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固体超强酸S2O82-/SnO2-SiO2催化合成增塑剂柠檬酸三丁酯
Catalytic synthesis of plasticizer tributyl citrate with solid superacid S2O82-/SnO2-SiO2
【摘要】 在固体超强酸S2O28-/SnO2-SiO2的催化下,以柠檬酸和正丁醇为原料,合成了标题化合物。实验结果表明,固体酸S2O82-/SnO2-SiO2催化合成柠檬酸三丁酯的最佳工艺条件为:催化剂用量占柠檬酸质量的2%,n(柠檬酸)∶n(正丁醇)=1∶4,回流温度120℃,反应时间4 h,酯化率96.2%,催化剂经重复使用5次,活性未见明显降低。产品经红外光谱、核磁进行定性分析,纯度经气相色谱分析>99.0%。
【Abstract】 A non-toxic plasticizer tributyl citrate was synthesized by the reaction of citric acid with n-butanol using solid superacid S2O2-8/SnO2-SiO2 as the catalyst.Experiment results indicated that the optimum process conditions were as follows.The mole ratio of citric acid to n-butanol was 1∶4.The amount of catalyst was 2 percent of the mass of citric acid.The refluxing temperature was 120 ℃ and the reaction time was 4 h,with the esterification yield reaching up to 96.2%.The catalyst after having been used for 5 times,didn′t show significant decline in its activity.The qualitative analysis of product was carried out by using IR and NMR spectroscopy.The purity of product analyzed by GC was above 99.0%.
【Key words】 solid superacid; plasticizer; catalytic synthesis; tributyl citrate;
- 【文献出处】 化学试剂 ,Chemical Reagents , 编辑部邮箱 ,2010年11期
- 【分类号】TQ414
- 【被引频次】21
- 【下载频次】266