SnCl4改性阳离子交换树脂催化合成柠檬酸三丁酯

以柠檬酸和正丁醇为原料,SnC l4改性阳离子交换树脂为催化剂,合成了柠檬酸三丁酯。FTIR和X射线荧光光谱表征结果表明,用SnC l4对阳离子交换树脂进行改性后,树脂骨架结构变化不大,Sn4+的负载量达13.47%(质量分数,下同)。合成柠檬酸三丁酯的最佳工艺条件为:反应温度155℃,反应时间6 h,n(正丁醇)∶n(柠檬酸)=4.1∶1,催化剂用量为反应物总质量的4.5%,柠檬酸三丁酯的产率可达97.3%。催化剂不经任何处理重复使用8次后,产率仍为96%。

Synthesis of Tributyl Citrate with Cation Exchange Resin Modified by SnCl4

The synthesis of tributyl citrate with citric acid and n-butanol alcohol as base material and catalyzed by cation resin modified by SnCl4 was investigated.As is shown in the results of characterization by means of Fourier transform infrared spectrum and X-ray fluorescence spectrum,the skeleton structure of the resin experienced little change and the loading factor of Sn4+ was 13.47% after it was modified by SnCl4.The optimization of reaction parameters was performed,showing that a maximum yield of tributyl citrate of 97.3% could be obtained under the following conditions:temperature was 155 ℃,duration was 6 h,molar ratio of n-butanol to citric acid was 4.1∶1 and catalyst dosage was 4.5% of the total mass of reactants.The catalyst could be reused 8 times without any disposal and the yield still reached 96%.