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以H2O_2(过氧化氢)/乙酸为反应试剂、IER(离子交换树脂)为催化剂,采用原位过酸法合成了环氧化LPIB(低相对分子质量聚异丁烯)。考察了反应温度、反应时间、原料配比及IER含量等对产物的双键转化率、环氧值和环氧基团收率等影响,并采用单因素试验法优选出LPIB环氧化的最佳工艺条件。研究结果表明:LPIB的末端双键易被环氧化,并伴有一定量的副反应;LPIB环氧化的最佳工艺条件为n(双键):n(乙酸):n(H_2O_2)=1:0.7:1.65、w(IER)=13.5%(相对于树脂质量而言)、反应温度70℃和反应时间12 h,此时产物的双键转化率为86.5%、环氧值为0.083 mol/100 g和环氧基团收率为79.2%;IER循环使用4次后,其催化效率基本不变。
The epoxidized LPIB (low molecular weight polyisobutylene) was synthesized by the in situ peracid method using H2O_2 (hydrogen peroxide) / acetic acid as reagent and IER (ion exchange resin) as catalyst. The effects of reaction temperature, reaction time, raw material ratio and IER content on the double bond conversion, epoxy value and epoxy group yield of the product were investigated. Single factor test was used to optimize the epoxidation of LPIB Good process conditions. The results showed that the terminal double bond of LPIB was easily epoxidized with a certain amount of side reactions. The optimum conditions of LPIB epoxidation were n (double bond): n (acetic acid): n (H 2 O 2) = 1 : 0.7: 1.65, w (IER) = 13.5% (relative to resin mass), reaction temperature 70 ° C and reaction time 12 h, at which time the double bond conversion of the product was 86.5% and the epoxy value was 0.083 mol / 100 g and epoxy group yield of 79.2%; IER recycling after 4 times, the catalytic efficiency of the same.