block general electrical fires, cannot effectively inhibit secondary or repeated afterburning of lithium battery fires, does not have the dual functions of cooling and extinguishing fires, and does not have applicability to lithium battery fires.
Disclosure of Invention
The invention provides a preparation method of a core-shell type cooling and flame-retardant lithium battery extinguishing agent, aiming at solving the problems that the existing gas extinguishing agent can only block general electric fires, can not effectively inhibit secondary or repeated re-combustion of lithium battery fires, does not have double functions of cooling and extinguishing fires, and does not have applicability to the fires of lithium batteries.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in pyrrolidone for reaction to prepare a coating solution;
(2) dispersing perfluorohexanone in the coating solution through spraying, and stirring to prepare a mixed solution after spraying is finished;
(3) and heating and curing the mixed solution, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
In the preparation process of the lithium battery extinguishing agent, firstly, styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene are dissolved in pyrrolidone for reaction to prepare a coating solution containing a styrene-methyl methacrylate-acrylonitrile-2-bromo-3, 3, 3-trifluoropropene copolymer, perfluorohexanone is dispersed in the coating solution through spraying, and then cured, so that the core-shell type temperature-reducing flame-retardant lithium battery extinguishing agent taking the styrene-methyl methacrylate-acrylonitrile-2-bromo-3, 3, 3-trifluoropropene copolymer as a shell material and the perfluorohexanone as a core material is prepared. In the fire extinguishing agent with the core-shell structure, the shell material can cover the core material fire extinguishing agent, so that the core material fire extinguishing agent can be efficiently and stably stored in the air, and can inhibit and extinguish open fire after high-temperature decomposition; and after the shell material is decomposed at high temperature to obtain the core material perfluorohexanone, the perfluorohexanone can be gasified by absorbing heat at the flame, so that the heat is taken away, and the aim of quickly cooling is fulfilled. The fire extinguishing agent with the core-shell structure is formed by coating the perfluorohexanone with the shell material, and the fire extinguishing agent with the dual functions of temperature reduction and fire extinguishment is prepared by combining the flame retardance of the shell material and the temperature reduction function of the core material, so that the fire extinguishing agent not only can effectively prevent the lithium battery fire, but also can quickly reduce the temperature of the battery, realize the temperature reduction range from 800-30 ℃, effectively prevent the secondary or repeated reburning of the lithium battery fire, and is suitable for extinguishing the fire of the lithium battery.
The shell material coating agent adopted by the invention is styrene-methyl methacrylate-acrylonitrile-2-bromo-3, 3, 3-trifluoropropene, wherein 2-bromo-3, 3, 3-trifluoropropene is a flame retardant, but the 2-bromo-3, 3, 3-trifluoropropene is easy to decompose in the daily environment due to the existence of double bonds and cannot be stored for a long time, and the shell material of the fire extinguishing agent with the core-shell structure not only has the flame retardant performance but also has the 2-bromo-3, 3, 3-trifluoropropene after the 2-bromo-3, 3, 3-trifluoropropene copolymer styrene-methyl methacrylate-acrylonitrile-2-bromo-3, 3, 3-trifluoropropene is grafted on the copolymer to be used as the coating agent, 3, 3-trifluoropropene is not easy to decompose and easy to store, and the prepared core-shell type cooling flame-retardant lithium battery extinguishing agent has stable performance.
Preferably, the molar ratio of the styrene, the methyl methacrylate, the acrylonitrile and the 2-bromo-3, 3, 3-trifluoropropene in the step (1) is 1-1.1:1-1.1:1-1.1:3, and the reaction is carried out for 8-12h at normal temperature;
the 2-bromo-3, 3, 3-trifluoropropene has flame retardance, and has higher compatibility with the perfluorohexanone compared with other monomers, in the monomer proportion, the 2-bromo-3, 3, 3-trifluoropropene is too little, which may cause the flame retardant property of the shell material to be insufficient, and meanwhile, the perfluorohexanone coating cannot be coated due to too low compatibility of the copolymer with the perfluorohexanone; and the structure of the copolymer can be damaged and a stable core-shell structure cannot be formed due to excessive 2-bromo-3, 3, 3-trifluoropropene.
Preferably, the concentration of the coating solution in the step (1) is 5 to 30 wt%.
Preferably, the mass ratio of the perfluorohexanone to the coating solution in the step (2) is 10-12: 1.
The concentration of the coating solution and the proportion of the coating solution to the perfluorohexanone are used for controlling the thickness of the shell material of the core-shell type temperature-reducing flame-retardant lithium battery extinguishing agent, and if the concentration of the coating solution is too low or the using amount of the coating solution is too low, the thickness of the shell material is too low, so that the purposes of stable storage and good flame retardance cannot be achieved; and the concentration of the coating solution is too high or the using amount of the coating solution is too large, the thickness of the shell material is too large, the core material cannot be released in time during fire extinguishing, and the good effect of inhibiting re-combustion cannot be achieved.
Preferably, in the spray dispersion in the step (2), the atomized particle size is 0.1 to 10 μm.
