邻苯二甲酸二缩水甘油酯合成的工艺条件研究

Studying the Technology Condition of the Synthesis with O-phthalic Acid and Glycerin Losing Water Molecular

以邻苯二甲酸酐和环氧氯丙烷为原料合成环氧树脂。采用L18（3^7）正交表设计试验，分别考察环氧氯丙烷、水、四丁基溴化铵的用量、酯化时间、氢氧化钠浓度和闭环时间等六个影响因素对环氧树脂合成的影响，最佳工艺条件为：邻苯二甲酸酐、环氧氯丙烷和水的配摩尔比为1：2．2：4／3，反应温度为100～110℃下，催化剂四丁基溴化铵的用量为2．2％，皂化反应时间为135分钟，在常温下25％的氢氧化钠条件下闭环反应60分钟；该条件下得到的产品外观无色清亮，有较高的产率（75．7％）与环氧值（0．6358），其中无机氯含量为0．0027％，可水解氯含量为0．0019％，改变了以往产品为黄色的缺陷，可水解氯的含量达到微电子工业环氧树脂中氯含量小于0．005％的要求。

The tetrabutylamlomium bromide has been compounded by o-phthalic anhydride and epichlorohydrin. Six factors for the synthesis tetrabutylamlomium has been investigated with the quantum of the epichlorohydrin , water and tetrabutylammonium bromide, the time of the esterification, density of the sodium hydroxide and the time of closed loop, respectively, throng orthogonal design L18（37） experiment. The best technology condition shows that the mole ratio of the o-phthalic anhydride, epichlorohydrin and water is 1：2.2：4/3, the react tempera ture is 100-110℃ and the time of the koettstorfffer is 135 minutes, the mass percent of the catalyst of tetrabuty lammonium bromide is 2.2%, the closed loop time is 60 minutes with 25% sodium hydroxide at the common temperature. The product looks colorless clearlight, with high productive rate about 75.7% and epoxide number about 0. 6358 synthesis at this condition. The percent of inorganic chlorine concentration in the product is 0. 0027% and the hydrolyzable chlorine concentration is 0. 0019% Changed . The shortcoming of the product, which is yellow color in the past has been changed. Hydrol yzable chlorine concentration has been up to scratch the qualification of the chlorine concentration of the tetrabutylamlomium bromide in the microelectronics industry is lower than 0. 005%.