Low-energy-consumption environment-friendly lithium battery passivation fire extinguishing agent and preparation method thereof
By adding special silicon surfactant to the lithium battery fire extinguishing agent, the complex and difficult problem of lithium battery fire is solved, rapid extinguishing and flame suppression are achieved, and environmental protection and energy-saving requirements are met.
Patent Information
- Application Number
- CN202510305350.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-14
- Publication Date
- 2025-06-06
- Estimated Expiration
- 2045-03-14
AI Technical Summary
Lithium battery fires are complex and difficult to effectively extinguish. Existing fire extinguishing agents are difficult to enter the lithium battery, resulting in rekindling and thermal runaway propagation, and environmental protection and energy consumption problems.
A low-energy-consuming and environmentally friendly lithium battery passivation fire extinguishing agent is adopted. By adding a special silicon surfactant, the agent has good adhesion and isolation, and can adhere to the surface and interior of the lithium battery, quickly extinguish open flames, and has good flame retardancy to inhibit combustion and flame propagation.
It has achieved rapid extinguishing of lithium battery fires and suppressed flame propagation, reduced the risk of rekindling, and met environmental protection and energy-saving requirements, and is suitable for various types of fires.
Smart Images

Figure CN120094157A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of fire protection engineering, and specifically relates to a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent and a preparation method thereof. Background Art
[0002] Lithium batteries are generally batteries with lithium alloy metal oxide as the positive electrode material, graphite as the negative electrode material, and non-aqueous electrolyte. They have high energy density, large capacity, and long cycle life, and are widely used in new energy vehicles and energy storage fields. However, lithium battery fires have occurred frequently in recent years. The reason is that lithium batteries are abused by heat during long-term use, which leads to thermal runaway of the battery. In particular, when lithium batteries are overheated, short-circuited, and squeezed, the imbalance of heat generation and heat dissipation will induce side reactions of the electrode materials and electrolytes inside the battery, produce a large amount of flammable and toxic gases, and release heat. Once an ignition source is encountered, it will cause a fire or even an explosion, seriously endangering people’s lives and property.
[0003] Lithium battery fires are very complex and special. They include gas fires, liquid fires, solid fires, and electrical fires. Some materials can release oxygen at high temperatures to support combustion. In addition, since it is difficult for fire extinguishing agents to enter the lithium battery casing and the internal thermal runaway reaction continues, it is easy for re-ignition and thermal runaway propagation to occur even after the use of fire extinguishing agents. Therefore, fire extinguishing work is very arduous and challenging. In recent years, the existing technology uses fine water mist, water spray, etc. to extinguish lithium battery fires, but the effect is not ideal. After the open fire is extinguished, the lithium battery will re-ignite, and it is impossible to effectively suppress the thermal runaway propagation between battery packs.
[0004] Through the study of thermal runaway of lithium batteries, it was found that lithium battery fires are not simple electrical fires, but involve three types of fire: A, B, and C. Among them, Class A fires are mainly caused by the combustion of solid objects such as battery shells caused by external thermal radiation or self-heating; Class B fires are mainly caused by the occurrence of thermal runaway of the battery, the internal temperature gradually rises, the pressure increases, and the battery pressure relief valve opens, and the electrolyte sprays out, causing a liquid jet fire; Class C fires are caused by the high temperature, and part of the electrolyte, negative electrode materials, and positive electrode materials are decomposed by heat to produce gas, which is also ejected from the pressure relief valve to form a premixed combustion, so it is difficult for general fire extinguishing agents to effectively extinguish fires. In addition, as the country continues to strengthen strict control over environmental protection and pays attention to environmental protection, energy conservation, and emission reduction, a low-energy and environmentally friendly lithium battery passivation fire extinguishing agent and its preparation method are urgently needed. Summary of the invention
[0005] In order to solve the deficiencies mentioned in the above background technology, the purpose of the present invention is to provide a low-energy and environmentally friendly lithium battery passivation fire extinguishing agent and a preparation method thereof. The special silicon surfactant added in the present invention has good adhesion and isolation properties, can adhere to the surface and inside of the lithium battery, and then quickly extinguish the open flame. At the same time, it has good flame retardancy, can inhibit combustion, and prevent the spread of flames.
