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采用过硫酸氢钾复合盐(Oxone)/丙酮体系制备二甲基双环氧乙烷(DMD)环氧化LMPIB(低相对分子质量聚异丁烯)。探讨了反应体系中溶剂、n(Oxone)∶n(NaHCO3)比例、V(H2O)∶V(丙酮)比例、反应温度和反应时间等对产物的双键转化率、环氧值和环氧收率的影响。结果表明:采用单因素试验法优选出DMD环氧化LMPIB的适宜工艺条件是“0~5℃反应0.5 h→25℃反应1.5 h”、n(Oxone)∶n(NaHCO3)=1∶2.40和V(H2O)∶V(丙酮)=5∶4,即反应体系中水150 mL、丙酮120 mL、Oxone和NaHCO3分别为23.05 g和15.12 g;此时,环氧化LMPIB的环氧值0.138 8 mol/100 g、双键转化率62.68%和环氧收率67.10%。
Dimethyldioxirane (DMD) epoxidized LMPIB (low molecular weight polyisobutylene) was prepared by oxone / acetone system. The double bond conversion rate, epoxy value and epoxy yield of the products such as the ratio of n (Oxone): n (NaHCO3), V (H2O): V (acetone), reaction temperature and reaction time were discussed. Rate of impact. The results showed that the optimal process conditions for the DMD epoxidation of LMPIB by single factor test were as follows: “reaction at 0 ~ 5 ℃ for 0.5 h → reaction at 25 ℃ for 1.5 h”, n (Oxone): n (NaHCO3) = 1: 2.40 and V (H2O): V (acetone) = 5: 4, namely, the reaction system water 150 mL, acetone 120 mL, Oxone and NaHCO3 were 23.05 g and 15.12 g; At this time, epoxidized LMPIB epoxy value 0.138 8 mol / 100 g, double bond conversion 62.68% and epoxy yield 67.10%.