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1,4-二氧杂螺[4.5]癸烷-8-酮的回收与提纯
引用本文:武生喜,董兆恒,王建文,闫刚,刘骞峰,杨学军,杨东杰,冯星. 1,4-二氧杂螺[4.5]癸烷-8-酮的回收与提纯[J]. 应用化工, 2009, 38(9): 1388-1390
作者姓名:武生喜  董兆恒  王建文  闫刚  刘骞峰  杨学军  杨东杰  冯星
作者单位:西安瑞联近代电子材料有限责任公司,陕西,西安,710077
基金项目:西安市重点技术创新项目 
摘    要:在生产液晶中间体4-羟基-4-(2,3-二氟-4-正丁氧基)苯基环己酮的废液中含有10%~30%的1,4-二氧杂螺[4.5]癸烷-8-酮,采用亚硫酸氢钠盐析法得到磺酸盐与有机物分离,然后还原得到1,4-二氧杂螺[4.5]癸烷-8-酮粗品,再经过重结晶得到合格的目的产品,GC含量>99.5%,回收率>80%。并对产品进行了GC-MSS,DCS,IR,1H NMR的确认。

关 键 词:1,4-二氧杂螺[4.5]癸烷-8-酮  单保护  合成  提纯

Recycling and purification of 1,4-dioxaspiro[4.5]decan-8-one
WU Sheng-xi,DONG Zhao-heng,WANG Jian-wen,YAN Gang,LIU Qian-feng,YANG Xue-jun,YANG Dong-jie,FENG Xing. Recycling and purification of 1,4-dioxaspiro[4.5]decan-8-one[J]. Applied chemical industry, 2009, 38(9): 1388-1390
Authors:WU Sheng-xi  DONG Zhao-heng  WANG Jian-wen  YAN Gang  LIU Qian-feng  YANG Xue-jun  YANG Dong-jie  FENG Xing
Abstract:In the production of liquid crystal intermediates 4-hydroxy-4-(2,3-difluoro-4-n-butoxy) phenyl cyclohexanone liquid containing 10%~30% of 1,4-dioxaspirodecan-8-one,by using sodium bisulfite salting-out method with organic acid salt with organic separation,then 1,4-dioxaspirodecan-8-one was obtained.After crystallization of qualified products,content of target product.GC is over 99.5%.Recovery is over 80% and the products were characterized by GC-MSS,IR,1H NMR.
Keywords:1
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