Preferably, the stirring speed is 200-800r/min after the spraying in the step (2) is finished, and the stirring time is 0.5-3 h.
Preferably, the curing and coating temperature in the step (3) is 60-70 ℃, and the curing and coating time is 0.5-1.5 h.
The temperature resistance of the shell material in the core-shell structure fire extinguishing agent is related to the molecular weight of the shell material, the molecular weight of the shell material is related to the curing time, when the shell material is cured for 0.5 to 1.5 hours at the temperature of between 60 and 70 ℃, the molecular weight of the shell material is 120-300MD, and the release temperature of the core material can be set to be more than 80 ℃ for release.
Preferably, the curing and coating temperature in the step (3) is 60-70 ℃, and the curing and coating time is 2-3 h.
When cured at 60-70 ℃ for 2-3h, the molecular weight is 300-500MD, and the release temperature of the core material can be set to be more than 120 ℃.
Setting the release temperature to be 80 ℃ and 120 ℃, which is because the initial temperature of the lithium battery in fire is generally 80 ℃, and in order to extinguish the fire in the early stage, the release temperature needs to be set to be 80 ℃; and because the temperature of the lithium battery can easily reach 80 ℃ in the using process, the release temperature is only set to 80 ℃, and the error spraying is easy, the release temperature also needs to be set to 120 ℃, and the release temperature is released when the thermal runaway of the lithium battery is ensured.
Therefore, the invention has the following beneficial effects: the fire extinguishing agent with the core-shell structure is prepared by coating the perfluorohexanone with the coating agent and combining the flame retardance of the shell material and the cooling function of the core material, so that the fire extinguishing agent with the dual functions of cooling and fire extinguishing can effectively prevent the fire of the lithium battery, can quickly reduce the temperature of the battery, can reduce the temperature from 800-30 ℃, can effectively inhibit secondary or repeated re-combustion of the fire of the lithium battery, and is suitable for extinguishing the fire of the lithium battery.
Drawings
FIG. 1 is a schematic structural diagram of a TEM fire extinguishing agent for a core-shell type cooling and fire-retardant lithium battery in example 1 of the invention.
FIG. 2 is a comparative schematic diagram of a scanning electron microscope before and after the fire extinguishing agent for the core-shell type cooling flame-retardant lithium battery in example 4 of the present invention is applied.
Detailed Description
The invention is further described with reference to specific embodiments.
General example: a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a pyrrolidone in a ratio of 1-1.1:1-1.1:1-1.1:3, placing the mixture in a reaction kettle, and reacting the mixture for 8 to 12 hours at normal temperature to prepare a coating solution with the concentration of 5 to 30 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 10-12:1, the atomized particle size is 0.1-10 mu m during spraying dispersion, and stirring for 0.5-3h at 800r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 60-70 ℃ for 0.5-3h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Example 1: a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 10 hours to prepare a coating solution with the concentration of 10 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 12:1, the atomized particle size is 0.5 mu m during spraying dispersion, and stirring for 1.5h at 600r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 65 ℃ for 0.9h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Example 2: a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1.1:1.1:1.1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 8 hours to prepare a coating solution with the concentration of 30 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 11:1, the atomized particle size is 1 mu m during spraying dispersion, and stirring for 0.5h at 800r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 70 ℃ for 0.5h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Example 3: a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 12 hours to prepare a coating solution with the concentration of 25 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 12:1, the atomized particle size is 8 mu m during spraying dispersion, and stirring for 2 hours at 600r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 70 ℃ for 2.5h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Example 4: a preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 10 hours to prepare a coating solution with the concentration of 30 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 10:1, the atomized particle size is 10 mu m during spraying dispersion, and stirring for 3h at 500r/min after spraying to prepare a mixed solution;
(3) and curing the mixed solution at 70 ℃ for 3h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Comparative example 1: the difference from example 1 is that the concentration of the coating solution is below the defined range
A preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 10 hours to prepare a coating solution with the concentration of 10 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 12:1, the atomized particle size is 0.5 mu m during spraying dispersion, and stirring for 1.5h at 600r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 65 ℃ for 0.8h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Comparative example 2: the difference from example 1 is that the maturation temperature and time are below the limits
A preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 10 hours to prepare a coating solution with the concentration of 10 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 12:1, the atomized particle size is 0.5 mu m during spraying dispersion, and stirring for 1.5h at 600r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 65 ℃ for 0.8h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
Comparative example 3: the difference from example 1 is that the maturation temperature and time are above the defined ranges
A preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent comprises the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in a ratio of 1:1:1:3 in pyrrolidone, placing the mixture in a reaction kettle, and reacting at normal temperature for 10 hours to prepare a coating solution with the concentration of 10 wt%;
(2) dispersing perfluorohexanone in a coating solution by spraying, wherein the mass ratio of the perfluorohexanone to the coating solution is 12:1, the atomized particle size is 0.5 mu m during spraying dispersion, and stirring for 1.5h at 600r/min after spraying to prepare a mixed solution;
(3) curing the mixed solution at 80 ℃ for 4h, and then screening to prepare the core-shell type cooling flame-retardant lithium battery extinguishing agent.
