【作者】 刘小欢；

【导师】 许振良； 曾义红；

【作者基本信息】 华东理工大学 ， 化学工程， 2012， 硕士

【摘要】 本文采用溶胶-凝胶法制备了催化剂PFSA/SiO2和PFSA/SiO2-Co0.5Fe2.5O4。运用XRD、BET、TG-DTA和FTIR等分析测试手段对催化剂的结构和性能进行了表征,分析和测试了催化剂的磁学性能；分别用于乙酸乙酯、乙酸异丙酯和乙酸正丁酯酯化反应,考察了催化剂用量、酸醇摩尔比、反应温度、反应时间对乙酸乙酯、乙酸异丙酯及乙酸正丁酯收率的影响；制备了挤条成型催化剂PFSA/SiO2,并考察了成型条件对催化剂结构和性能的影响。具体结果如下：首先,采用XRD、BET、TG、FTIR等方法进行了表征,结果表明活性组分全氟磺酸树脂和磁性材料Co0.5Fe2.5O4均匀分布在多孔二氧化硅载体上,催化剂有较好的孔径和比表面积。同时,催化剂表现出一定的磁性性能。其次,将全氟磺酸树脂制成全氟磺酸树脂溶液,通过溶胶-凝胶技术制得磁性催化剂PFSA/SiO2-Co0.5Fe2.5O4,充分暴露活性组分全氟磺酸树脂的酸性位,提高了催化剂催化活性,同时也提高了催化剂的回收利用率。在最优工艺条件下,磁性催化剂PFSA/SiO2-Co0.5Fe2.5O4催化合成乙酸乙酯、乙酸异丙酯、乙酸正丁酯的收率分别为92.8%、81.0%、92.4%。最后,采用挤条成型法制备了催化剂PFSA/SiO2,其孔径和比表面积有所下降活性降低,但仍处于较高水平。粘合剂和助挤剂对成型催化剂的强度影响明显,当粘合剂硅溶胶用量为30%,助挤剂田菁粉用量为5%,成型催化剂强度适宜。更多还原

【Abstract】 The catalysts of PFSA/SiO2 and PFSA/SiO2-Co0.5Fe2.5O4 were prepared by sol-gel method which respectively applied for esterification reaction of ethyl acetate, isopropyl acetate and n-butyl acetate. The structure and performance of the catalysts was characterized by techniques such as XRD, BET, TG and FTIR, and magnetism performance was measured as well. The effect of the yield of ethyl acetate, isopropyl acetate and n-butyl acetate was investigated by amount of catalyst, molar ratio, reaction temperature and reaction time: forming catalyst PFSA/SiO2 was prepared and the effect of structure and performance of the catalyst was researched by forming conditions. Specific results are as follows:First. the active component of perfluorosulfonic acid resin and magnetic materials Co0.5Fe2.5O4 uniformly distributed in porous silicon dioxide carrier. The pore size and specific surface area of the catalysts are good and the catalysts show some of the magnetism performance.Then, perfluorosulfonic acid resin was made to perfluorosulfonic acid resin solution. The magnetic catalyst of PFSA/SiO2-Co0.5Fe2.5O4 was obtained through sol-gel technique. Exposed the acidic position of perfluorosulfonic acid resin and improved the catalytic activity and recovery rate. The yield of ethyl acetate, isopropyl acetate and n-butyl acetate by magnetic catalyst of PFSA/SiO2-Co0.5Fe2.5O4 can reach to 92.8%,81.0% and 92.4% in the most optimal process conditions.Finally, extruded catalyst of PFSA/SiO2 was prepared. The pore size and specific surface area of the catalyst decreased, as well as the activity, but remained at a high level. Adhesives and extrusion assistant have obvious effect on strength of forming catalyst. The strength of forming catalyst is suitable when the dosage of adhesive silica sol is 30%, extrusion assistant sesbania powder is 5%.更多还原