CN118325268B - Low-compression permanent deformation battery sealing material and preparation method thereof - Google Patents
Low-compression permanent deformation battery sealing material and preparation method thereof Download PDFInfo
- Publication number
- CN118325268B CN118325268B CN202410590326.8A CN202410590326A CN118325268B CN 118325268 B CN118325268 B CN 118325268B CN 202410590326 A CN202410590326 A CN 202410590326A CN 118325268 B CN118325268 B CN 118325268B
- Authority
- CN
- China
- Prior art keywords
- parts
- sealing material
- ethylene propylene
- diene monomer
- propylene diene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sealing Battery Cases Or Jackets (AREA)
Abstract
The application relates to the technical field of ethylene propylene diene monomer rubber sealing material processing, in particular to a low-compression permanent deformation battery sealing material and a preparation method thereof, wherein the low-compression permanent deformation battery sealing material is prepared from the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer, 40-50 parts of carbon black, 25-30 parts of nano modified aluminum magnesium silicate, 10-15 parts of gas-phase white carbon black, 5-6 parts of polytetrafluoroethylene micropowder, 8-12 parts of paraffin oil, 1-2 parts of stearic acid, 6-8 parts of zinc oxide, 3-5 parts of polyethylene glycol, 2-3 parts of vulcanizing agent and 1-2 parts of anti-aging agent, and the high temperature resistance and electrolyte resistance of the battery sealing material can be effectively improved by adopting the raw materials together, so that the permanent compression deformation of the battery sealing material is reduced, and the battery sealing material can be used for a long time at high temperature.
Description
Technical Field
The application relates to the technical field of ethylene propylene diene monomer rubber sealing material processing, in particular to a low-compression permanent deformation battery sealing material and a preparation method thereof.
Background
The battery sealing member functions to prevent leakage of electrolyte inside the battery and entry of external impurities into the battery so that the battery can operate normally. The rubber material has excellent elasticity and plasticity, can effectively adapt to the deformation and vibration of the battery shell, so that good sealing performance is maintained, and therefore, the rubber is one of the materials commonly used for battery sealing elements.
The rubber materials for the battery sealing member mainly comprise perfluoro ether rubber, ethylene propylene diene monomer rubber and the like. The perfluoro ether rubber has excellent high temperature resistance and acid and alkali resistance, can stably work for a long time in a high temperature environment, but has poor processing performance, needs to adopt a special processing method and equipment, has high processing difficulty, and meanwhile, the raw materials of the perfluoro ether rubber are high in price, so that the production cost of the perfluoro ether rubber battery sealing piece is high, and the use of the perfluoro ether rubber is limited. Ethylene propylene diene monomer rubber is cheaper than perfluoroether rubber, but the high temperature resistance is good without perfluororubber, and the compression set is high when used at high temperature for a long time.
Disclosure of Invention
The application provides a low compression set battery sealing material and a preparation method thereof in order to improve the high temperature resistance of ethylene propylene diene monomer and reduce the compression set of the ethylene propylene diene monomer.
In a first aspect, the present application provides a low compression permanent deformation battery sealing material, which adopts the following technical scheme: the low-compression permanent deformation battery sealing material is prepared from the following raw materials in parts by weight:
Ethylene propylene diene monomer 100 parts
40-50 Parts of carbon black
25-30 Parts of nano modified aluminum magnesium silicate salt
10-15 Parts of gas-phase white carbon black
5-6 Parts of polytetrafluoroethylene micropowder
8-12 Parts of paraffin oil
Stearic acid 1-2 parts
6-8 Parts of zinc oxide
Polyethylene glycol 3-5 parts
2-3 Parts of vulcanizing agent
1-2 Parts of an anti-aging agent.
By adopting the technical scheme, the prepared battery sealing material has low permanent compression set, good electrolyte resistance and high temperature resistance, can be used in an environment of 200 ℃ for a long time without deformation, and has low manufacturing cost. According to the application, the ethylene propylene diene monomer is used together with carbon black, nano modified aluminum magnesium silicate, gas phase white carbon black, polytetrafluoroethylene micro powder, paraffin oil, stearic acid, zinc oxide, polyethylene glycol, vulcanizing agent, coupling agent and anti-aging agent, so that the electrolyte resistance of the high temperature resistance of the ethylene propylene diene monomer can be effectively improved, the permanent compression deformation of the ethylene propylene diene monomer is reduced, the ethylene propylene diene monomer can be used for a long time at high temperature, and the raw material cost is low.
