摘要
采用碾磨-活化法制备了SiO2-ZnCl2(Silzic)催化剂,并将其用于异丁烯与甲醛Prins缩合合成3-甲基-3-丁烯-1-醇(MBOH)。系统研究了温度、物料比、时间和催化剂的组成及用量对该反应的影响。结果表明,在不同的条件下,甲醛都保持着99%以上的高转化率;然而,不同的条件对MBOH的选择性和收率的影响程度不同,其中,反应温度、催化剂的酸量是影响该反应的关键因素;物料比和反应时间对MBOH的选择性和收率的影响相对较小。实验得到最佳的反应条件为,反应温度210℃、二氧六环8 g、三聚甲醛1.5 g、n(异丁烯)/n(三聚甲醛)=7∶1、30 mg 1 mmol/g Silzic和反应时间2 h,在此条件下MBOH的选择性和收率可分别达到93.8%和93.4%。当催化剂循环使用五次时,MBOH的收率降为85.2%,表明该催化剂具有一定的重复使用性。
Immobilized ZnCl2（Silzic） catalyst was prepared and used in the synthesis of 3-methyl-3-buten-1-ol（MBOH） from isobutylene and formaldehyde;the effects of the reaction parameters,such as temperature,molar ratio of isobutene to formaldehyde,reaction time and catalyst content on the reaction behavior w ere investigated.The results show ed that the conversion of formaldehyde is over 99% under various conditions.The reaction temperature as w ell as the catalyst acidity and the amount of the acid sites are dominant factors in influencing the selectivity to MBOH.Under the optimum reaction conditions,i.e.210 ℃,8 g 1,4-dioxane,1.5 g polyoxymethylene,n（isobutylene） / n（polyoxymethylene） ratio of 7,30 mg Silzic（1 mmol / g）,and reaction time of 2 h,the selectivity and yield of MBOH reach 93.8% and 93.4%,respectively.The Silzic catalyst exhibits certain reusability;the yield of MBOH remains 85.2% after reusing the catalyst for 5 times.
出处
《燃料化学学报》
EI
CAS
CSCD
北大核心
2013年第9期1146-1152,共7页
Journal of Fuel Chemistry and Technology
