Flame-retardant potting adhesive for lithium battery and preparation method thereof

By preparing flame-retardant nanosheets and spraying boric acid at high temperature to form a boron-oxygen-silicon structure potting compound, the problems of flammability of epoxy resin and low efficiency of HP-RTM process were solved, achieving halogen-free flame retardancy and high-efficiency production.

CN116694278BActive Publication Date: 2026-02-27ANHUI ZHONGBO NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202310701045.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-14
Publication Date
2026-02-27
Estimated Expiration
2043-06-14

AI Technical Summary

Technical Problem

Existing epoxy resin potting materials are flammable and produce toxic fumes and corrosive gases when burned, which limits their application. In addition, the traditional HP-RTM process has requirements on resin viscosity and reaction rate, which affects production efficiency.

Method used

A potting compound containing bisphenol A type epoxy resin, special epoxy, flame-retardant nanosheets, carbon black, and fluoropolymer phosphate is used. Flame-retardant nanosheets are prepared and boric acid is sprayed at high temperature to form a borosilicate structure, which improves the high temperature resistance and flame retardant properties of the material. The viscosity is adjusted by using special epoxy to make it suitable for HP-RTM molding process.

Benefits of technology

It achieves halogen-free flame retardancy, improves the high temperature resistance and mechanical properties of the material, is suitable for HP-RTM molding process, and the resulting composite material reaches UL94-V0 level after curing at 120℃, with a tensile strength of 1.2MPa.

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Abstract

The application discloses a kind of lithium battery with flame-retardant potting adhesive and preparation method thereof, it is related to potting adhesive technical field.The potting adhesive prepared by the application includes component A, component B and component C, when applying, component A, component B, component C are mixed and used according to mass ratio 100:14:1.5;Wherein, component A includes the following raw materials: bisphenol A type epoxy resin, special epoxy, flame-retardant nanosheet, carbon black;The component B includes the following raw materials: triethylene tetramine, polyether amine, alicyclic amine;Component C includes the following raw materials: phosphoric acid fluoro alcohol ester 100 parts.The special epoxy of the application is added to adjust the viscosity of potting adhesive, so that it is suitable for HP-RTM forming process, while adding flame-retardant nanosheet to improve the halogen-free flame-retardant performance and mechanical properties of potting adhesive, with wide application prospect.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of potting glue, in particular to a kind of lithium battery with flame-retardant potting glue and preparation method thereof. BACKGROUND

[0002] Epoxy resin refers to organic high molecular compound containing two or more than two epoxy groups in molecule, which has good dielectric property, mechanical property, bonding property and corrosion resistance, and small curing shrinkage and linear expansion coefficient, and the size of cured product is relatively stable, with excellent comprehensive performance. Because epoxy resin has excellent electrical insulation and operation process, it is widely used in potting field. But the traditional epoxy resin is flammable material, and its limiting oxygen index is only about 19.5, thereby limiting its application.

[0003] At present, halogen-containing polymers or halogen-containing flame retardants are mainly added in epoxy resin to improve its flame-retardant property. However, when fire occurs, such halogen-containing flame-retardant materials will produce a large amount of smoke and toxic corrosive hydrogen halide gas, causing secondary harm. New flame-retardant system has small smoke emission amount and does not produce toxic and corrosive gas when burning. Halogen-free flame-retardant is to add suitable halogen-free flame-retardant into material to achieve this purpose. Halogen-free flame-retardant additives include phosphorus compounds, metal hydroxides, silicon flame retardants, nitrogen flame retardants and other types, which are not volatile and do not produce corrosive gas when burning, and are called nuisance-free flame retardants. HP-RTM (High Pressure Resin Transfer Molding) process technology is a new RTM process technology for mass production of high-performance thermosetting composite parts in recent years, which uses preformed parts, steel mold, vacuum assisted exhaust, high pressure injection and high pressure to complete resin impregnation and curing process, and has obvious advantages in product consistency, air tightness reliability and future cost reduction space. But HP-RTM molding process has requirements for viscosity and reaction speed of matrix resin, and the lower the viscosity and the faster the reaction speed, the faster the production efficiency. SUMMARY

[0004] The present application aims to provide a kind of lithium battery with flame-retardant potting glue and preparation method thereof, to solve the problems in the prior art.