The polytetrafluoroethylene and the nano modified aluminum magnesium silicate salt can improve the high temperature resistance of the ethylene propylene diene monomer. Wherein the nano modified aluminum magnesium silicate salt has good high temperature resistance and can not be decomposed in the use process. The nano modified aluminum magnesium silicate salt can be subjected to crosslinking reaction with ethylene propylene diene monomer at high temperature, so that the stability and heat resistance of the ethylene propylene diene monomer are improved, and the heat resistance of the sealing material can be greatly improved, so that the sealing material can be used in an environment of 200 ℃. Meanwhile, the nano modified aluminum magnesium silicate salt has stable chemical property, is stable in both acid medium and alkaline medium, is used together with ethylene propylene diene monomer, and can further improve the battery liquid resistance of the sealing material. The processing difficulty of the ethylene propylene diene monomer is further increased by adding the nano modified aluminum magnesium silicate, the fluidity of the nano modified aluminum magnesium silicate in the ethylene propylene diene monomer is improved by adding polyethylene glycol, the full mixing of the nano modified aluminum magnesium silicate and the ethylene propylene diene monomer is promoted, the high temperature resistance, the tensile strength and the hardness of the sealing material are improved, and the compression set of the sealing material is reduced.
Stearic acid can improve the mechanical properties of various raw materials, such as tensile strength, hardness and the like, of sealing materials, wherein the raw materials are further uniformly dispersed in the ethylene propylene diene monomer and permeate into an ethylene propylene diene monomer macromolecular chain to form a stable network structure.
The carbon black can effectively improve the hardness of the ethylene propylene diene monomer, but the excessive dosage of the carbon black can improve the compression set of the ethylene propylene diene monomer, so the hardness of the ethylene propylene diene monomer can be improved by adding a proper amount of gas phase white carbon black to be matched with the carbon black, and the compression set of the ethylene propylene diene monomer is not improved. The vulcanizing agent and zinc oxide can improve the vulcanizing speed and the crosslinking degree, so that the ethylene propylene diene monomer rubber has deeper vulcanizing degree and smaller compression set. The paraffin oil and the ethylene propylene diene monomer have better compatibility, and can improve the processability of the ethylene propylene diene monomer.
Preferably, the ethylene propylene diene monomer is modified ethylene propylene diene monomer, and the modified ethylene propylene diene monomer is prepared by the following method:
A: mixing a silane coupling agent, cyclohexene-4, 5-diglycidyl carboxylic acid ester and a solvent to obtain a mixed solution;
B: mixing ethylene propylene diene monomer and the mixed solution, heating to 80-90 ℃, dropwise adding a solution containing an initiator at the dropwise speed of 5-8g/min, continuing to perform heat preservation reaction for 4-6h after the dropwise adding is finished, and removing the solvent to obtain modified ethylene propylene diene monomer powder; the mass fraction of the solution containing the initiator is 30-40%.
By adopting the technical scheme, the compatibility of the ethylene propylene diene monomer with carbon black, modified nano aluminum magnesium silicate salt and gas-phase white carbon black is further improved, and the processability and high temperature resistance of the ethylene propylene diene monomer are improved.
According to the application, the problems of poor adhesiveness and processability of ethylene propylene diene monomer are further improved by grafting cyclohexene-4, 5-diglycidyl carboxylate, and simultaneously, the heat resistance and ageing resistance of the ethylene propylene diene monomer are improved by introducing siloxane bonds, and the compatibility of the ethylene propylene diene monomer with carbon black, modified nano aluminum magnesium silicate salt and gas phase white carbon black is enhanced, so that the heat resistance of the sealing material is improved and the compression set of the sealing material is reduced. By the preparation method, the silane coupling agent and cyclohexene-4, 5-diglycidyl carboxylate can be efficiently introduced, and the preparation process is simple and easy to operate.
