5-异辛基水杨醛肟氨肟化及Minitab参数优化

Optimization of 5-iso-octyl Salicylic Aldehyde Aminoximation and MINITAB Parameters

以TS-1分子筛为催化剂,以5-异辛基水杨醛(ISA)、氨水和过氧化氢为原料进行直接氨肟化合成5-异辛基水杨醛肟(ISAO).借助Minitab软件进行正交试验对催化剂用量、反应温度、反应时间、氨醛物质的量比和过氧化氢醛物质的量比等反应条件进行优化,确定了最佳反应参数:5-异辛基水杨醛与过氧化氢、氨水的物质的量比分别为1∶1.3和1∶1.8,反应温度为65℃,TS-1的用量为17.5 g/mol(5-异辛基水杨醛),加料时间1 h.实验表明5-异辛基水杨醛肟(ISAO)的收率高达95.80%,该方法反应条件温和,避免了硫酸铵副产物的产生,无环境污染.

5-isooctylsalicylaldehydeoxime(ISAO)was synthesized by direct ammoximation of 5-isoo-ctylsalicylaldehyde(ISA),ammonia and hydrogen peroxide using TS-1 titanium silicalite-1 as catalyst.With the help of Minitab software,the orthogonal test was carried out to optimize the reaction parameters,such as the amount of catalyst,reaction temperature,reaction time,the molar ratio of ammonia to aldehyde and the molar ratio of hydrogen peroxide to aldehyde.The optimal reaction parameters were determined as follows:the molar ratio of 5-isooctylsalicylaldehyde and hydrogen peroxide or ammonia were 1∶1.3 or 1.8,respectively;the reaction temperature was 65℃;the dosage of TS-1 was 17.5 g/(mol 5-isooctylsalicylaldehyde);and the feeding time was 1 hour.Under these reaction conditions,the yield of 5-isooctylsalicylaldoxime(ISAO)was 95.80%.This method has mild reaction conditions without by-products of hydroxylamine salt byproducts and environmental pollution.