缚酸剂对合成2,2′-亚甲基双(4,6-二叔丁基苯基)磷酰氯的影响  

Effects of acid binding agents on synthesis of 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphorus oxychloride

作　　者：张达[1] 李效军[1] 申冰洁 

机构地区：[1]河北工业大学化工学院,天津300130

出　　处：《石油化工》2016年第3期335-339,共5页Petrochemical Technology

摘　　要：以2,2′-亚甲基双(4,6-二叔丁基)苯酚(简称双酚)和三氯氧磷为原料,乙腈为溶剂,合成聚丙烯成核剂NA-11(2,2′-亚甲基双(4,6-二叔丁基苯基)磷酸钠)的中间体2,2′-亚甲基双(4,6-二叔丁基苯基)磷酰氯。考察了缚酸剂的种类、用量、加入方式及三氯氧磷滴加温度等因素对产物收率和性状的影响。实验结果表明,在以二异丙基乙胺为缚酸剂,双酚与二异丙基乙胺的摩尔比为1∶2.65,先加入60%(w)的二异丙基乙胺,剩余二异丙基乙胺与三氯氧磷在20℃下同时滴加,25℃下反应1 h的条件下,2,2′-亚甲基双(4,6-二叔丁基)磷酰氯收率为90.2%,纯度可达99.2%(w)。以此原料制备的NA-11的HPLC纯度达99.8%以上,色度可达优级标准。2,2′-Methylene-bis（4,6-di-tert-butylphenyl）phosphorus oxychloride,an intermediate for the synthesis of sodium 2,2′-methylene-bis（4,6-di-tert-butylphenyl） phosphate（NA-11）,a polypropylene nucleating agent,was synthesized from 2,2′-methylene-bis（4,6-di-tert-butylphenyl）phenol and phosphoryl chloride with acetonitrile as solvent. The effects of types,dosage,adding mode of acid binding agents and the dropping temperature of phosphoryl chloride on the synthesis were investigated. The results indicated that under the condition of ethyldiisopropylamine as acid binding agent,n（bisphenol）∶n（ethyldiisopropylamine） is 1∶2.65, pre-adding 60%（w） ethyldiisopropylamine before dropping phosphoryl chloride（the rest of the acid binding agent and phosphoryl chloride were dropped simultaneously at 20 ℃）,and reaction time 1 h at 25 ℃,the yield of the intermediate was 90.2% with the p urity of 99.2%（w）. The purity of NA-11 prepared from the intermediate reached more than 99.8% and its chroma could reach the superior standard.

关 键 词：聚丙烯成核剂 缚酸剂 2 2′-亚甲基双(4 6-二叔丁基苯基)磷酰氯 二异丙基乙胺 三氯氧磷 2 2′-亚甲基双(4 6-二叔丁基苯基)磷酸钠 

分 类 号：TQ032.4[化学工程]