[0006] The purpose of the present invention can be achieved through the following technical solutions: A low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent, which is composed of the following raw material components by weight ratio: 10-15% penetrant, 25-35% passivator, 10-15% impedance agent, 35-55% composite cooling agent, 0.5-2% hydrocarbon surfactant, 0.1-1% special silicon surfactant, and the rest is deionized water; The special silicon surfactant is prepared by a silylation reaction between a maltose powder-modified organosilicon intermediate and an organic ammonium salt type fluorocarbon surfactant; the maltose powder-modified organosilicon intermediate is prepared by a silylation reaction between tetramethyldisiloxane and an allyl glycidyl ether molecule, followed by a ring-opening reaction with maltose powder; the organic ammonium salt type fluorocarbon surfactant is prepared by a nucleophilic substitution reaction between N,N-dimethyl-1,3-diaminopropane and perfluorobutylsulfonyl fluoride, followed by a quaternization treatment with 3-bromopropylene.
[0007] Preferably, the preparation method of the special silicon surfactant comprises the following steps: A. Tetramethyldisiloxane, allyl glycidyl ether and isopropanol are placed in a reactor, ultrasonically mixed, nitrogen is introduced, the temperature is raised to 80-90°C, 0.002-0.005% of chloroplatinic acid catalyst is added, the reaction is carried out at a constant temperature for 3-5 hours, and then the isopropanol and unreacted products are removed by reduced pressure distillation to prepare an organosilicon intermediate; B. Put the organosilicon intermediate, N,N-dimethylformamide and isopropanol in a reactor, mix them evenly by ultrasonication, then add maltose powder, deionized water and sodium hydroxide, stir for 0.5-1h, then heat to 85-95°C, and react at constant temperature for 4-5h. After the reaction is completed, adjust the pH value of the system to neutral, then remove isopropanol and unreacted substances by vacuum distillation to prepare a maltose powder modified organosilicon intermediate; C. Place N,N-dimethyl-1,3-diaminopropane, triethylamine and dichloromethane in a reactor, pass nitrogen gas through the reactor, add perfluorobutylsulfonyl fluoride in an ice bath, stir and react at 25-30°C for 5-6 hours to prepare a fluorocarbon surfactant; D. Take 3-bromopropylene and anhydrous ethanol in a reactor, react with nitrogen, heat to 40-45°C, add fluorocarbon surfactant, stir and react for 1-2h, heat to 50-55°C, continue constant temperature reaction for 6-8h, and remove anhydrous ethanol and unreacted products by vacuum distillation after the reaction is completed to prepare an organic ammonium salt type fluorocarbon surfactant; E. Place an organic ammonium salt type fluorocarbon surfactant, isopropanol, maltose powder modified organosilicon intermediate and chloroplatinic acid in a reactor, introduce nitrogen into the reaction, stir and mix evenly, raise the temperature to 85-100°C, and react for 6-8 hours. After the reaction is completed, remove isopropanol and unreacted products by vacuum distillation to prepare a special silicone surfactant.
[0008] Preferably, the molar ratio of tetramethyldisiloxane to allyl glycidyl ether in step A is 1:1-1.2; and the molar ratio of the organosilicon intermediate to maltose powder in step B is 1:1-1.7.
[0009] Preferably, in step D, the molar ratio of 3-bromopropylene to the fluorocarbon surfactant is 1-1.2:1; and in step E, the molar ratio of the organic ammonium salt type fluorocarbon surfactant to the maltose powder modified organosilicon intermediate is 1-1.2:1.
[0010] Preferably, the penetrant is formed by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5-1.
[0011] Preferably, the passivating agent is one or more combinations of magnesium oxide, magnesium carbonate, potassium carbonate, basic magnesium carbonate, sodium carbonate, strontium carbonate and calcium carbonate; the resisting agent is one or more combinations of aluminum oxide, silicon dioxide, boron nitride, silicon carbide and titanium dioxide.
[0012] Preferably, the composite cooling agent is a mixture of sodium chloride and ethylene glycol in a mass ratio of 1:1-2; and the hydrocarbon surfactant is cocoamide.
[0013] Preferably, the conductivity of the deionized water is lower than 50 us / cm.
[0014] A method for preparing a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent comprises the following steps: S1. Weigh each raw material component according to the weight ratio, put the penetrant, passivator, impedance agent and composite cooling agent into a reaction kettle, stir and mix to form a composite; S2. Add hydrocarbon surfactant, special silicon surfactant and deionized water to the composite in sequence, stir and mix evenly, and let stand at room temperature for 2-3 hours to obtain a pre-finished product; S3. The pre-finished product is allowed to settle for 10 days and is shipped out after being qualified, thereby preparing a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent.
