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机构地区:[1]西北师范大学化学化工学院,甘肃兰州730070 [2]河南理工大学理化系,河南焦作454000
出 处:《化工时刊》2009年第1期14-17,共4页Chemical Industry Times
基 金:河南省基础与前沿技术研究计划项目(072300460050);河南省教育厅创新人才支持计划项目(2009HASTIT021);甘肃省高分子材料重点实验室资助项目(ZD-04-11)
摘 要:采用回流蒸发吸附法制备聚苯胺掺杂磷钨杂多酸,用红外光谱和X-射线粉末衍射表征其结构并进行了热重分析;以之为催化剂,通过柠檬酸和异辛醇反应合成了柠檬酸三辛酯(2-乙基己酯),探讨了磷钨酸掺杂聚苯胺催化剂对酯化反应的催化活性。利用单因素法系统考察了酸醇物质的量比,催化剂用量以及反应时间诸因素对产品收率的影响。确定了最佳的反应条件,即在柠檬酸为0.025 mol时,使醇酸物质的量比为1∶5,反应时间2.0 h,反应温度为150℃,催化剂使用量为1.4 g时,酯化率可达95.8%。另外,催化剂的稳定性试验表明,4次反应的酯化率依次有所降低。The catalyst of phosphotungstic acid doped polyaniline was prepared via adsorption through reflux and evaporation. The catalyst was characterized by FTIR, XRD spectroscopy as well as thermogravimetry. Trioctyl citrate was synthesized by citric acid together with isooctyl alcohol catalyzed by the same catalyst and then its activity per-formance could also be made available, simultaneously. Several factors including the amount of catalyst, the ratio of acid to alcohol and reaction times were discussed by means of single factor experiment to get the optimum conditions. The yield was up to 95.8% under the optimum reaction condition' as the molar ratio of citric acid to isooctyl alcohol was 1:5, the reaction time was 2.0 h, mass of catalyst was 1.4 g, the reaction temperature was at 145℃ and the amount of citric acid was 0. 025 mol. The recycling tests showed that the conversion of the reaction catalyzed decreased to some extent after being reused repeatedly for four times.
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