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CN-121991618-A - Preparation method of battery pack sealant

CN121991618ACN 121991618 ACN121991618 ACN 121991618ACN-121991618-A

Abstract

The invention relates to a preparation method of a battery pack sealant, which belongs to the technical field of adhesive preparation and comprises the steps of S1, heating and adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, hydroxyalkyl polysiloxane containing double bond ends and an initiator at 90-110 ℃ under protective gas, devolatilizing an intermediate, dehydrating and adding diisocyanate to react with a catalyst to obtain a prepolymer, dripping glycidol to block until an isocyanate peak disappears to obtain a modifier, S2, 100 parts of matrix resin, 15-40 parts of modifier, 100-300 parts of insulating heat-conducting filler and 1-5 parts of coupling agent to obtain a component A, S3, taking 20-50 parts of curing agent as a component B, uniformly mixing, and primarily solidifying and heating at room temperature to obtain the sealant.

Inventors

  • CHEN XIAOYANG
  • ZHENG QING
  • CHEN RONG
  • DENG ZHIJUN

Assignees

  • 东莞市博翔电子材料有限公司
  • 广东省博翔新材料有限公司

Dates

Publication Date
20260508
Application Date
20260323

Claims (9)

  1. 1. The preparation method of the battery pack sealant is characterized by comprising the following steps of: S1, preparing a phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier: (1) Mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with hydroxyl-terminated polysiloxane containing carbon-carbon double bonds in a protective gas atmosphere, adding a free radical initiator, performing addition reaction under a heating condition, and performing vacuum volatile removal treatment after the reaction is finished to obtain a phosphorus-containing silicon diol intermediate; (2) Vacuum dehydration treatment is carried out on the phosphorus-containing silicon diol intermediate, the temperature is reduced to 50-60 ℃, diisocyanate and a catalyst are added, and the heat preservation reaction is carried out under the heating condition, so that isocyanate-terminated prepolymer is obtained; (3) Cooling a system containing the isocyanate-terminated prepolymer, slowly dropwise adding glycidol at a speed of 1-3 drops/second for end capping reaction, and preserving heat until the characteristic absorption peak of the isocyanate group in the infrared spectrum disappears, thereby obtaining the phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier; s2, preparing a component A, namely adding 100 parts of matrix resin, 15-40 parts of the phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier prepared in the step S1, 100-300 parts of insulating heat-conducting filler and 1-5 parts of silane coupling agent into stirring equipment according to parts by weight, and carrying out high-speed dispersion and mixing under a vacuum condition to obtain the component A; S3, preparing a component B, namely weighing 20-50 parts of curing agent serving as the component B according to parts by weight; And S4, crosslinking and curing, namely uniformly mixing the component A and the component B, and curing after primary curing at room temperature and heating to obtain the battery pack sealant.
  2. 2. The preparation method of the battery pack sealant according to claim 1, wherein in the step (1) of the step S1, the feeding mole ratio of the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to the hydroxyalkyl polysiloxane containing carbon-carbon double bonds is 1:1, namely the mole ratio of P-H bonds to C=C double bonds is 1:1, the reaction temperature under the heating condition is 90-110 ℃, and the protective gas atmosphere is nitrogen atmosphere.
  3. 3. The method for preparing the battery pack sealant according to claim 2, wherein in the step (1) of the step S1, the hydroxyalkyl polysiloxane containing carbon-carbon double bonds is hydroxypropyl silicone oil containing vinyl groups at side chains, and the free radical initiator is azobisisobutyronitrile.
  4. 4. The preparation method of the battery pack sealant according to claim 1 is characterized in that in the step (2) of the step S1, the condition of vacuum dehydration treatment is that the vacuum dehydration is carried out for 2 hours at 110 ℃, the temperature is reduced to 60 ℃, the feeding mole ratio of hydroxyl in the phosphorus-containing silicon diol intermediate to isocyanate groups in diisocyanate is 1:2.05-1:2.2, and the temperature of the thermal insulation reaction under the heating condition is 75-85 ℃.
  5. 5. The method for preparing a battery pack sealant according to claim 4, wherein in the step (2) of the step S1, the diisocyanate is isophorone diisocyanate, and the catalyst is an organobismuth catalyst or a dibutyl tin dilaurate catalyst.
  6. 6. The preparation method of the battery pack sealant according to claim 1 is characterized in that in the step (3) of the step S1, the system is cooled to 50-60 ℃, the molar ratio of hydroxyl in glycidol to the residual isocyanate groups in the isocyanate-terminated prepolymer is 1:1, and the reaction temperature is controlled to be not more than 65 ℃ in the end-capping reaction process.
  7. 7. The method for preparing the battery pack sealant according to claim 1, wherein in the step S2, the vacuum degree of the vacuum condition is less than or equal to-0.09 MPa, and the matrix resin is at least one selected from bisphenol A type epoxy resin and bisphenol F type epoxy resin.
  8. 8. The method of claim 1, wherein in step S2, the insulating and heat conducting filler is spherical aluminum oxide subjected to surface treatment, and the water extractable ion content of the insulating and heat conducting filler is lower than 800ppm.
  9. 9. The method for preparing the battery pack sealant according to claim 1, wherein in the step S3, the curing agent is at least one selected from modified aliphatic amine, polyether amine and liquid anhydride, and in the step S4, the condition of curing after heating is that the battery pack sealant is cured for 2 hours at 80 ℃.

Description

Preparation method of battery pack sealant Technical Field The invention relates to the field of adhesive preparation, in particular to a preparation method of battery pack sealant. Background The linear polyolefin has excellent chemical stability and mechanical property, is widely applied to the fields of high polymer packaging materials, film preparation and the like, but has a plurality of defects in the aspects of inherent physical properties of matrix resin, such as the use of battery pack sealant and high-requirement film materials, the traditional additive flame retardant is extremely easy to migrate and precipitate, and the resin is easy to damage due to internal stress after solidification; In order to overcome the limitations of the materials, polymer modification is considered as an effective way for making up inherent defects and comprehensively optimizing comprehensive performance, and the method is characterized in that the precise regulation of chemical structures is realized by introducing a hybrid flexible chain segment and an intrinsic flame retardant group into a molecular main chain to reconstruct a crosslinked network, so that the difficult problem of brittleness after the material is solidified can be remarkably improved, and a durable flame retardant effect and excellent buffering and energy absorbing characteristics can be obtained; At present, the effective means for preparing the high-performance composite material is methods of in-situ construction, crosslinking, curing and the like, and the method forms a microscopic phase-separated island structure interpenetrating network by synthesizing the hybrid multifunctional modifier and carrying out deep covalent crosslinking with matrix resin, so that the method becomes a main way for solving the technical bottleneck. Disclosure of Invention The invention aims to provide a preparation method of battery pack sealant, which aims to solve the problems in the background technology. The technical scheme of the invention comprises the following steps of S1, preparing a phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier: (1) Mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with hydroxyl-terminated polysiloxane containing carbon-carbon double bonds in a protective gas atmosphere, adding a free radical initiator, performing addition reaction under a heating condition, and performing vacuum volatile removal treatment after the reaction is finished to obtain a phosphorus-containing silicon diol intermediate; (2) Vacuum dehydration treatment is carried out on the phosphorus-containing silicon diol intermediate, the temperature is reduced to 50-60 ℃, diisocyanate and a catalyst are added, and the heat preservation reaction is carried out under the heating condition, so that isocyanate-terminated prepolymer is obtained; (3) Cooling a system containing the isocyanate-terminated prepolymer, slowly dropwise adding glycidol at a speed of 1-3 drops/second for end capping reaction, and preserving heat until the characteristic absorption peak of the isocyanate group in the infrared spectrum disappears, thereby obtaining the phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier; s2, preparing a component A, namely adding 100 parts of matrix resin, 15-40 parts of the phosphorus-containing silicon hybrid polyurethane-epoxy multifunctional modifier prepared in the step S1, 100-300 parts of insulating heat-conducting filler and 1-5 parts of silane coupling agent into stirring equipment according to parts by weight, and carrying out high-speed dispersion and mixing under a vacuum condition to obtain the component A; S3, preparing a component B, namely weighing 20-50 parts of curing agent serving as the component B according to parts by weight; And S4, crosslinking and curing, namely uniformly mixing the component A and the component B, and curing after primary curing at room temperature and heating to obtain the battery pack sealant. Further, in step (1) of step S1, the feeding molar ratio of the P-H bond in the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to the hydroxyalkyl polysiloxane containing carbon-carbon double bond in step (1) is 1:1, that is, the molar ratio of the P-H bond to the c=c double bond is 1:1, the reaction temperature under the heating condition is 90-110 ℃, and the protective gas atmosphere is a nitrogen atmosphere. Further, in the step (1) of the step S1, the hydroxyl-terminated polysiloxane containing carbon-carbon double bonds is hydroxyl-terminated silicone oil containing vinyl groups at the side chains, and the free radical initiator is azobisisobutyronitrile. Further, in the step (2) of the step S1, the condition of vacuum dehydration is that vacuum dehydration is performed for 2 hours at 110 ℃, the temperature is reduced to 60 ℃, the feeding molar ratio of hydroxyl groups in the phosphorus-containing silicon diol intermediate to isocyanate groups in the diisocy