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采用原位合成法将Keggin型结构的磷钨酸(PW_(12))负载于分子筛SBA-15上,制备出负载型催化剂,利用XRD、N2吸附-脱附、FTIR、NH3-TPD等技术对其进行表征。将负载型催化剂PW_(12)-SBA-15用于柠檬酸三丁酯(TBC)的催化合成,并对多种影响因素进行了分析。结果表明:SBA-15及PW_(12)的基本结构均能得到保持,催化剂具有良好的酸性中心;当PW_(12)负载量为27%、催化剂用量为1.4%、醇酸摩尔比为4:1、反应温度为150℃、反应时间为6 h时,酯化率达到95.59%;催化剂重复应用10次,催化性能稳定。
The in-situ synthesis method was used to prepare the supported catalyst by loading phosphotungstic acid (PW 12) with Keggin structure onto molecular sieve SBA-15. The supported catalysts were characterized by XRD, N2 adsorption-desorption, FTIR and NH3-TPD It is characterized. The supported catalyst PW_ (12) -SBA-15 was used for the catalytic synthesis of tributyl citrate (TBC), and various influencing factors were analyzed. The results show that the basic structure of SBA-15 and PW 12 can be maintained and the catalyst has a good acidic center. When PW 12 loading is 27%, catalyst dosage is 1.4% and molar ratio of alkyd to acid is 4: 1, the reaction temperature was 150 ℃, the reaction time was 6 h, the esterification rate reached 95.59%; the catalyst was applied 10 times repeatedly, the catalytic performance was stable.