[0005] In order to solve the above technical problems, the present application provides the following technical solutions:

[0006] A kind of lithium battery with flame-retardant potting glue, the lithium battery with flame-retardant potting glue includes A component, B component and C component, the A component includes the following raw materials: bisphenol A type epoxy resin, special epoxy, flame-retardant nanosheet, carbon black;The B component includes the following raw materials: triethylene tetramine, polyether amine, alicyclic amine;The C component includes the following raw materials: phosphoric acid fluoro alcohol ester.

[0007] Further, the bisphenol A type epoxy resin is one or more of epoxy resin E51, epoxy resin E55; the special epoxy resin is one or more of trifunctional glycidyl amine XY636, tetrafunctional glycidyl amine AG-602.

[0008] Further, the flame-retardant nanosheet is prepared from tetraethoxysilane, graphene oxide and boric acid.

[0009] Further, the polyetheramine is one or more of polyetheramine D230, polyetheramine T403.

[0010] Further, the alicyclic amine is one or more of 1,3-cyclohexanedimethylamine and isophorone diamine.

[0011] Further, a preparation method of the flame-retardant potting adhesive for lithium batteries comprises the following preparation steps:

[0012] (1) preparing a flame-retardant nanosheet;

[0013] (2) sequentially adding epoxy resin, special epoxy resin, flame-retardant nanosheet and carbon black into a stirring tank, the mass ratio of the epoxy resin, special epoxy resin, flame-retardant nanosheet and carbon black being 30:20:15:0.3~50:35:30:0.3, using a stirrer to stir and defoam at 60r / min for 45min to obtain component A;

[0014] (3) sequentially adding triethylenetetramine, alicyclic amine and polyetheramine into a stirring tank, the mass ratio of the triethylenetetramine, polyetheramine and alicyclic amine being 6:4:6~9:6:6, using a stirrer to stir and defoam at 60r / min for 45min to obtain component B;

[0015] (4) taking phosphoric acid fluorol ester as component C, and respectively packaging components A, B and C to obtain the flame-retardant potting adhesive for lithium batteries.

[0016] Further, the preparation method of the flame-retardant nanosheet in step (1) is as follows: graphene oxide and N,N-dimethylformamide are mixed at a mass ratio of 1:400-3:400, ultrasonic treatment is carried out at 500-800 W for 1 h, then tetraethoxysilane with a mass of 1.1-1.3 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.006-0.008 times that of N,N-dimethylformamide are added, reaction is carried out at 100-200 r / min and 60-80 DEG C for 24-32 h, then centrifugal separation is carried out at 15000 r / min for 5-10 min, the precipitate is taken out, the precipitate is washed with N,N-dimethylformamide by centrifugal separation for 3-5 times at 15000 r / min, and the precipitate is taken out; the precipitate and ammonia water are mixed at a mass ratio of 1:20-1:30, reaction is carried out at 200-300 r / min for 24-32 h, then the precipitate is washed with deionized water by centrifugal separation for 3-5 times at 15000 r / min, and freeze-drying is carried out at 50-70 DEG C for 24 h to obtain the silicon dioxide nanosheet; under a nitrogen / oxygen mixed atmosphere, the volume ratio of nitrogen to oxygen in the nitrogen / oxygen mixed gas is 1:3, the silicon dioxide nanosheet is preheated at 700-800 DEG C for 20-40 min, then the temperature is increased to 900-1000 DEG C, the silicon dioxide nanosheet is sprayed with boric acid with a mass of 0.1-0.3 times that of the silicon dioxide nanosheet, and the reaction is continued for 20-40 min to obtain the flame-retardant nanosheet.

