SnCl4改性阳离子交换树脂催化合成柠檬酸三丁酯

Synthesis of Tributyl Citrate with Cation Exchange Resin Modified by SnCl4

摘要:

以柠檬酸和正丁醇为原料， SnCl4改性阳离子交换树脂为催化剂，直接酯化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SnCl4对阳离子交换树脂进行改性后，树脂骨架结构变化不大，Sn4+的负载量达到13.47%。SnCl4改性阳离子交换树脂催化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%，在此条件下，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，产率仍高达96%。

Abstract:

The synthesis of tributyl citrate catalyzed by cation exchange resin modified by SnCl4 was investigated.As shown in the results of Fourier transform infrared spectrum and X-Ray fluorescence spectrum, the skeleton structure has not changed and loading factor of Sn4+ is 13.47% after modified by SnCl4. The optimization of reaction parameters was performed ,showing that maximum yield of tributyl citrate of 97.3% could be obtained under the conditions that temperature was 155 ℃,duration was 6 h,molar ratio of n-butanol to citric acid was 4.1:1 and catalyst amounts was 4.5%(based on the total mass of reactants).The catalyst could be reused 8 times without any disposal and the yield still reached 96%.