【作者】 于坤；

【导师】 陈霄榕；

【作者基本信息】 河北工业大学 ， 化学工艺， 2013， 硕士

【摘要】 环戊醇是一种贵重的精细化工原料，广泛的应用于制药、染料、香料等工业，是有机合成中重要的中间体。合成环戊醇的方法主要有己二酸法、环戊烯硼氢化-氧化法、环戊烯水合法等。近年来石油化工的迅速发展使环戊烯资源日趋丰富，国内外学者对环戊烯水合制备环戊醇的研究也越来越重视。目前的水合方法有间接法和直接法。直接水合法与硫酸间接水合法相比，虽然单程转化率较低，但由于环戊烯沸点较低可以循环使用，所产生的污染物较少，属于环境友好工艺，有很大的发展前景。本论文是以环戊烯为原料，采用自制的固体超强酸作催化剂一步催化水合制备环戊醇。本文首先对环戊烯水合反应的固体超强酸催化剂进行了改性研究，利用沉淀-浸渍法制备了SO₄²-/SnO₂、SO₄²-/SnO₂-SiO₂、S₂O₈²-/SnO₂-SiO₂三种固体超强酸催化剂，通过BET、IR、XRD、NH₃-TPD和TG对催化剂进行表征，结果显示引入二氧化硅可以明显增加催化剂的比表面积，使固体超强酸表面的催化活性中心增多；并考察了催化剂的制备条件，得出最佳的催化剂制备条件为：（NH₄）NO₃为酸性沉淀剂，m（SnO₂）:m（SiO₂）=1:1，浸渍液浓度为3mol/L，焙烧温度500℃。然后对催化剂SO₄²-/SnO₂-SiO₂催化环戊烯水合制备环戊醇的工艺条件进行了优化，得到最佳的工艺条件为：环戊烯的质量=溶剂苯酚的质量，水烯摩尔比为6:1，催化剂的质量为H2O质量的15%，反应温度130℃，反应时间4h，反应初始压力1.5MPa，搅拌速度600r/min，在上述条件下环戊烯的转化率为9.65%，环戊醇的选择性为97.73%。更多还原

【Abstract】 Cyclopentanol is a kind of valuable fine chemical raw materials which widely used inpharmaceutical, dye, spices, and other industries and also is an important intermediate fororganic synthesis. Cyclopentanol can be prepared by adipic acid、borohydride-oxidation andhydration of cyclopentene. With the rapid development of the petroleum chemical industry inrecent years, cyclopenten resource is rich. Scholars both at home and abroad pay attention tostudy on the preparation of cyclopentanol by catalysis hydration of cyclopenten.The present hydration method is the indirect hydration and the direct hydration ofcyclopenten. Compared with indirect hydration of H2SO4, Direct hydration has disadvantages oflow conversion, but it has advantages of less waste pollution, recycling of cyclopentene whichhas low boiling point and so on. Therefor, Direct hydration belongs to the environmental friendlyprocess and has very good development prospect. This paper prepared cyclopentanol usedcyclopenten as raw material by one-step catalyze hydration using self-regulating solid superacidas catalyst.Firstly, the modification on solid superacid catalyst of hydration reaction is studied. Thethree kinds of catalysts were prepared via impregnation-deposition method. The acid strengthand structure of the solid superacid were characterized by BET、IR、XRD、NH3-TPD and TG.The results showed that the introduction of SiO₂can increase specific surface area of catalyst,concequently increasing the activty centre of solid super acid surface. It was found that catalyst,SO42/SnO₂-SiO₂, had optimum activity. Furthermore, the suitable conditions of preparation ofthe catalyst were obtained: acid precipitant is （NH₄）NO₃, m（SnO₂）:m（SiO₂）=1:1, the concentration of impregnant is3mol/L, the calcination temperature is500℃.Secondly, The cyclopentanol was synthesized by hydration reaction of cyclopentene,catalyzed by solid superacid of SO₄²/SnO₂-SiO₂.The influencing factors of the hydration havebeen discussed. The optimal reaction conditions were as followings: the quality of phenol equalsto the quality of cyclopentene, that molar ratio of H2O to cyclopentene was6:1, the quality ofcatalyst equals to15%water’s quality mass, the reactive temperature was130℃, reaction timewas4h, the initial pressure was1.5MPa, stirring speed was600r/min. Under these conditions, theconversion of cyclopentene was9.65%, and the selectivity to cyclopentanol was97.73%.更多还原