2,2'-亚甲基双(4-叔丁基苯基)磷酰氯的制备及表征  

Preparation and Characterization of 2,2'-Methylene-bis( 4-tert-butylphenyl) Phosphate Chloride

作　　者：黄金[1,2] 张凯[1,2] 于杰[1,2] 杨应娟[1,2] 秦舒浩[2] 何文涛[2] 

机构地区：[1]贵州大学材料与冶金学院,贵州贵阳550025 [2]国家复合改性聚合物材料工程技术研究中心,贵州贵阳550014

出　　处：《塑料工业》2014年第9期84-87,共4页China Plastics Industry

基　　金：贵州省国际科技合作项目(黔科合外G字[2012]7029号);国家支撑计划课题(2013BAB07B03)

摘　　要：以2,2'-亚甲基-双(4-叔丁基苯)酚和三氯氧磷为原料,通过滴加缚酸剂和催化剂三乙胺,反应生成了2,2'-亚甲基双(4-叔丁基苯基)磷酰氯。主要研究了加料顺序、时间、温度和溶剂量对反应产物和收率的影响。当滴加三乙胺,加入25 mL溶剂,反应时间2 h和反应温度为45℃时收率可以达到68%。对产物进行了傅里叶红外变换光谱仪(FTIR)、核磁共振仪(NMR)、质谱仪(MS)和差式扫描量热分析(DSC)表征,各项检测表明,合成的产物为2,2'-亚甲基双(4-叔丁基苯基)磷酰氯。2,2＇-Methylene-bis （4-tert-butylphenyl） phosphate chloride was synthesized through drop wise acid binding agent and catalyst triethylamine with 2,2＇-methylene-bis （4-tertbutylphenol） and phosphorns oxychloride.The influences of the addition order,the time,the temperature and amount of the solvent on the yield of the product were discussed.The result showed adding triethylamine,the reacting temperature was 45 ℃,the reacting time was 2 h and amount of the solvent was 25 ml,the yield of the product with good quality was 68％.The structure of the product was characterized by FT-IR,DSC,1H-NMR and MS methods.The result indicated that the structure of the product was consistent with that of 2,2＇-methylene-bis （4-tert-butylphenyl） phosphate chloride.

关 键 词：2 2'-亚甲基双(4-叔丁基苯基)磷酰氯 三乙胺 工艺条件 收率 

分 类 号：TQ314.24[化学工程—高聚物工业]