Preferably, the modified ethylene propylene diene monomer is prepared from the following raw materials in parts by weight:
10-15 parts of silane coupling agent
Cyclohexene-4, 5-diglycidyl carboxylic acid ester 20-25 parts
200-250 Parts of solvent
Ethylene propylene diene monomer 100 parts
10-20 Parts of solution containing an initiator.
By adopting the technical scheme, the dosage of the modified ethylene propylene diene monomer raw material is optimized, so that the ethylene propylene diene monomer is high in grafting rate, is more easily mixed with carbon black, modified nano aluminum magnesium silicate salt and gas-phase white carbon black uniformly, improves the high temperature resistance, tensile strength and hardness of the sealing material, and reduces the compression set of the sealing material.
Preferably, the silane coupling agent includes at least one of gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane, gamma-aminopropyl triethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma-glycidoxypropyl triethoxysilane, and gamma-methacryloyloxy propyl trimethoxysilane.
By adopting the silane coupling agent, the grafting rate of the ethylene propylene diene monomer is improved, so that the ethylene propylene diene monomer has better compatibility with carbon black, modified nano aluminum magnesium silicate salt and gas phase white carbon black.
Preferably, the average particle size of the polytetrafluoroethylene micro powder is 5-40 μm.
By adopting the technical scheme, the average particle size of the polytetrafluoroethylene micro powder is further optimized, so that the polytetrafluoroethylene and the ethylene propylene diene monomer can be fully mixed, the high temperature resistance of the sealing material is further improved, and the compression set is reduced.
Preferably, ethylene content of ethylene propylene diene monomer is 40-60%, mooney viscosity ML (1+4) 125 ℃ is 50-100, and the third monomer content is 5-10%.
By adopting the technical scheme, the parameters of the ethylene propylene diene monomer are optimized, so that the ethylene propylene diene monomer has proper fluidity during processing, and the processability of the ethylene propylene diene monomer is improved. More preferably, ethylene propylene diene monomer rubbers of different ethylene contents are used in combination.
Preferably, the average particle size of the carbon black is 50-100nm, and the average particle size of the gas phase white carbon black is 200-400nm.
By adopting the technical scheme, the average particle size of the carbon black and the gas-phase white carbon black is optimized, the heat resistance, tensile strength, hardness and the like of the sealing material are further improved, and the compression set of the sealing material is reduced.
Preferably, the vulcanizing agent comprises at least one of dicumyl peroxide, di-tert-butyl-di-isopropylbenzene peroxide, N' -bifurfurylidene acetone, 1-di-tert-butyl-peroxy-3, 5-trimethylcyclohexane and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane.
By adopting the vulcanizing agent, the processability of the ethylene propylene diene monomer can be greatly optimized, and the crosslinking density of the sealing material can be improved even if a small amount of the vulcanizing agent is added, so that the heat resistance, the electrolyte resistance and the mechanical strength of the sealing material are improved, the electrolyte resistance is improved, and the service life of a product is prolonged.
Preferably, the anti-aging agent includes at least one of 2, 6-di-t-butyl-4-methylphenol, styrenated diphenylamine, 2-bis-4-hydroxyphenyl-hexafluoropropane, 2-methylene-bis (4-methyl-6-t-butylphenol), nickel dibutyldithiocarbamate, and 4, 4-bis (2, 2-dimethylbenzyl) diphenylamine.
By adopting the anti-aging agent, the heat resistance of the ethylene propylene diene monomer is improved, the aging of the ethylene propylene diene monomer is delayed, and the service life of the sealing material is further prolonged.
In a second aspect, the present application provides a method for preparing a low compression permanent deformation battery sealing material, which adopts the following technical scheme:
the preparation method of the low compression permanent deformation battery sealing material comprises the following preparation steps:
s1, mixing ethylene propylene diene monomer according to parts by weight, wherein the mixing time is 5-10min, and the mixing temperature is 40-50 ℃;
s2, mixing the mixed ethylene propylene diene monomer with zinc oxide, polytetrafluoroethylene micropowder, stearic acid and a cross-linking agent for 5-10min at the mixing temperature of 60-70 ℃ to obtain a mixture A;
S3, mixing the mixture A with carbon black, gas-phase white carbon black, paraffin oil, vulcanizing agent, nano modified aluminum magnesium silicate salt and anti-aging agent for 10-15min at 60-70 ℃ to obtain a mixture B;
S4, vulcanizing the mixture B, wherein the vulcanizing time of primary vulcanization is 5-10min at the vulcanizing temperature of 150-160 ℃, the vulcanizing temperature of secondary vulcanization is 120-140 ℃ and the vulcanizing time is 1-1.5h, and thus the low-compression permanent deformation battery sealing material is obtained.
