含硼三烯丙基化合物改性环氧树脂的研究  

Study on epoxy resin modified by boron-containing triallyl compounds

作　　者：袁志刚 刘博 张斌[1] 孙明明[1] 张绪刚[1] 薛刚[1] 宋彩雨 李坚辉[1] 王磊[1] Yuan Zhigang;Liu Bo;Zhang Bin;Sun Mingming;Zhang Xugang;Xue Gang;Song Caiyu;Li Jianhui;Wang Lei(Institute of Petrochemistry Heilongjiang Academy of Sciences,Harbin 150040,Heilongjiang,China;College of Materials Science and Chemical Engineering,Harbin Engineering University,Harbin 150001,Heilongjiang,China)

机构地区：[1]黑龙江省科学院石油化学研究院,黑龙江哈尔滨150040 [2]哈尔滨工程大学材料科学与化学工程学院,黑龙江哈尔滨150001

出　　处：《中国胶粘剂》2024年第9期28-34,共7页China Adhesives

基　　金：黑龙江省科学院科学研究基金项目(CXMS2023SH01);黑龙江省财政厅基金项目(CZKYF2022-2-A001)。

摘　　要：采用含硼三胺(TAB)和香草醛衍生的烯类化合物(AM)为原料,通过希夫碱合成反应设计制备了一种含硼三烯丙基化合物(TABM),通过改变TABM的添加量得到一系列改性树脂(E-51+TABM)。对固化后树脂的结构、热稳定性、热机械性能、拉伸剪切性能、阻燃性能以及微观断裂形貌进行了表征。研究结果表明:(1)红外光谱和核磁氢谱的测试结果均表明,成功地制备了目标产物TABM。(2)热稳定性和热机械性能研究表明,随着TABM用量的增加,固化后环氧树脂的储能模量和残碳率也随之增大,但其玻璃化转变温度和交联密度降低。这表明TABM的添加可以降低材料的刚性,提升环氧树脂的韧性。(3)添加TABM后,环氧树脂在室温和100℃条件下的拉伸剪切强度均得到提升,当添加10份TABM时,拉伸剪切强度在25℃的条件下提升了25.5%,在100℃的条件下提升了37.5%。(4)随着树脂中TABM含量的增加,固化后树脂的极限氧指数(LOI)值也随之提升,直到添加量达到20份时达到最大值,说明TABM的添加,使得固化后树脂的阻燃性得到了有效改善。(5)微观断裂形貌分析表明,共混树脂(E-51+TABM)的断裂韧性得到了提高。A boron-containing triallyl compound(TABM)was designed and prepared by Schiff base synthesis reaction using boron-containing triamine(TAB)and vanillin derived alkene compounds(AM)as raw materials.A series of modified resins(E-51+TABM)were obtained by changing the addition amount of TABM.The structure,thermal stability,thermomechanical properties,tensile shear properties,flame retardancy and microscopic fracture morphology of the cured resin were characterized.The research results showed that,(1)The test results of infrared spectroscopy and nuclear magnetic hydrogen spectroscopy both indicated that the target product TABM was successfully prepared.(2)The research on thermal stability and thermomechanical properties showed that with the increase of TABM dosage,the storage modulus and residual carbon rate of cured epoxy resin also increased,but its glass transition temperature and crosslinking density decreased.This indicated that the addition of TABM could reduce the rigidity of the material and improve the toughness of epoxy resin.(3)After adding TABM,the tensile shear strength of epoxy resin was improved at both room temperature and 100℃.When 10 parts of TABM were added,the tensile shear strength increased by 25.5%at 25℃and 37.5%at 100℃(.4)As the content of TABM in the resin increased,the limit oxygen index(LOI)value of the cured resin also increased,reaching its maximum value when the addition amount reached 20 parts,indicating that the addition of TABM effectively improved the flame retardancy of the cured resin.(5)The microscopic fracture morphology analysis showed that the fracture toughness of the blended resin(E-51+TABM)was improved.

关 键 词：共聚改性 环氧树脂 热稳定性 热机械性能 剪切强度 

分 类 号：TQ430.4[化学工程]