The appearance of the core-shell type cooling and flame-retardant lithium battery extinguishing agent prepared in example 1 is characterized, and the result is shown in fig. 1, which shows that the core-shell type cooling and flame-retardant lithium battery extinguishing agent has a typical core-shell structure.
The appearance characterization of the core-shell type cooling and flame-retardant lithium battery fire extinguishing agent prepared in the embodiment 4 is carried out before and after release, and the result is shown in fig. 2, wherein after the appearance observation of the fire extinguishing agent before and after release is carried out by a scanning electron microscope, the core-shell type cooling and flame-retardant lithium battery fire extinguishing agent is spherical before release, the particle size distribution is uniform, the sphere is broken and pulverized after release, the internal pressure of the fire extinguishing agent in the surface is increased under the action of temperature, and the shell is broken, so that the core material fire extinguishing agent is released.
The application time of the core-shell type cooling and flame-retardant lithium battery extinguishing agent prepared in the examples and the comparative examples is characterized, and the results are shown in the following table.
From the above data, it can be seen that the discharge temperature of examples 1 and 2 is higher than 80 ℃, and the discharge temperature of examples 3 and 4 is higher than 120 ℃, which is suitable for the fire situation of the lithium ion battery under different conditions; the shell materials of the core-shell type cooling and flame-retardant lithium battery fire extinguishing agents prepared in the comparative examples 1 and 2 are thin or low in heat-resistant temperature, so that the discharge temperature is too low, and the shell materials of the core-shell type cooling and flame-retardant lithium battery fire extinguishing agents prepared in the comparative examples 3 are too high in heat-resistant temperature, so that the discharge temperature is too high, and the shell materials are not suitable for the fire condition of the lithium ion battery.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (6)
1. A preparation method of a core-shell type cooling flame-retardant lithium battery extinguishing agent is characterized by comprising the following preparation steps:
(1) dissolving styrene, methyl methacrylate, acrylonitrile and 2-bromo-3, 3, 3-trifluoropropene in pyrrolidone for reaction to prepare a coating solution;
(2) dispersing perfluorohexanone in the coating solution through spraying, and stirring to prepare a mixed solution after spraying is finished;
(3) and heating and curing the mixed solution at 65 ℃ for 0.9h, or heating and curing at 70 ℃ for 0.5h or 2.5-3h, and then screening to prepare the core-shell type cooling and flame-retardant lithium battery extinguishing agent.
2. The preparation method of the core-shell type temperature-reducing flame-retardant lithium battery extinguishing agent according to claim 1, wherein the molar ratio of the styrene, the methyl methacrylate, the acrylonitrile and the 2-bromo-3, 3, 3-trifluoropropene in the step (1) is 1-1.1:1-1.1:1-1.1:3, and the reaction condition is that the reaction is carried out for 8-12 hours at normal temperature.
3. The preparation method of the core-shell type cooling and flame-retardant lithium battery extinguishing agent according to claim 1, wherein the concentration of the coating solution in the step (1) is 5-30 wt%.
4. The preparation method of the core-shell type temperature-reducing flame-retardant lithium battery extinguishing agent according to claim 1, wherein the mass ratio of the perfluorohexanone to the coating solution in the step (2) is 10-12: 1.
5. The method for preparing the core-shell type cooling and flame-retardant lithium battery extinguishing agent according to claim 1, wherein the atomized particle size is 0.1-10 μm during the spray dispersion in the step (2).
6. The method for preparing the core-shell type temperature-reducing flame-retardant lithium battery extinguishing agent as claimed in claim 1, wherein the stirring speed is 200-800r/min after the spraying in the step (2) is finished, and the stirring time is 0.5-3 h.
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| CN102822261A (en) * | 2010-03-26 | 2012-12-12 | 索尔维公司 | Polymer compositions comprising core/shell particles |
| CN110478842A (en) * | 2019-06-28 | 2019-11-22 | 浙江南都电源动力股份有限公司 | Lithium electricity compound fire-extinguishing agent |
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| GB676723A (en) * | 1949-03-30 | 1952-07-30 | British Thomson Houston Co Ltd | Improvements in and relating to copolymers of a diene hydrocarbon and unsaturated fluorinated compounds |
| GB744677A (en) * | 1950-02-20 | 1956-02-15 | British Cellophane Ltd | Improvements in or relating to the production of moistureproof films |
| US3409589A (en) * | 1964-09-02 | 1968-11-05 | Rohm & Haas | Addition copolymers of alkoxy-substituted phenyl esters of acrylic or methacrylic acid |
| CN101417166A (en) * | 2008-11-14 | 2009-04-29 | 中国科学技术大学 | Gas-solid composite powder base fire-extinguishing agent and preparation method thereof |
| CN102822261A (en) * | 2010-03-26 | 2012-12-12 | 索尔维公司 | Polymer compositions comprising core/shell particles |
| CN110478842A (en) * | 2019-06-28 | 2019-11-22 | 浙江南都电源动力股份有限公司 | Lithium electricity compound fire-extinguishing agent |
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