[0015] Preferably, in step S1, the stirring speed is set to 30-50 r / min, the temperature is set to 15-40°C, and the stirring time is set to 30 min; in step S2, the stirring speed is set to 45-50 r / min, the temperature is set to 15-40°C, and the stirring time is set to 60 min.
[0016] Beneficial effects of the present invention: The invention uses tetramethyl disiloxane and an allyl glycidyl ether molecule to undergo a silylation reaction to prepare an organosilicon intermediate, and then the epoxy group in the structure of the organosilicon intermediate and the hydroxyl group in the structure of maltose powder undergo a ring-opening reaction to prepare the maltose powder modified organosilicon intermediate. At the same time, the invention uses the amino group in the structure of N,N-dimethyl-1,3-diaminopropane and the sulfonyl fluoride group in the structure of perfluorobutylsulfonyl fluoride to undergo a nucleophilic substitution reaction to prepare a fluorocarbon surfactant, and then uses the fluorocarbon surfactant as a raw material and uses 3-bromopropylene to perform a quaternization treatment on the fluorocarbon surfactant to prepare an organic ammonium salt type fluorocarbon surfactant, and then the double bond group introduced in the structure of the organic ammonium salt type fluorocarbon surfactant is reacted with the maltose powder modified organosilicon intermediate. The ungrafted silicon-hydrogen bonds in the body structure further undergo silicon-hydrogen addition reaction to prepare a special silicon surfactant, which contains hydrophilic maltose powder and hydrophobic fluorine-containing long chains in its structure, and can be better adsorbed on the surface of the passivator or impedance agent, so that the particles are evenly dispersed in the system, and the physical stability of the fire extinguishing agent is improved. In addition, the special silicon surfactant has a branched carbon chain structure, which can increase the steric hindrance of the molecule, make the molecule more compact when adsorbed on the interface, and improve its surface activity. At the same time, the longer fluorocarbon chain and organosilicon increase the hydrophobicity of the molecule, and can form a more stable protective film in the fire extinguishing agent, improving the effect of suppressing flames. The introduced ether bond increases the flexibility of the molecule and can change the surface activity of the molecule at the same time, thereby adjusting its interfacial activity and the effect of suppressing flames in the fire extinguishing agent. The special silicon surfactant added by the present invention has good adhesion and isolation, can adhere to the surface and inside of the lithium battery, and then quickly extinguish the open flame. At the same time, it has good flame retardancy, can suppress combustion, and prevent the spread of flames.
[0017] The penetrant and passivator added in the present invention are conducive to slowing down and terminating the electrochemical reaction of the lithium battery, the impedance agent blocks the electron movement rate, so that the current is reduced and the thermal efficiency is further reduced, and the composite cooling agent added in addition reduces the battery thermochemical energy, further reducing the occurrence of battery fire. The fire extinguishing agent prepared by the present invention has practicality and versatility, a wide range of applications, and is suitable for various types of fires. In the production process, the production cycle is short, the required energy consumption is low, the storage and transportation are convenient, the stability is good, and the effective use period can reach 5 years. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0019] Figure 1 It is a schematic diagram of the process flow of the low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent of the present invention. DETAILED DESCRIPTION
[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0021] Example 1 A method for preparing a special silicon surfactant comprises the following steps: A. 3.4 g of tetramethyldisiloxane, 3.4 g of allyl glycidyl ether and 50 mL of 30% isopropanol solution were placed in a reactor, ultrasonically mixed, nitrogen was introduced, the temperature was raised to 85° C., 0.003% of chloroplatinic acid catalyst was added, the reaction was carried out at a constant temperature for 4 h, and then the isopropanol and unreacted products were removed by reduced pressure distillation to prepare an organosilicon intermediate; B. 5.2 g of the organosilicon intermediate, 10 mL of N,N-dimethylformamide and 30 mL of isopropanol were placed in a reactor and mixed evenly by ultrasonication. Then, 9 g of maltose powder, 40 mL of deionized water and 0.3 g of sodium hydroxide were added. After stirring for 0.5 h, the temperature was raised to 90° C. and the reaction was carried out at a constant temperature for 4 h. After the reaction was completed, a cationic resin was added to adjust the pH value of the system to neutral. The resin in the solution was removed by suction filtration, and then the isopropanol and unreacted products were removed by reduced pressure distillation to prepare a maltose powder-modified organosilicon intermediate; C. Take 5.1 g of N,N-dimethyl-1,3-diaminopropane, 5.1 g of triethylamine and 40 mL of dichloromethane in a reactor, pass nitrogen gas through the reaction, add 9.1 g of perfluorobutylsulfonyl fluoride in an ice bath, stir and react at 25°C for 6 hours to prepare a fluorocarbon surfactant; D. Take 6.5g of 3-bromopropylene and 50mL of anhydrous ethanol in a reactor, pass nitrogen gas through the reaction, heat to 45°C, add 19.2g of fluorocarbon surfactant, stir and react for 1h, heat to 55°C, continue constant temperature reaction for 8h, and after the reaction is completed, remove anhydrous ethanol and unreacted products by vacuum distillation to prepare an organic ammonium salt type fluorocarbon surfactant; E. Take 12.6g of organic ammonium salt type fluorocarbon surfactant, 50mL of isopropanol, 15.2g of maltose powder modified organosilicon intermediate and 25μL of chloroplatinic acid in a reactor, pass nitrogen gas through the reaction, stir and mix evenly, raise the temperature to 100℃, react for 7h, and after the reaction is completed, remove isopropanol and unreacted products by reduced pressure distillation to prepare a special silicone surfactant.
