过氧化新癸酸叔丁酯的合成研究

Study of the synthesis of tert-butyl peroxyneodecanoate

以叔丁醇和新癸酰氯为原料,合成了过氧化新癸酸叔丁酯引发剂。第一步是以叔丁醇、浓硫酸和双氧水为原料合成叔丁基过氧化氢,考察了叔丁基过氧化氢的合成反应条件。结果表明,在硫酸浓度80%,硫酸与叔丁醇摩尔比1.2∶1,双氧水与叔丁醇摩尔比1.3∶1,反应温度5~10℃,酯化时间和氧化时间1.5 h和2.0 h条件下,叔丁基过氧化氢的收率可达64.9%。第二步是以新癸酰氯和叔丁基过氧化氢、氢氧化钠为原料,合成过氧化新癸酸叔丁酯引发剂。考察了其合成条件,结果表明,在反应时间1.5 h,新癸酰氯与叔丁基过氧化氢摩尔比为1∶1.2,反应温度20℃条件下,过氧化新癸酸叔丁酯的收率为74.3%。

Initiator tert-butyl peroxyneodecanoate was synthesized from tert-butanol and neodecanoyl chloride. The first step is the synthesis of tert-butyl hydroperoxide from tert-butanol,concentrated sulfuric acid and hydrogen peroxide. The reaction conditions of tert-butyl hydroperoxide synthesis were investigated.The results showed that when the concentration of sulfuric acid was 80%,the molar ratio of sulfuric acid to t-butyl alcohol was 1. 2∶ 1,the molar ratio of hydrogen peroxide to tert-butyl alcohol was 1. 3∶ 1,the reaction temperature was 5 ~ 10 ℃,the esterification time and oxidation time were 1. 5 h and 2. 0 h. Under this condition,tert-butyl hydroperoxide yield is up to 64. 9%. The second step is to synthesize tert-butyl peroxyneodecanoate as initiator by using neodecanoyl chloride,t-butyl hydroperoxide and sodium hydroxide as raw materials. The synthesis conditions were investigated. The results showed that when the reaction time was 1. 5 h,the yield of tert-butyl peroxyneodecanoate was 74. 3% with the molar ratio of decanoyl chloride to tert-butyl hydroperoxide being 1∶ 1. 2 and the reaction temperature being 20 ℃.