[0017] Further, the preparation method of the flame-retardant nanosheet in step (1) is as follows: graphene oxide and N,N-dimethylformamide are mixed at a mass ratio of 1:400-3:400, ultrasonic treatment is carried out at 500-800 W for 1 h, then tetraethoxysilane with a mass of 1.1-1.3 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.006-0.008 times that of N,N-dimethylformamide are added, reaction is carried out at 100-200 r / min and 60-80 DEG C for 24-32 h, then centrifugal separation is carried out at 15000 r / min for 5-10 min, the precipitate is taken out, the precipitate is washed with N,N-dimethylformamide by centrifugal separation for 3-5 times at 15000 r / min, and the precipitate is taken out; the precipitate and ammonia water are mixed at a mass ratio of 1:20-1:30, reaction is carried out at 200-300 r / min for 24-32 h, then the precipitate is washed with deionized water by centrifugal separation for 3-5 times at 15000 r / min, and freeze-drying is carried out at 50-70 DEG C for 24 h to obtain the silicon dioxide nanosheet; under a nitrogen / oxygen mixed atmosphere, the volume ratio of nitrogen to oxygen in the nitrogen / oxygen mixed gas is 1:3, the silicon dioxide nanosheet is preheated at 700-800 DEG C for 20-40 min, then the temperature is increased to 900-1000 DEG C, the silicon dioxide nanosheet is sprayed with boric acid with a mass of 0.1-0.3 times that of the silicon dioxide nanosheet, and the reaction is continued for 20-40 min to obtain the flame-retardant nanosheet.

[0018] Compared with the prior art, the present application has the following beneficial effects:

[0019] The present application adds the flame-retardant nanosheet, uses the graphene oxide sheet as a template, polymerizes the tetraethoxysilane on the surface of the graphene oxide sheet to form a silicon dioxide layer, uses high temperature to decompose the graphene oxide, sprays boric acid at the same time, and makes boron doped into the silicon dioxide to form a boron-oxygen-silicon structure, thereby preparing the flame-retardant nanosheet, improving the high-temperature resistance of the material through the high-temperature resistance of the boron-oxygen-silicon structure and the barrier effect of the sheet structure, and promoting the resin dehydration and carbonization by generating boric acid during combustion, and the silicon, boron and carbon crosslinking to form a flame-retardant layer to block the combustible gas and heat transfer, so as to realize the halogen-free flame-retardant effect of the pouring sealant; in addition, the addition of the nanosheet can improve the mechanical properties of the pouring sealant. The present application uses the special epoxy (trifunctional glycidyl amine XY636 and tetrafunctional glycidyl amine AG-602) to adjust the viscosity of the epoxy system and improve the wetting and permeability thereof, so that the epoxy system is suitable for the HP-RTM forming process. The pouring sealant prepared by the present application is used in the HP-RTM forming process to prepare a 1.5 mm thick composite material, the Tg of the composite material can reach more than 120 DEG C after curing at 120 DEG C for 3-5 min, the flame-retardant performance reaches the UL94-V0 level, and the tensile strength can reach 1.2 MPa. Detailed Implementation

[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0021] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The test methods for various indicators of the flame-retardant potting compound for lithium batteries prepared in the following embodiments are as follows:

[0022] Flame retardant performance: The cut 4-layer fiber woven fabric is laid in the mold according to the layup requirements. After heating to 120℃ and vacuuming to -0.1MPa, the components A, B and C in the example are mixed evenly in a ratio of 100:14:1.5 and injected into the mold cavity using the HP-RTM process. After heat preservation and pressure preservation for 5 minutes, the mold is demolded to obtain the test sample. The flame retardant rating of the test sample is tested according to UL94 and the Tg is tested according to the DSC midpoint method.

[0023] Tensile strength: Take examples and comparative examples of the same mass and test the tensile strength according to GB / T6329.