[0022] Example 2 A low-energy, environmentally friendly lithium battery passivation fire extinguishing agent is composed of the following raw material components by weight ratio: 13.6% penetrant, 25.7% passivator magnesium carbonate, 10.1% impedance agent silicon dioxide, 50% composite cooling agent, 1.8% hydrocarbon surfactant cocamide, 0.9% special silicon surfactant prepared in Example 1, and the rest is deionized water; wherein the penetrant is formed by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5, and the composite cooling agent is formed by mixing sodium chloride and ethylene glycol in a mass ratio of 1:1.
[0023] The preparation method of the low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent comprises the following steps: S1. Weigh each raw material component according to the weight ratio, put the penetrant, passivator, impedance agent and composite cooling agent into a reaction kettle, stir and mix, set the stirring speed to 30r / min, the temperature to 20°C, and the stirring time to 30min to form a composite; S2. Add hydrocarbon surfactant, special silicon surfactant and deionized water to the composite in sequence, stir and mix evenly, set the stirring speed to 45r / min, the temperature to 30°C, the stirring time to 60min, and let stand at room temperature for 2h to obtain a pre-finished product; S3. The pre-finished product is allowed to settle for 10 days and is shipped out after being qualified, thereby preparing a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent.
[0024] Example 3 A low-energy, environmentally friendly lithium battery passivation fire extinguishing agent is composed of the following raw material components by weight ratio: 11.7% of penetrant, 28.8% of passivator magnesium carbonate, 14.4% of impedance agent silicon dioxide, 45.2% of composite cooling agent, 1.6% of hydrocarbon surfactant cocamide, 0.5% of special silicon surfactant prepared in Example 1, and the rest is deionized water; wherein the penetrant is formed by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5, and the composite cooling agent is formed by mixing sodium chloride and ethylene glycol in a mass ratio of 1:1.
[0025] The preparation method of the above-mentioned low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent is the same as that of Example 2.
[0026] Example 4 A low-energy, environmentally friendly lithium battery passivation fire extinguishing agent is composed of the following raw material components by weight ratio: 14.5% penetrant, 32.8% passivator magnesium carbonate, 12.6% impedance agent silicon dioxide, 37.9% composite cooling agent, 0.7% hydrocarbon surfactant cocamide, 1% special silicon surfactant prepared in Example 1, and the rest is deionized water; wherein the penetrant is formed by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5, and the composite cooling agent is formed by mixing sodium chloride and ethylene glycol in a mass ratio of 1:1.
[0027] The preparation method of the above-mentioned low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent is the same as that of Example 2.
[0028] Comparative Example 1 A method for preparing an organic ammonium salt type fluorocarbon surfactant comprises the following steps: A. Take 5.1 g of N,N-dimethyl-1,3-diaminopropane, 5.1 g of triethylamine and 40 mL of dichloromethane in a reactor, pass nitrogen gas through the reaction, add 9.1 g of perfluorobutylsulfonyl fluoride in an ice bath, stir and react at 25°C for 6 hours to prepare a fluorocarbon surfactant; B. Take 6.5g of 3-bromopropylene and 50mL of anhydrous ethanol in a reactor, pass nitrogen through the reaction, heat up to 45°C, add 19.2g of fluorocarbon surfactant, stir and react for 1h, heat up to 55°C, continue constant temperature reaction for 8h, and after the reaction is completed, remove anhydrous ethanol and unreacted products by reduced pressure distillation to prepare an organic ammonium salt type fluorocarbon surfactant.