By adopting the technical scheme, the raw materials are fully mixed, and the obtained sealing material has good high temperature resistance, tensile strength, electrolyte resistance and sealing performance and low compression set. The two-stage vulcanization can further improve the crosslinking density, remove small molecules and reduce the compression set.
In summary, the application has the following beneficial effects:
1. according to the application, the ethylene propylene diene monomer is used together with carbon black, nano modified aluminum magnesium silicate, gas phase white carbon black, polytetrafluoroethylene micro powder, paraffin oil, stearic acid, zinc oxide, polyethylene glycol, vulcanizing agent, coupling agent and anti-aging agent, so that the electrolyte resistance of the high temperature resistance of the ethylene propylene diene monomer can be effectively improved, the permanent compression deformation of the ethylene propylene diene monomer is reduced, and the ethylene propylene diene monomer can be used for a long time at high temperature.
2. According to the application, the ethylene propylene diene monomer is modified by adopting the silane coupling agent and cyclohexene-4, 5-diglycidyl carboxylate, so that the compatibility of the ethylene propylene diene monomer with carbon black, modified nano aluminum magnesium silicate salt and gas-phase white carbon black is improved, and the processing performance and heat resistance of the ethylene propylene diene monomer can be improved.
Detailed Description
Examples
In the application, polytetrafluoroethylene micropowder is purchased from Suzhou land and Tuo materials limited company, the average particle size is 5 mu m, and the brand is Zonyl; the model number of the nano modified magnesium aluminum silicate salt is SiliterN, which is purchased from Liyun harbor Ruiba chemical industry Co.
Example 1
A low compression permanent deformation battery sealing material is prepared by the following method:
S1, mixing 1000g of ethylene propylene diene monomer rubber for 5min at a mixing temperature of 40 ℃;
S2, mixing the mixed ethylene propylene diene monomer with 60g of zinc oxide, 50g of polytetrafluoroethylene micropowder (average particle size is 5 mu m) and 10g of stearic acid for 5min at a mixing temperature of 60 ℃ to obtain a mixture A;
S3, mixing the mixture A with 400g of carbon black (with the average particle size of 50 nm), 100g of gas-phase white carbon black (with the average particle size of 200 nm), 80g of paraffin oil, 20g of vulcanizing agent (dicumyl peroxide), 250g of nano modified aluminum magnesium silicate salt and 10g of anti-aging agent (2, 6-di-tert-butyl-4-methylphenol), wherein the mixing time is 15min, and the mixing temperature is 60 ℃ to obtain a mixture B;
s4, vulcanizing the mixture B, wherein when the vulcanization temperature of primary vulcanization is 150 ℃, the vulcanization time is 5min, the vulcanization temperature of secondary vulcanization is 120 ℃, and the vulcanization time is 1h, so that the low-compression permanent deformation battery sealing material is obtained.
Ethylene content of ethylene propylene diene monomer is 40%, mooney viscosity ML (1+4) is 50 at 125 ℃, and the content of the third monomer is 10%.
Examples 1 and examples 2-3 differ in the types, amounts and parameters of the materials used to prepare the low compression set battery sealant parts, as shown in Table 1:
table 1 examples 1-3 preparation of low compression set battery sealing materials types, amounts and parameters of raw materials
Example 4
A low compression set battery sealing material, the present embodiment is different from embodiment 1 in that: the ethylene propylene diene monomer is modified ethylene propylene diene monomer, and the modified ethylene propylene diene monomer is prepared by the following method:
A: 100g of a silane coupling agent (gamma- (methacryloyloxy) propyl trimethoxysilane), 200g of cyclohexene-4, 5-diglycidyl carboxylate and 2000g of a solvent (ethyl acetate) were mixed to obtain a mixed solution;
B: mixing 1000g of ethylene propylene diene monomer with the mixed solution, heating to 80 ℃, dropwise adding 100g of solution containing an initiator (di- (tert-butyl peroxy isopropyl) benzene) at a dropwise speed of 5g/min, continuing to perform heat preservation reaction for 4 hours after the dropwise adding is finished, and removing the solvent to obtain modified ethylene propylene diene monomer powder; the mass fraction of the initiator-containing solution was 30%.
