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三苯基膦与三苯基氧膦分离
引用本文:王庭恭,倪蕾蕾,何佳玲,刘剑,励华群,杨泽慧.三苯基膦与三苯基氧膦分离[J].宁波工程学院学报,2009,21(3):71-76.
作者姓名:王庭恭  倪蕾蕾  何佳玲  刘剑  励华群  杨泽慧
作者单位:宁波工程学院,浙江,宁波,315016
摘    要:研究了用化学反应一结晶联用法从wittig反应废渣中回收三苯基膦(TPP)和三苯基氧膦(TPPO)的分离技术,探讨了各种条件对产品纯度和回收率的影响。结果表明,洗涤酸对样品中的TPP和TPPO无影响;处理量的大小对产品无影响;洗涤过的干燥样品与浓硫酸反应生成沉淀,抽滤,滤液用饱和碳酸氢钠洗至中性,旋干,用氨苯重结晶,得TPP,收率为92%,滤渣用氯苯和饱和碳酸氢钠处理,将有机层浓缩,得TPPO,收率为98%。产品经红外分析、高效液相色谱和熔点测定,与文献值一致。

关 键 词:化学反应-结晶联用法  三苯基膦  三苯基氧膦  分离

Separation of Triphenylphosphine and Triphenylphosphine Oxide
WANG Ting-gong,NI Lei-lei,HE Jia-ling,LIU Jian,LI Hua-qun,YANG Ze-hui.Separation of Triphenylphosphine and Triphenylphosphine Oxide[J].Journal of Ningbo University of Technology,2009,21(3):71-76.
Authors:WANG Ting-gong  NI Lei-lei  HE Jia-ling  LIU Jian  LI Hua-qun  YANG Ze-hui
Affiliation:Ningbo University of Technology;Ningbo;Zhejiang;315016;China
Abstract:The paper studies the new process for recovering triphenylphosphine and triphenylphosphine oxide from the waste residue produced by Witting reaction and discusses the effect of various conditions on the purity and the recovery of the product.Results show that washing acid won't affect the TPP and TPPO in the sample,nor will the feed on the product;Precipitation is formed when the dry sample washed reacts with the concentrated sulfuric acid.TPPO is obtained in 98% yield(99.5% in purity by HPLC) while the pre...
Keywords:chemical reaction and crystallization method  triphenylphosphine  triphenylphosphine oxide  separation  
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