抗氧剂168的改进合成  

Improved Synthesis of Antioxidant 168

作　　者：王伟杰[1] 阎圣刚[2] 陈宏博[1] 李刚月[2] 蒋山[2] 

机构地区：[1]大连理工大学化工学院,辽宁大连116024 [2]大连海事大学材料科学与工程系高分子材料研究所,辽宁大连116026

出　　处：《广东化工》2009年第3期23-25,共3页Guangdong Chemical Industry

摘　　要：研究了以2,4-二叔丁基苯酚、三氯化磷为原料通过酯化反应合成抗氧剂168的工艺,考察了催化剂种类、用量、反应温度、反应压力、原料配比对168收率的影响。研究表明,最佳工艺条件为n(2,4-二叔丁基苯酚)︰n(PCl3)=3.5︰1;反应温度第一阶段56℃反应2.5 h,第二阶段124℃反应2.5 h;催化剂用量为2,4-酚质量的0.5%,产品收率可达97%以上,纯度大于98%。通过核磁谱图对合成化合物的结构进行了表征。The synthesis of antioxidant 168 was studied by esterification of 2,4-ditertbutylphenol and phosphorus trichloridc. The effects of the variety and content of catalyst, reaction temperature, reaction pressure, the molar ratio of reagents on the reaction were studied, and the results showed the optimum conditions were determined as follows： the molar ratio of 2,4-ditertbutylphenol and phosphorus trichloride was 3.5 ： 1, the first stage reaction temperature was 56 ℃ and the reaction time was 2.5 h, the second stage reaction temperature was 124 ℃ and the reaction time was 2.5 h, and the catalyst quantity was 0.5 % of the 2,4-ditertbutylphenol mass. Under the optimum conditions, the yield of 168 was higher than 97 % and the purity exceeded 98 %. The structure of the product was defined by ^1H NMR.

关 键 词：2 4-二叔丁基苯酚 三氯化磷 抗氧剂168 4-二甲氨基吡啶 

分 类 号：TQ3[化学工程]