固相反应合成4,4′-硫代双(5-甲基-2-叔丁基苯酚)低聚物抗氧剂  

Synthesis of the Polymers of 4,4′-Thiobis(5-Methyl-2-Tert-Butyl Phenol) Used as Antioxidant by Solid Reaction

作　　者：刘文涛[1] 袁光[1] 胡应喜[1] 吕九琢[1] 

机构地区：[1]北京石油化工学院化工系

出　　处：《抚顺石油学院学报》1998年第3期24-27,35,共5页Journal of Fushun Petroleum Institute

摘　　要：以４，４′－硫代双（５－甲基－２－叔丁基苯酚）为原料，氯化铁作氧化偶联剂，在碳酸钠的存在下应用超声波辐射进行固相反应合成了４，４′－硫代双（５－甲基－２－叔丁基苯酚）低聚物抗氧剂（ＰＴＢＰ），收率为９８．５％。ＰＴＢＰ合成条件为：４，４′－硫代双（５－甲基－２－叔丁基苯酚）：三氯化铁：碳酸钠（摩尔比）＝１：２：１，超声波频率３３ｋＨｚ，功率１５０Ｗ，反应时间３ｈ，反应温度２５～５０℃。以核磁共振谱（１３Ｃ－ＮＭＲ）、场解吸质谱（ＦＤ／ＭＳ）和元素分析对低聚物结构进行了表征。该方法无反应溶剂，设备空间利用率高，副产物少。In the presence of ultrasonic wave radiation, the low molecular weight polymer of 4,4′-thiobis(5-methyl-2-tert-butyl phenol), that is PTBP, is synthesized to yield 98.5 % by mixing of the powders of ferric chloride crystal, 4,4′-thiobis(5-methyl-2-tert-butyl phenol) and sodium carbonate. In this reaction, the molar ratio of 4,4′-thiobis (5-methyl-2-tert-butyl phenol), ferric chloride crystal and sodium carbonate is 1:2:1. The ultrasonic wave radiation frequency is equal to 33 kHz, and the ultrasonic wave radiation power is 150 W. The reaction time is 3 h, and temperature is 25～50℃. The polymer is characterized by 13 C-NMR, FD/MS and element analysis. Compared with the preceding methods, this method has the virtue of no solvent, higher space efficiency and less by-products.

关 键 词：固相反应 聚合 抗氧剂 

分 类 号：TQ314.249[化学工程—高聚物工业]