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机构地区:[1]阜宁县安勤化学有限公司,江苏阜宁224403 [2]盐城工学院化学与生物工程学院,江苏盐城224051
出 处:《盐城工学院学报(自然科学版)》2012年第1期15-18,57,共5页Journal of Yancheng Institute of Technology:Natural Science Edition
基 金:国家自然科学基金面上项目(31170543);应用化学江苏省重点学科建设开放基金项目(XKY2009005)
摘 要:以环氧氯丙烷(ECH)和叔丁醇(TBA)为原料,经加成反应和环化作用,合成了缩水甘油基叔丁基醚(TBGE);研究了催化剂类型、ECH与TBA物料比、催化剂用量、加成反应温度及时间等因素对TBGE收率的影响,用气相色谱法分析了产品中TBGE含量,GC-MS和FT-IR等表征了产物结构。实验结果表明,三氟化硼(BF3)-乙醚是性能优良的催化剂;在BF3-乙醚的用量为TBA质量的3.0%、加成反应的温度和时间分别为50.0℃和5.0 h、nECH/nTBA为2.5的条件下,TBGE的收率可达85%以上;气相色谱的分析结果表明产品中TBGE含量在99.0%以上。The tert-butyl glycidyl ether(TBGE) was synthesized through additive reaction and cyclic action with epichlorohydrin(ECH) and tert-butanol(TBA) as raw materials.The effects of catalyst type,the amount of catalyst,the temperature and time of addition reaction and the molar ratio of ECH versus TBA on the yield of TBGE were investigated.The content of TBGE in product was determined by GC and the structure of product was characterized by GC-MS and FT-IR.When the BF3-etherate was utilized as catalyst and the mass ratio of BF3-etherate versus TBA was 3.0%,the temperature of addition reaction was 50.0 ℃,reaction time was 5.0 h,and the molar ratio of ECH versus TBA was 2.5,experimental results indicated the yield of TBGE was above 85 %.The result of GC showed the content of TBGE in the product surpassed 99.0%.
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