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作 者:武宝萍[1] 林可宏[2] 许前会[1] 朱平华[1] 张秋荣[1]
机构地区:[1]淮海工学院化工学院,江苏连云港222005 [2]浙江台州学院,医药化工学院,浙江临海317000
出 处:《化学研究与应用》2010年第12期1492-1497,共6页Chemical Research and Application
摘 要:采用后合成法制备了介孔分子筛催化剂P-SBA-1,并用XRD和SEM对催化剂进行分析,表征结果表明催化剂P-SBA-1具有立方结构(空间点群Pm3n)。选用液体酸H2SO4和微孔分子筛HY、ZSM-5与SBA-1进行对比,结果表明催化剂的活性高低顺序为:H2SO4>SBA-1>HY>ZSM-5。将改性后的介孔分子筛P-SBA-1作为固体酸催化剂合成柠檬酸三丁酯。重点考察了催化剂用量、酸醇摩尔比、反应温度、反应时间等因素以及催化剂的重复使用性能。结果表明P-SBA-1催化合成柠檬酸三丁酯的最佳条件为:反应温度140℃,酸醇摩尔比1∶6,催化剂用量为反应物总质量的1.5%,反应时间5h。催化剂P-SBA-1重复使用性能良好。The mesoporous molecular sieve P-SBA-1 functionalized with phosphoric acid group was prepared by post-synthetic method.The samples were characterized with XRD and SEM.The results confirmed that P-SBA-1 catalyst remains the well ordered cubic structure(space group Pm3n).The catalytic activity of SBA-1,as compared with H2SO4,HY、ZSM-5,was tested on the esterification reaction of citric acid.From the results,it was clear that the activity of the catalysts for esterification of citric acid was found to follow the sequence: H2SO4SBA-1HYZSM-5.The tri-butyl citrate was prepared using P-SBA-1 as solid acid catalyst.The effects of amount of catalyst,acid/alcohol molar ratio,reaction temperature and reaction time were investigated.The optimum conditions for the synthesis of TBC over P-SBA-1 were: reaction temperature was 140℃;the ratio of citric acid to butanol was 1∶6;mass ratio of catalyst to reactant was 1.5﹪ and reaction time was 5h.The catalyst was highly stable and can be used for several times without much loss of its activity.
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