[0024] Example 1

[0025] (1) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 1:400, sonicated at 500W for 1 h, and then tetraethoxysilane (1.1 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.006 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 100 r / min and 60 °C for 24 h, centrifuged at 15000 r / min for 5 min, and the precipitate was collected. The precipitate was washed three times by centrifugation with N,N-dimethylformamide at 15000 r / min. The precipitate was then collected. Ammonia and water were mixed at a mass ratio of 1:20 and reacted at 200 r / min for 24 h. After centrifugation and washing three times with deionized water at 15000 r / min, the mixture was freeze-dried at 50 °C for 24 h to obtain silica nanosheets. In a nitrogen / oxygen mixed atmosphere at 700 °C, with a nitrogen to oxygen volume ratio of 1:3, the silica nanosheets were preheated for 20 min and then heated to 900 °C. Boric acid with a mass ratio of 0.1 times that of the silica nanosheets was sprayed onto the silica nanosheets, and the reaction was continued for 20 min to obtain flame-retardant nanosheets.

[0026] (2) epoxy resin E51, trifunctional glycidyl amine XY636, flame-retardant nanosheet, carbon black were added into a stirring tank in sequence, the mass ratio of epoxy resin E51, trifunctional glycidyl amine XY636, flame-retardant nanosheet, carbon black was 30:20:15:0.3, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain A component;

[0027] (3) triethylenetetramine, 1,3-cyclohexanedimethylamine, polyether amine D230 were added into a stirring tank in sequence, the mass ratio of triethylenetetramine, 1,3-cyclohexanedimethylamine, polyether amine D230 was 6:4:6, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain B component;

[0028] (4) phosphoric acid fluoroalkyl ester was used as C component, A component, B component and C component were respectively packaged to obtain the flame-retardant pouring sealant for lithium battery.

[0029] Example 2

[0030] (1) graphene oxide and N,N-dimethylformamide were mixed according to a mass ratio of 2:400, then tetraethoxysilane with a mass of 1.2 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.007 times that of N,N-dimethylformamide were added after ultrasonic treatment at 650 W for 1 h, reaction was carried out at 150 r / min and 70℃ for 28 h, then the precipitate was obtained after centrifugation at 15000 r / min for 8 min, the precipitate was washed with N,N-dimethylformamide by centrifugation at 15000 r / min for 4 times, then ammonia water was added according to a mass ratio of 1:25, reaction was carried out at 250 r / min for 28 h, then the precipitate was washed with deionized water by centrifugation at 15000 r / min for 4 times, and the precipitate was obtained after freeze-drying at 60℃ for 24 h, to obtain silica nanosheet; the silica nanosheet was preheated at 750℃ for 30 min under a nitrogen / oxygen mixed atmosphere, the volume ratio of nitrogen to oxygen in the nitrogen / oxygen mixed gas was 1:3, the temperature was increased to 950℃, boric acid with a mass of 0.2 times that of the silica nanosheet was sprayed on the silica nanosheet, and the reaction was continued for 30 min, to obtain flame-retardant nanosheet;

[0031] (2) epoxy resin E55, tetrafunctional glycidyl amine AG-602XY636, flame-retardant nanosheet, carbon black were added into a stirring tank in sequence, the mass ratio of epoxy resin E55, tetrafunctional glycidyl amine AG-602XY636, flame-retardant nanosheet, carbon black was 40:28:23:0.3, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain A component;

[0032] (3) triethylenetetramine, isophorone diamine, polyether amine T403 were added into the stirring tank in turn, the mass ratio of triethylenetetramine, isophorone diamine, polyether amine T403 was 7.5:5:6, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain the B component;

[0033] (4) fluorophosphonate was used as the C component, the A component, the B component and the C component were packaged respectively to obtain the flame-retardant pouring sealant for lithium batteries.

[0034] Example 3

[0035] (1) graphene oxide and N,N-dimethylformamide were mixed in a mass ratio of 3:400, ultrasonic was performed at 800 W for 1 h, then tetraethoxysilane with a mass of 1.3 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.008 times that of N,N-dimethylformamide were added, reaction was performed at 80℃ under 200 r / min for 32 h, then centrifugation was performed at 15000 r / min for 10 min, the precipitate was taken, centrifugation was performed with N,N-dimethylformamide at 15000 r / min for 5 times, the precipitate was taken, graphene oxide and ammonia were mixed in a mass ratio of 1:30, reaction was performed at 300 r / min for 32 h, then centrifugation was performed with deionized water at 15000 r / min for 5 times, freeze-drying was performed at 70℃ for 24 h, to obtain the silica nanosheet, the silica nanosheet was preheated at 800℃ under a nitrogen / oxygen mixed atmosphere for 40 min, the volume ratio of nitrogen to oxygen in the nitrogen / oxygen mixed gas was 1:3, the temperature was increased to 1000℃, boracic acid with a mass of 0.3 times that of the silica nanosheet was sprayed on the silica nanosheet, and the reaction was continued for 40 min, to obtain the flame-retardant nanosheet;

[0036] (2) epoxy resin E55, tetrafunctional glycidyl amine, flame-retardant nanosheet and carbon black were added into the stirring tank in turn, the mass ratio of epoxy resin E55, tetrafunctional glycidyl amine, flame-retardant nanosheet and carbon black was 50:35:30:0.3, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain the A component;

[0037] (3) triethylenetetramine, isophorone diamine, polyether amine T403 were added into the stirring tank in turn, the mass ratio of triethylenetetramine, isophorone diamine, polyether amine T403 was 9:6:6, a stirrer was used to stir and defoam at 60 r / min for 45 min, to obtain the B component;

[0038] (4) fluorophosphonate was used as the C component, the A component, the B component and the C component were packaged respectively to obtain the flame-retardant pouring sealant for lithium batteries.

[0039] Example 4

[0040] (1) mixing graphene oxide and N,N-dimethylformamide according to a mass ratio of 2:400, ultrasonicating for 1 h under 650 W, adding tetraethoxysilane with a mass of 1.2 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.007 times that of N,N-dimethylformamide, reacting for 28 h under 150 r / min and 70 ℃, centrifuging for 8 min under 15000 r / min, taking the precipitate, centrifuging for 4 times with N,N-dimethylformamide under 15000 r / min, and taking the precipitate; mixing the precipitate and ammonia water according to a mass ratio of 1:25, reacting for 28 h under 250 r / min, centrifuging for 4 times with deionized water under 15000 r / min, and freeze-drying for 24 h under 60 ℃ to obtain silica nanosheets; preheating the silica nanosheets for 30 min under a nitrogen / oxygen mixed atmosphere with a volume ratio of nitrogen to oxygen of 1:3, heating to 950 ℃, spraying boric acid with a mass of 0.2 times that of the silica nanosheets on the silica nanosheets, and continuing to react for 30 min to obtain flame-retardant nanosheets;

[0041] (2) adding epoxy resin E55, trifunctional glycidyl amine XY636, flame-retardant nanosheets, and carbon black into a stirring tank in sequence, the mass ratio of the epoxy resin E55, trifunctional glycidyl amine XY636, flame-retardant nanosheets, and carbon black being 40:28:23:0.3, and using a stirrer to stir and defoam for 45 min at 60 r / min to obtain an A component;

[0042] (3) adding triethylenetetramine, 1,3-cyclohexanedimethylamine, and polyether amine T403 into a stirring tank in sequence, the mass ratio of the triethylenetetramine, 1,3-cyclohexanedimethylamine, and polyether amine T403 being 9:6:6, and using a stirrer to stir and defoam for 45 min at 60 r / min to obtain a B component;

[0043] (4) taking phosphoric acid fluorol ester as a C component, and packaging the A component, the B component, and the C component to obtain a flame-retardant pouring sealant for lithium batteries.

[0044] Comparative Example 1

[0045] (1) adding epoxy resin E55, tetrafunctional glycidyl amine, and carbon black into a stirring tank in sequence, the mass ratio of the epoxy resin E55, tetrafunctional glycidyl amine, and carbon black being 50:35:0.3, and using a stirrer to stir and defoam for 45 min at 60 r / min to obtain an A component;

[0046] (2) adding triethylenetetramine, isophorone diamine, and polyether amine T403 into a stirring tank in sequence, the mass ratio of the triethylenetetramine, isophorone diamine, and polyether amine T403 being 9:6:6, and using a stirrer to stir and defoam for 45 min at 60 r / min to obtain a B component;

[0047] (3) taking fluorophosphonate as the C component, the A component, the B component and the C component are respectively packaged to prepare the flame-retardant pouring sealant for lithium batteries.

[0048] Comparative Example 2

[0049] (1) graphene oxide and N,N-dimethylformamide were mixed in a mass ratio of 3:400, and after ultrasonic treatment at 800 W for 1 h, tetraethoxysilane in an amount of 1.3 times the mass of N,N-dimethylformamide and azobisisobutyronitrile in an amount of 0.008 times the mass of N,N-dimethylformamide were added, and after reaction at 80°C for 32 h at 200 r / min, the precipitate was taken after centrifugation at 15000 r / min for 10 min, and the precipitate was washed with N,N-dimethylformamide by centrifugation at 15000 r / min for 5 times, and the precipitate was taken; the precipitate and ammonia water were mixed in a mass ratio of 1:30, and after reaction at 300 r / min for 32 h, the precipitate was washed with deionized water by centrifugation at 15000 r / min for 5 times, and the precipitate was freeze-dried at 70°C for 24 h to obtain the flame-retardant nanosheet;

[0050] (2) epoxy resin E55, tetrafunctional glycidyl amine, flame-retardant nanosheet and carbon black were sequentially added to a stirring tank, and the mass ratio of epoxy resin E55, tetrafunctional glycidyl amine, flame-retardant nanosheet and carbon black was 50:35:30:0.3, and a stirrer was used to stir and degas at 60 r / min for 45 min to obtain the A component;

[0051] (3) triethylenetetramine, isophorone diamine and polyether amine T403 were sequentially added to a stirring tank, and the mass ratio of triethylenetetramine, isophorone diamine and polyether amine T403 was 9:6:6, and a stirrer was used to stir and degas at 60 r / min for 45 min to obtain the B component;

[0052] (4) taking fluorophosphonate as the C component, the A component, the B component and the C component are respectively packaged to prepare the flame-retardant pouring sealant for lithium batteries.

[0053] Effect Example

[0054] Table 1 below shows the performance analysis results of the flame-retardant pouring sealant for lithium batteries using the examples 1 to 4 and the comparative examples 1 to 2 of the present application.

[0055] Table 1

[0056] Flame retardant class Temperature (°C) Tensile strength (MPa) Example 1 V-0 122 0.7 Example 2 V-0 123 0.9 Example 3 V-0 128 1.2 Example 4 V-0 133 1.1 Comparative Example 1 None 90 0.3 Comparative Example 2 V-2 105 1.1

[0057] From the comparison of the flame-retardant grades and temperature data of the examples and the comparative examples in Table 1, it can be found that the flame-retardant grade of the potting adhesive prepared by the present application can reach UL94-V0, the Tg can reach 133℃, and the tensile strength can reach 1.2MPa. It is obvious for those skilled in the art that the present application is not limited to the details of the above exemplary embodiments, and the present application can be implemented in other specific forms without departing from the spirit or essential characteristics of the present application. Therefore, the examples should be regarded as exemplary and non-limiting from any point of view, and the scope of the present application is defined by the appended claims rather than the above description, and therefore all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present application. Any mark in the claims should not be regarded as limiting the involved claim.

