NaHSO_3法分离紫罗兰酮异构体过程研究

Study on separation process of ionone isomers by NaHSO_3 method

采用NaHSO_3为亲核试剂与紫罗兰酮异构体反应生成α-羟基磺酸钠,利用紫罗兰酮异构体的NaHSO_3加成物在碱液中分解再生速度的不同实现α-紫罗兰酮和β-紫罗兰酮的分离。重点考察了水、助剂、物料摩尔比、反应温度及反应时间对紫罗兰酮转化率的影响,同时探讨了溶液pH对β-紫罗兰酮收率及纯度的影响。结果表明,在最优反应条件下,α-羟基磺酸钠合成过程中紫罗兰酮的转化率可达98%以上;通过调节溶液pH至最优范围内,可得到纯度高于95%且收率在75%以上的β-紫罗兰酮;继续调节溶液pH至13.5,经多次回收富集后可得到纯度高于90%的α-紫罗兰酮。

NaHSO3 is used as a nucleophile reagent to react with the ionone isomers to synthesize sodium alpha hydroxy sulfonate.The separation of α-ionone and β-ionone is achieved by the different decomposition and regeneration rates of the NaHSO3 adduct substances with different ionone isomers.The effects of water,assistants,molar ratio between materials,reaction temperature and reaction time on the conversion of ionone are investigated.The influence of pH value on the yield and purity of β-ionone is also studied. The results show that the conversion rate of ionone can exceed 98%under the optimum reaction conditions during the synthesis process of sodium alpha hydroxy sulfonate,and the purity ofβ-ionone can exceed 95% while its yield can be above 75% by adjusting the pH value of the solution into the optimum range.Furthermore,α-ionone with a purity of more than 90% can be recovered by continuing to adjust the pH value to13. 5 and through multiple enrichments.