Example 5
A low compression set battery sealing material, the present embodiment is different from embodiment 2 in that: the ethylene propylene diene monomer is modified ethylene propylene diene monomer, and the modified ethylene propylene diene monomer is prepared by the following method:
A: 120g of silane coupling agent (gamma-mercaptopropyl triethoxysilane), 220g of cyclohexene-4, 5-diglycidyl carboxylate and 2300g of solvent (ethylene glycol diethyl ether) are mixed to obtain a mixed solution;
B: mixing 1000g of ethylene propylene diene monomer with the mixed solution, heating to 85 ℃, dropwise adding 150g of solution containing an initiator (tert-butylcumene peroxide) at a dropwise speed of 6g/min, continuing to perform heat preservation reaction for 5 hours after the dropwise adding is finished, and removing the solvent to obtain modified ethylene propylene diene monomer powder; the mass fraction of the initiator-containing solution was 30%.
Example 6
A low compression set battery sealing material, the present embodiment is different from embodiment 3 in that: the ethylene propylene diene monomer is modified ethylene propylene diene monomer, and the modified ethylene propylene diene monomer is prepared by the following method:
a: 150g of silane coupling agent (gamma-aminopropyl triethoxysilane), 250g of cyclohexene-4, 5-diglycidyl carboxylate and 2500g of solvent (acetone) are mixed to obtain a mixed solution;
B: mixing 1000g of ethylene propylene diene monomer with the mixed solution, heating to 90 ℃, dropwise adding 40g of (3, 3-bis (tert-amyl peroxy) ethyl butyrate) containing an initiator, wherein the dropwise adding speed is 8g/min, continuing to perform heat preservation reaction for 6 hours after the dropwise adding is finished, and removing the solvent to obtain modified ethylene propylene diene monomer powder; the mass fraction of the initiator-containing solution was 40%.
Example 7
A low compression set battery sealing material, the present embodiment is different from embodiment 4 in that: the amount, type and experimental parameters of the remaining materials were identical to those of example 4, using a solvent instead of the same amount of silane coupling agent.
Example 8
A low compression set battery sealing material, the present embodiment is different from embodiment 4 in that: the amount, type and experimental parameters of the remaining raw materials were the same as in example 4, except that the solvent was used instead of the same amount of cyclohexene-4, 5-diglycidyl carboxylic acid ester.
Example 9
A low compression set battery sealing material, the present embodiment is different from embodiment 4 in that: the silane coupling agent is vinyltriethoxysilane, and the dosage, the types and the experimental parameters of the rest raw materials are the same as those of the example 4.
Example 10
A low compression set battery sealing material, the present embodiment is different from embodiment 4 in that: the amount of the other starting materials, the types and the experimental parameters were the same as in example 4 except that maleic anhydride was used instead of the equivalent amount of cyclohexene-4, 5-diglycidyl carboxylic acid ester.
Example 11
A low compression set battery sealing material, the present embodiment is different from embodiment 1 in that: the average particle diameter of the carbon black was 200nm, and the amounts, types and experimental parameters of the remaining raw materials were the same as those of example 1.
Comparative example
Comparative example 1
A battery sealing material, this comparative example is different from example 1 in that: the use of silica in place of the nano-modified aluminum magnesium silicate salt and the amounts, types and experimental parameters of the remaining materials were the same as in example 1.
Comparative example 2
A battery sealing material, this comparative example is different from example 1 in that: the amount, type and experimental parameters of the remaining raw materials were identical to those of example 1, using silica instead of the equivalent amount of carbon black.
Comparative example 3
The sealing material of this comparative example is different from that of example 1 in that: the polyimide was used instead of the equivalent polytetrafluoroethylene powder, and the amounts, types and experimental parameters of the remaining raw materials were the same as those of example 1.
