硅胶负载型催化剂催化合成新型增塑剂柠檬酸三戊酯

Synthesis of new-style plasticizer tri(n-amyl)citrate catalyzed by silica gel load-typed catalyst

以硅胶负载型Ti(SO4)2、Zr(SO4)2、Fe2(SO4)3、Se(SO4)2为催化剂,由柠檬酸和正戊醇合成新型增塑剂柠檬酸三戊酯,考察了各反应因素对酯化率的影响。结果表明,在柠檬酸与正戊醇物质的量比为1∶4.0,硅胶负载Ti(SO4)2用量为柠檬酸总量的3%,催化剂活化温度400℃,反应温度155～165℃和反应时间3.0 h条件下,柠檬酸三戊酯的酯化率可达到97.2%,纯度经气相色谱分析大于99%。催化剂硅胶负载Ti(SO4)2重复使用多次,活性未见明显降低。

New-style plasticizer tri（n-amyl） citrate was synthesized from citric acid and n-amyl alcohol using silica gel load-typed Ti（SO4）2,Zr（SO4）2,Fe2（SO4）3,Se（SO4）2 as the catalyst.Effects of esterification rate of different factors on the reaction were investigated.The results indicated that the amount of citric acid to n-amyl alcohol was 1 ∶ 4.0,the dosage of silica gel load Ti（SO4）2 was 3% of the total citric acid,the catalyst activation temperature was 400 ℃,the reaction temperature was 155-165 ℃,and the reaction time was 3.0 h,tri（n-amyl） citrate yield of 97.2% was attained,the purity determined by GC was over 99%.When the catalyst was repetitively used,the active didn＇t reduce obviously.