[0029] Comparative Example 2 A low-energy, environmentally friendly lithium battery passivation fire extinguishing agent is composed of the following raw material components by weight ratio: 13.6% penetrant, 25.7% passivator magnesium carbonate, 10.1% impedance agent silicon dioxide, 50% composite cooling agent, 1.8% hydrocarbon surfactant cocamide, 0.9% organic ammonium salt type fluorocarbon surfactant prepared in Comparative Example 1, and the rest is deionized water; wherein the penetrant is formed by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5, and the composite cooling agent is formed by mixing sodium chloride and ethylene glycol in a mass ratio of 1:1.
[0030] The preparation method of the low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent comprises the following steps: S1. Weigh each raw material component according to the weight ratio, put the penetrant, passivator, impedance agent and composite cooling agent into a reaction kettle, stir and mix, set the stirring speed to 30r / min, the temperature to 20°C, and the stirring time to 30min to form a composite; S2. Add hydrocarbon surfactant, organic ammonium salt type fluorocarbon surfactant and deionized water to the composite in sequence, stir and mix evenly, set the stirring speed to 45r / min, the temperature to 30°C, the stirring time to 60min, and let stand at room temperature for 2h to obtain a pre-finished product; S3. The pre-finished product is allowed to settle for 10 days and is shipped out after being qualified, thereby preparing a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent.
[0031] Performance Testing The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent prepared in Example 2 was subjected to performance testing in accordance with GB 15308-2006, and the data results are shown in Table 1.
[0032] Table 1 Test results of fire extinguishing agent performance prepared in Example 2
[0033] It can be seen from the data in Table 1 that the fire extinguishing agent prepared by the present invention is suitable for extinguishing a variety of fires, including Class A and Class B, especially alcohol gasoline fires, and is more practical than foam fire extinguishing agents on the market.
[0034] The low-energy and environmentally friendly lithium battery passivation fire extinguishing agents prepared in Examples 2-4 and Comparative Example 2 were tested for fire extinguishing performance. The ternary lithium battery was charged to a battery state of charge ≥ 100%, and placed on a fire extinguishing plate in an explosion test box. Two thermocouples were arranged on the upper and lower surfaces of the lithium battery, respectively. The fire extinguishing agent was sprayed onto the lithium battery through a water mist nozzle on the upper part of the explosion test box. The nozzle was an ordinary foam type nozzle with an aperture of 5.8 mm and a flow rate of 0.06 L / s. The main nozzle and the spare nozzle were 52.44 cm away from the upper surface of the lithium battery, respectively. The heating device was a 3kW electric furnace at the bottom of the lithium battery. The data results are shown in Table 2.
[0035] Table 2 Test results of sample fire extinguishing performance
[0036] It can be seen from the data in Table 2 that the fire extinguishing agent prepared in Examples 2-4 of the present invention can extinguish an open flame within 8 seconds, and the cooling rate of the lower surface temperature of the lithium battery from the beginning of spraying the fire extinguishing agent to 95°C is faster than that of Comparative Example 2. The fire extinguishing agent is sprayed again to continue cooling. The total amount of the fire extinguishing agent is about 3.4 kg, which can effectively extinguish the open flame generated by thermal runaway of the lithium battery and curb the development and spread of the fire.
[0037] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0038] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.
Claims
1. A low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent, characterized in that: The composition is composed of the following raw material components by weight ratio: penetrant 10~15%, passivator 25~35%, impedance agent 10~15%, composite cooling agent 35~55%, hydrocarbon surfactant 0.5~2%, special silicon surfactant 0.1~1%, and the rest is deionized water; The special silicon surfactant is prepared by a silylation reaction between a maltose powder-modified organosilicon intermediate and an organic ammonium salt type fluorocarbon surfactant; the maltose powder-modified organosilicon intermediate is prepared by a silylation reaction between tetramethyldisiloxane and an allyl glycidyl ether molecule, followed by a ring-opening reaction with maltose powder; the organic ammonium salt type fluorocarbon surfactant is prepared by a nucleophilic substitution reaction between N,N-dimethyl-1,3-diaminopropane and perfluorobutylsulfonyl fluoride, followed by a quaternization treatment with 3-bromopropylene.
2. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 1 is characterized in that: The preparation method of the special silicon surfactant comprises the following steps: A. Tetramethyldisiloxane, allyl glycidyl ether and isopropanol are placed in a reactor, ultrasonically mixed, nitrogen is introduced, the temperature is raised to 80-90°C, 0.002-0.005% of chloroplatinic acid catalyst is added, the reaction is carried out at a constant temperature for 3-5 hours, and then the isopropanol and unreacted products are removed by reduced pressure distillation to prepare an organosilicon intermediate; B. Put the organosilicon intermediate, N,N-dimethylformamide and isopropanol in a reactor, mix them evenly by ultrasonication, then add maltose powder, deionized water and sodium hydroxide, stir for 0.5-1h, then heat to 85-95°C, and react at constant temperature for 4-5h. After the reaction is completed, adjust the pH value of the system to neutral, then remove isopropanol and unreacted substances by vacuum distillation to prepare a maltose powder modified organosilicon intermediate; C. Place N,N-dimethyl-1,3-diaminopropane, triethylamine and dichloromethane in a reactor, pass nitrogen gas through the reactor, add perfluorobutylsulfonyl fluoride in an ice bath, stir and react at 25-30°C for 5-6 hours to prepare a fluorocarbon surfactant; D. Take 3-bromopropylene and anhydrous ethanol in a reactor, react with nitrogen, heat to 40-45°C, add fluorocarbon surfactant, stir and react for 1-2h, heat to 50-55°C, continue constant temperature reaction for 6-8h, and remove anhydrous ethanol and unreacted products by vacuum distillation after the reaction is completed to prepare an organic ammonium salt type fluorocarbon surfactant; E. Place an organic ammonium salt type fluorocarbon surfactant, isopropanol, maltose powder modified organosilicon intermediate and chloroplatinic acid in a reactor, introduce nitrogen into the reaction, stir and mix evenly, raise the temperature to 85-100°C, and react for 6-8 hours. After the reaction is completed, remove isopropanol and unreacted products by vacuum distillation to prepare a special silicone surfactant.
3. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 2 is characterized in that: The molar ratio of tetramethyldisiloxane to allyl glycidyl ether in step A is 1:1-1.2; the molar ratio of the organosilicon intermediate to maltose powder in step B is 1:1-1.
7.
4. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 2 is characterized in that: The molar ratio of 3-bromopropylene to the fluorocarbon surfactant in step D is 1-1.2:1; the molar ratio of the organic ammonium salt type fluorocarbon surfactant to the maltose powder modified organosilicon intermediate in step E is 1-1.2:
1.
5. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 1 is characterized in that: The penetrant is prepared by mixing perfluorohexanone and polydimethylsiloxane in a mass ratio of 1:0.5-1.
6. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 1 is characterized in that: The passivating agent is one or more combinations of magnesium oxide, magnesium carbonate, potassium carbonate, basic magnesium carbonate, sodium carbonate, strontium carbonate and calcium carbonate; the impedance agent is one or more combinations of aluminum oxide, silicon dioxide, boron nitride, silicon carbide and titanium dioxide.
7. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 1 is characterized in that: The composite cooling agent is a mixture of sodium chloride and ethylene glycol in a mass ratio of 1:1-2; and the hydrocarbon surfactant is cocoamide.
8. The low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 1 is characterized in that: The conductivity of the deionized water is lower than 50 us / cm.
9. The method for preparing the low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1. Weigh each raw material component according to the weight ratio, put the penetrant, passivator, impedance agent and composite cooling agent into a reaction kettle, stir and mix to form a composite; S2. Add hydrocarbon surfactant, special silicon surfactant and deionized water to the composite in sequence, stir and mix evenly, and let stand at room temperature for 2-3 hours to obtain a pre-finished product; S3. The pre-finished product is allowed to settle for 10 days and is shipped out after being qualified, thereby preparing a low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent.
10. The method for preparing the low-energy consumption and environmentally friendly lithium battery passivation fire extinguishing agent according to claim 9, characterized in that: In step S1, the stirring speed is set to 30-50 r / min, the temperature is set to 15-40°C, and the stirring time is set to 30 min; in step S2, the stirring speed is set to 45-50 r / min, the temperature is set to 15-40°C, and the stirring time is set to 60 min.
Citation Information
Patent Citations
Vitamin K1 orally disintegrating tablets preparation and preparation method thereof
CN101120928A
Quaternary ammonium salt fluorinated polysiloxane cationic surfactant and synthesis method thereof
CN109261069A
Environment-friendly lithium battery fire extinguishing agent and preparation method and application thereof
CN114177564A
Aluminum silicate gel fire extinguishing agent for lithium battery fire and preparation method of aluminum silicate gel fire extinguishing agent
CN119499602A
Method for forming functional layers
US20060246291A1