Polyimide was purchased from Guangzhou Dihuan plastics Co., ltd, under the trademark PISP-1.
Comparative example 4
The cell sealing material of this comparative example is different from that of example 1 in that: the amount, type and experimental parameters of the remaining materials were identical to those of example 1, using oleic acid instead of the equivalent amount of stearic acid.
Comparative example 5
A low compression set battery sealing material, this comparative example differs from example 1 in that: the amount, type and experimental parameters of the other raw materials are the same as those of example 1 by using polyoxyethylene alkyl ether to replace the equivalent polyethylene glycol
Performance test the low compression set battery sealants prepared in examples 1-11 and the battery sealants prepared in comparative examples 1-5 were subjected to tensile strength test, hardness test, compression set and hot air aging properties.
Detection method/test method
Tensile strength test: the tensile strength of the resulting battery seal material was tested using the standard number ASTM D412;
hardness testing: the hardness of the resulting battery sealing material was tested using the standard number ASTM D2240;
compression set: the resulting battery sealing material was tested for compression set using the standard number ASTM D395 (test method B,120 ℃ c. X70 h, 25%);
the hot air aging performance is measured according to GB/T3512, the conditions are: 200 ℃ and 72 hours, and then testing the tensile strength and the hardness; experimental data are shown in table 2:
TABLE 2 Experimental data for examples 1-11 and comparative examples 1-5
As is clear from examples 1 to 11 and comparative examples 1 to 5 in combination with Table 2, the low compression set battery sealing material prepared by using the formulation of the present application has good heat resistance, high tensile strength, good hardness, and lower compression set.
Compared with comparative example 1, the tensile strength and the hardness in comparative example 1 are reduced, the compression set is increased, and the tensile strength and the hardness in comparative example 1 are greatly changed after the thermal aging test, which shows that the high temperature resistance, the tensile strength and the hardness of the sealing material can be further improved by adding the nano modified aluminum magnesium silicate, and the compression set of the sealing material is reduced.
The tensile strength and hardness in comparative example 2 were substantially unchanged, but the compression set was increased, compared with those in comparative example 1 and comparative example 2, indicating that the compression set of the sealing material could be effectively reduced by adding an appropriate amount of carbon black.
Compared with the comparative examples 3-5, the tensile strength and the hardness of the sealing materials are reduced in the comparative examples 3-5, the compression set is increased, and the tensile strength and the hardness of the sealing materials are greatly changed in the comparative examples 3-5 after the thermal aging test, which proves that the high temperature resistance, the tensile strength and the hardness of the sealing materials are improved by adding the polytetrafluoroethylene, the stearic acid and the polyethylene glycol, and the compression set of the sealing materials is reduced.
Examples 4 to 6 show an increase in tensile strength and hardness and a decrease in compression set in examples 1 to 4, examples 2 to 5, and examples 3 to 6; and after thermal aging test, the tensile strength and hardness in examples 4-6 are less in change, which shows that the high temperature resistance, tensile strength and hardness of the sealing material can be effectively improved and the compression set of the sealing material can be reduced by modifying the ethylene propylene diene monomer rubber.
Example 4 compared to examples 7-10, examples 7-9 have lower tensile strength and hardness than example 4, and examples 7-10 have lower compression set than example 4; and the tensile strength and hardness in example 4-changed less after heat aging test; the modified ethylene propylene diene monomer prepared by the method can effectively improve the high temperature resistance, tensile strength and hardness of the sealing material and reduce the compression set of the sealing material.
