系统地研究了无溶剂条件下,H2O2为氧源,反应控制相转移催化剂[(C16H33(70%)+C18H37(30%))N(CH3)3]3[PW4O16]催化氯丙烯环氧化制环氧氯丙烷反应.结果表明,在氯丙烯/H2O2/催化剂(摩尔比)=400∶100∶1条件下,50~55℃反应3 h,环氧氯丙烷的收率为85~87%.在NaH2PO4存在下,催化剂循环使用5次,活性无明显降低,新鲜催化剂和回收催化剂的31P MAS NMR谱分析结果表明NaH2PO4对催化剂结构和组成具有稳定作用.
Epoxidation of allyl chloride without solvent catalyzed by reaction controlled phase transfer catalyst [(C16H33(70%)+C18H37(30%))N(CH3)3]3[PW4O16] using H2O2 as oxidant was described.Under the optimized conditions(allyl chloride / H2O2/catalyst(molar ratio) =400∶100∶1,50~55 ℃,3 h.),85~87% yield of epichlorohydrin was obtained.The catalyst can be reused with good stability in the presence of NaH2PO4.The structure and the composition of the fresh catalyst and the recovered catalysts were investigated by 31P MAS NMR spectra..The results demonstrated that NaH2PO4 could keep the catalyst stable.