【作者】 彭红星；

【导师】 刘跃进；

【作者基本信息】 湘潭大学 ， 化学工程， 2007， 硕士

【摘要】 电子材料是发展微电子工业的基础,作为生产集成电路的主要结构材料——环氧塑封料随着芯片技术的发展正在飞速发展。研制并开发性能优异的电子封装材料,以国产封装料替代进口产品,这是一个极待研究的问题。1,1,2,2-四对羟基苯基乙烷四缩水甘油醚环氧树脂(简称:四酚基乙烷四缩水甘油醚环氧树脂)是一种高强韧性对称结构骨架的电子封装料。它不仅具有一般环氧树脂的功能还具有高玻璃化温度、高耐热、防UV穿透和适应AOI等特殊功能。关于该产品的研究,国内鲜见报道。这里以苯酚、乙二醛、环氧氯丙烷和氢氧化钠为原料,采用两步法合成了1,1,2,2-四对羟基苯基乙烷四缩水甘油醚环氧树脂。首先用苯酚、乙二醛在草酸和甲醇存在下,进行亲核加成缩合反应,制备了1,1,2,2—四对羟基苯基乙烷(TPE)。研究了草酸用量、反应温度、反应时间、原料配比对TPE收率的影响。结果表明:在草酸用量2%、苯酚与乙二醛的摩尔比20:1、反应温度82℃、反应8小时,TPE收率达42%。再用1,1,2,2-四对羟基苯基乙烷与环氧氯丙烷在醚化催化剂四乙基溴化铵和溶剂异丙醇存在下,先进行醚化反应,然后加入等当量(n(TEP)∶n(NaOH)为1:4.0)氢氧化钠进行环氧化脱氯反应,再经水洗、分离、精制,得到1,1,2,2-四对羟基苯基乙烷四缩水甘油醚环氧树脂。研究了原料配比、反应时间和温度对产品氯含量和环氧值的影响,结果表明,当环氧氯丙烷与四酚基乙烷摩尔比为21:1,四酚基乙烷与氢氧化钠摩尔比为1:4,醚化反应温度85℃,醚化反应时间4 h,闭环反应温度70℃,闭环反应时间2.5 h时,所得产品环氧值为0.513,软化点83℃,可水解氯含量为1.92×10-4,收率为57%。经傅里叶变换红外光谱(FTIR)和核磁共振( 1HNMR和13CNMR)分析,初步确认了所合成产品为四酚基乙烷四缩水甘油醚环氧树脂。更多还原

【Abstract】 Electronic materials are the basic of the microelectronic industry, as the mostly structural materials of integrated circuits——epoxy resin molding compounds are developing fast along with the development of the technology of chips. It is a stringent problem to be researched that how to researching and exploiting epoxy resin molding compounds with high properties and using domestic packages to replace import products.1,1,2,2-tetrakis(hydroxyphenyl) ethane tetraglycidyl ether epoxy resin (tetraphenol ethane tetraglycidyl ether epoxy resin ) which is electronic encapsulation materials of the symmetric framework of high strength and toughness. It has not only the properties of common epoxy resin, but also has high glass transition temperature, high heat-resistant, UV-block and AOI(Automatic Optic Inspection) properties and so on. It is little reported on the study of the product in home. 1,1,2,2-tetrakis(hydroxyphenyl) ethane tetraglycidyl ether epoxy resin was prepared in a two-step process by using phenol, glyoxal, epichlorohydrin and sodium hydroxide as raw materials.Firstly, 1,1,2,2-tetrakis(hydroxyphenyl) ethane was synthesized by nueleophilie addition and condensation reaction of phenol with glyoxal in the presence of oxalic acid and methanol. The factors affecting the yield of the production was investigated, including the amount of oxalic acid, reaction temperature, reaction time and reagent proportion . The result showed that oxalic acid was the 2% , the molar ratio of phenol to glyoxal was 20:1; the temperature of the reaction was 82℃, the time of the reaction was 8 h, the yield could reach 42% .Then, the 1,1,2,2-tetrakis(hydroxyphenyl) ethane tetraglycidyl ether epoxy resin was obtained with 1,1,2,2-tetrakis(hydroxyphenyl) ethane and epichlorohydrin in the presence of both the tetraethylammonium bromide as a etherification catalyst and the isopropanol as a solvent. First the etherification reaction and then the epoxidation reaction (dehydrochlorination) occurred by adding an equivalent amount of sodium hydroxide. Subsequently water washing and refining were performed. The effects of reagent proportion, reaction time and reaction temperature on both the chlorine content and the epoxy value for synthesized resin product were investigated. The obtained results showed that under the conditions of the molar ratio of epichlorohydrin to tetraphenol ethane 21:1, the molar ratio of tetraphenol ethane to sodium hydroxide 1:4, the etherification reaction temperature 85℃, the etherification reaction time 4h, the ring-closing reaction temperature 70℃and the ring-closing reaction time 2.5h, the epoxy value, softening point, the hydrolyzable chlorine and the yield of resin product were 0.513, 83℃, 57% and 1.92×10-4 respectively.The structure of epoxy resin of 1,1,2,2-tetrakis(hydroxyphenyl) ethane tetraglycidyl ether was preliminary confirmed by analysis of both the Fourier Transform Infrared Spectrum (FTIR) and the Nuclear Magnetic Resonance (1HNMR and 13CNMR).更多还原