In example 1, tensile strength and hardness were slightly improved and compression set was slightly reduced as compared with example 11, indicating that the sealing material performance was improved by optimizing the average particle size of carbon black and fumed silica.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (8)
1. The low compression permanent deformation battery sealing material is characterized by being prepared from the following raw materials in parts by weight:
ethylene propylene diene monomer 100 parts
40-50 Parts of carbon black
25-30 Parts of nano modified aluminum magnesium silicate salt
10-15 Parts of gas-phase white carbon black
5-6 Parts of polytetrafluoroethylene micropowder
8-12 Parts of paraffin oil
Stearic acid 1-2 parts
6-8 Parts of zinc oxide
Polyethylene glycol 3-5 parts
2-3 Parts of vulcanizing agent
1-2 Parts of an anti-aging agent;
The ethylene propylene diene monomer is modified ethylene propylene diene monomer, and the modified ethylene propylene diene monomer is prepared by the following method:
A: mixing a silane coupling agent, cyclohexene-4, 5-diglycidyl carboxylic acid ester and a solvent to obtain a mixed solution;
B: mixing ethylene propylene diene monomer and the mixed solution, heating to 80-90 ℃, dropwise adding a solution containing an initiator at the dropwise speed of 5-8g/min, continuing to perform heat preservation reaction for 4-6h after the dropwise adding is finished, and removing the solvent to obtain modified ethylene propylene diene monomer powder; the mass fraction of the solution containing the initiator is 30-40%;
The raw materials for preparing the modified ethylene propylene diene monomer are as follows in parts by weight:
10-15 parts of silane coupling agent
Cyclohexene-4, 5-diglycidyl carboxylic acid ester 20-25 parts
200-250 Parts of solvent
Ethylene propylene diene monomer 100 parts
10-20 Parts of solution containing an initiator.
2. The low compression set battery sealing material according to claim 1, wherein: the silane coupling agent comprises at least one of gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane, gamma-aminopropyl triethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma-glycidoxypropyl triethoxysilane and gamma-methacryloyloxy propyl trimethoxysilane.
3. The low compression set battery sealing material according to claim 1, wherein: the ethylene content of the ethylene propylene diene monomer is 40-60%, the Mooney viscosity ML (1+4) is 50-100 at 125 ℃, and the third monomer content is 5-10%.
4. The low compression set battery sealing material according to claim 1, wherein: the vulcanizing agent comprises at least one of dicumyl peroxide, di-tert-butyl dicumyl peroxide, N' -bifurfuryl acetone, 1-di-tert-butyl peroxy-3, 3, 5-trimethylcyclohexane and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.
5. The low compression set battery sealing material according to claim 1, wherein: the average grain diameter of the polytetrafluoroethylene micro powder is 5-40 mu m.
6. The low compression set battery sealing material according to claim 1, wherein: the average grain diameter of the carbon black is 50-100nm, and the average grain diameter of the gas phase white carbon black is 200-400nm.
7. The low compression set battery sealing material according to claim 1, wherein: the anti-aging agent comprises at least one of 2, 6-di-tert-butyl-4-methylphenol, styrenated diphenylamine, 2-bis-4-hydroxyphenyl-hexafluoropropane, 2-methylene-bis (4-methyl-6-tert-butylphenol), nickel dibutyldithiocarbamate and 4, 4-bis (2, 2-dimethylbenzyl) diphenylamine.
8. A method for producing the low compression set battery sealing material as defined in any one of claims 1 to 7, comprising the steps of:
s1, mixing ethylene propylene diene monomer according to parts by weight, wherein the mixing time is 5-10min, and the mixing temperature is 40-50 ℃;
S2, mixing the mixed ethylene propylene diene monomer with zinc oxide, polytetrafluoroethylene micro powder and stearic acid for 5-10min at 60-70 ℃ to obtain a mixture A;
S3, mixing the mixture A with insulating carbon black, gas-phase white carbon black, paraffin oil, vulcanizing agent, nano modified aluminum magnesium silicate salt and anti-aging agent for 10-15min at 60-70 ℃ to obtain a mixture B;
S4, vulcanizing the mixture B, wherein the vulcanizing time of primary vulcanization is 5-10min at the vulcanizing temperature of 150-160 ℃, the vulcanizing temperature of secondary vulcanization is 120-140 ℃ and the vulcanizing time is 1-1.5h, and thus the low-compression permanent deformation battery sealing material is obtained.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410590326.8A CN118325268B (en) | 2024-05-13 | 2024-05-13 | Low-compression permanent deformation battery sealing material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410590326.8A CN118325268B (en) | 2024-05-13 | 2024-05-13 | Low-compression permanent deformation battery sealing material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN118325268A CN118325268A (en) | 2024-07-12 |
