正交试验法制备耐热型萘基环氧树脂

Preparation of heat-resistant naphthyl epoxy resin by orthogonal experiment

为了改善环氧树脂的耐热性能,将刚性基团萘环引入环氧树脂分子骨架中,制备了萘基环氧树脂。使用红外光谱仪、紫外-可见分光光度计、核磁共振波谱仪、热重分析仪、示差扫描量热仪等表征了萘基环氧树脂的结构及耐热性能,测定了其环氧值和氯含量。设计正交试验,研究2,7-二羟基萘和环氧氯丙烷原料物质的量比、催化剂四丁基溴化铵和氢氧化钠用量对产物环氧值、产率和氯含量的影响。结果表明,制备的萘基环氧树脂的耐热性较纯环氧树脂高。在不同实验条件下,得到的产物环氧值最高可达0.461 mol/100 g,产率最高可达81.3%,无机氯和可水解氯含量最低可达14μg/g和491μg/g。

In order to improve the heat resistance of epoxy resin,the rigid group naphthalene ring structure was introduced into the epoxy resin skeleton to prepare heat-resistant naphthyl epoxy resin. Infrared spectrometer,ultraviolet-visible spectrophotometer,nuclear magnetic resonance spectrometer,thermogravimetric analyzer,differential scanning calorimeter were used to characterize the structure and heat resistance of the resultant naphthyl epoxy resin.The chlorine content and epoxy value of the resin were determined.The orthogonal experiments were designed to study the effects of the ratio of the raw materials of 2,7-dihydroxynaphthalene and epichlorohydrin,the amounts of catalyst tetrabutylammonium bromide and sodium hydroxide on the epoxy value,yield and chlorine content of the product. The results showed that the prepared naphthyl epoxy resin had higher heat resistance than the pure epoxy resin. Under different experimental conditions,the epoxy value of the obtained product could reach as high as 0.461 mol/100 g,the yield reached as high as 81.3%,and the content of inorganic chlorine and hydrolyzable chlorine could reach as low as 14 μg/g and491 μg/g,respectively.