Claims

1. A flame-retardant potting adhesive for lithium batteries, characterized by, The lithium battery flame-retardant pouring sealant comprises an A component, a B component and a C component, the A component comprises the following raw materials: bisphenol A type epoxy resin, special epoxy, flame-retardant nanosheet and carbon black; triethylenetetramine, polyetheramine and alicyclic amine; the C component comprises the following raw material: phosphoric acid fluoro alcohol ester; the flame-retardant nanosheet is prepared from tetraethoxysilane, graphene oxide and boric acid; The preparation method of the flame-retardant nanosheet is as follows: graphene oxide and N,N-dimethylformamide are mixed at a mass ratio of 1:400-3:400, ultrasonic treatment is carried out at 500-800 W for 1 h, then tetraethoxysilane with a mass of 1.1-1.3 times that of N,N-dimethylformamide and azobisisobutyronitrile with a mass of 0.006-0.008 times that of N,N-dimethylformamide are added, reaction is carried out at 100-200 r / min and 60-80 DEG C for 24-32 h, then centrifugal washing is carried out with N,N-dimethylformamide at 15000 r / min for 3-5 times, the precipitate is taken out, centrifugal washing is carried out with N,N-dimethylformamide at 15000 r / min for 3-5 times, the precipitate is taken out, graphene oxide nanosheet is obtained by mixing the precipitate and ammonia water at a mass ratio of 1:20-1:30, reaction is carried out at 200-300 r / min for 24-32 h, centrifugal washing is carried out with deionized water at 15000 r / min for 3-5 times, and freeze-drying is carried out at 50-70 DEG C for 24 h, the flame-retardant nanosheet is obtained by preheating the graphene oxide nanosheet at 700-800 DEG C in a nitrogen / oxygen mixed atmosphere for 20-40 min, then increasing the temperature to 900-1000 DEG C, spraying boric acid with a mass of 0.1-0.3 times that of the graphene oxide nanosheet on the graphene oxide nanosheet, and continuing to react for 20-40 min.

2. The fire-retardant potting adhesive for lithium batteries according to claim 1, characterized in that, The bisphenol A type epoxy resin is one or more of epoxy resin E51 and epoxy resin E55; the special epoxy is one or more of trifunctional glycidyl amine XY636 and tetrafunctional glycidyl amine AG-602.

3. The fire-retardant potting adhesive for lithium batteries according to claim 1, characterized in that, The polyetheramine is one or more of polyetheramine D230 and polyetheramine T403.

4. The fire-retardant potting adhesive for lithium batteries according to claim 1, characterized in that, The alicyclic amine is one or more of 1,3-cyclohexanedimethylamine and isophorone diamine.

5. A method for preparing a flame-retardant potting compound for lithium batteries according to claim 1, characterized in that, The preparation steps are as follows: (1) preparing the flame-retardant nanosheet; (2) adding epoxy resin, special epoxy, flame-retardant nanosheet and carbon black into a stirring tank in sequence, the mass ratio of the epoxy resin, special epoxy, flame-retardant nanosheet and carbon black is 30:20:15:0.3-50:35:30:0.3, using a stirrer to stir and defoam at 60 r / min for 45 min, and obtaining the A component; (3) adding triethylenetetramine, alicyclic amine and polyetheramine into a stirring tank in sequence, the mass ratio of the triethylenetetramine, polyetheramine and alicyclic amine is 6:4:6-9:6:6, using a stirrer to stir and defoam at 60 r / min for 45 min, and obtaining the B component; (4) taking phosphoric acid fluoro alcohol ester as the C component, and packaging the A component, B component and C component to obtain the lithium battery flame-retardant pouring sealant.

6. The preparation method of the fire-retardant potting glue for lithium batteries according to claim 5, characterized in that, The preparation method of the lithium battery flame-retardant pouring sealant is used to prepare the lithium battery flame-retardant pouring sealant, and when used, the components A, B and C are mixed in a mass ratio of 100:14:1.5.

Citation Information

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