CN118325268B true CN118325268B (en) | 2024-10-15 |
Family
ID=91765914
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202410590326.8A Active CN118325268B (en) | 2024-05-13 | 2024-05-13 | Low-compression permanent deformation battery sealing material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN118325268B (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101796125A (en) * | 2007-07-02 | 2010-08-04 | 阿肯马法国公司 | Elastomer thermoplastic mixtures and compositions having improved properties, method of making said compositions and applications thereof |
CN108546364A (en) * | 2018-02-28 | 2018-09-18 | 中国铁道科学研究院金属及化学研究所 | A kind of cold-resistant low compression set rubber composition and preparation method thereof |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114672101B (en) * | 2022-04-26 | 2024-05-03 | 安徽中鼎密封件股份有限公司 | Low-temperature-compression-resistant permanent deformation ethylene propylene diene monomer rubber material and preparation method thereof |
CN115028927B (en) * | 2022-05-30 | 2024-03-29 | 安徽中鼎密封件股份有限公司 | Ultralow-hardness high-resilience low-pressure-change ethylene propylene diene monomer rubber material and preparation method thereof |
CN117965131B (en) * | 2024-01-23 | 2024-08-20 | 东莞市创进塑胶五金有限公司 | Low-compression permanent deformation silicone rubber sealant and preparation method thereof |
-
2024
- 2024-05-13 CN CN202410590326.8A patent/CN118325268B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101796125A (en) * | 2007-07-02 | 2010-08-04 | 阿肯马法国公司 | Elastomer thermoplastic mixtures and compositions having improved properties, method of making said compositions and applications thereof |
CN108546364A (en) * | 2018-02-28 | 2018-09-18 | 中国铁道科学研究院金属及化学研究所 | A kind of cold-resistant low compression set rubber composition and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN118325268A (en) | 2024-07-12 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101681727B (en) | Sealing body for electrolytic capacitor and electrolytic capacitor using the same | |
US4251432A (en) | Method of providing curable fluoroelastomer gums having coupling agent coated particulate carbonaceous fillers | |
CN109777115A (en) | A kind of automobile engine sealing ring silicon rubber and preparation method thereof | |
CN111394054A (en) | Silicone rubber for self-adhesive tape and preparation method thereof | |
CN105733087A (en) | Rubber composition and preparation method thereof | |
JP5728297B2 (en) | Crosslinked polymer composition and method for producing the same | |
CN118325268B (en) | Low-compression permanent deformation battery sealing material and preparation method thereof | |
CN114790342B (en) | Silane modified carbon black composite filler and preparation method thereof | |
CN114163822B (en) | Organosilicon modified ethylene propylene diene monomer rubber and preparation method thereof | |
CN104356422A (en) | Maleopimaric acid modified white carbon black, fluorinated silicone rubber mixing rubber and preparation method thereof | |
CN108587068B (en) | A kind of hydrophobic flame-retardant epoxy resin and preparation method thereof | |
US5039718A (en) | Fillers | |
CN109135649A (en) | Low modulus elastomeric sealant and preparation method thereof | |
CN109337631B (en) | Preparation method of silane-terminated sealant with excellent medium resistance | |
US4908396A (en) | Fillers | |
CN117304614A (en) | Rubber elastomer material for vehicle and preparation method thereof | |
CN114044987A (en) | Oil-resistant ethylene propylene insulating material | |
CN115093628A (en) | Polyisoprene rubber modified graphene modified chloroprene rubber and synthesis method thereof | |
CN115558282A (en) | Environment-friendly efficient flame-retardant cable material and preparation method thereof | |
CN116529302A (en) | Rubber composition, sulfide of the rubber composition, and vulcanized molded article of the rubber composition | |
CN111500240A (en) | Silane modified polyether sealant with excellent chemical medium resistance and preparation method thereof | |
CN118496611A (en) | High-hardness low-compression permanent deformation perfluoroether rubber and preparation method and application thereof | |
CN114672112B (en) | Flame-retardant flexible polyvinyl chloride plastic and preparation method thereof | |
CN119331556A (en) | A two-component hybrid glue and its preparation method and application | |
CN117186654A (en) | Additive for reducing compression set, fluorosilicone rubber composition and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |