光稳定剂2，2′-硫代双(4-叔辛基苯酚)正丁胺镍的合成

Synthesis of Light Stabilizer 2,2′-Thiobis (4-t-octylphenolato)-n-butylamine Nickel

以对叔辛基苯酚、二氯化硫、正丁胺和乙酸镍为原料,经缩合、络合两步反应合成了2,2′-硫代双(4-叔辛基苯酚)正丁胺镍。考察了反应条件对产物收率的影响,得到了最佳反应条件。缩合反应中,采用正己烷作溶剂,对叔辛基苯酚与二氯化硫摩尔比2:1.1,反应温度10℃,二氯化硫滴加时间80 min,此条件下2,2′-硫代双对叔辛基苯酚的收率为85.5%。络合反应中,2,2′-硫代双对叔辛基苯酚、乙酸镍和正丁胺的摩尔比为1:1.25:3,此时2,2′-硫代双(4-叔辛基苯酚)正丁胺镍的收率为97.6%。两步反应总收率83.4%,中间体及产物结构经红外光谱和元素分析确证。

2,2＇-thiobis（4- t-octylphenolato）- n-butylamine nickel was prepared from p-t-octylphenol, sulfur dichlo- ride, n-butylamine and nickel acetate by means of condensation and complexation. Effects of the reaction conditions on the product yields were investigated and the optimal synthetic conditions were obtained. In condensation reaction, the optimal conditions were as follows： n-hexane as solvent, molar ratio of p-t-octylphenol to sulfur dichloride 2：1.1 ,temperature 10 ℃ ,dropping time of sulfur dichloride 80 min, and the yield of 2,2＇-thiobis-4-t-octylphenol was 85.5% .In complexation reaction, the optimal conditions were as follows： molar ratio of 2, 2＇-thiobis-4-t- octylphenol, nickel acetate and n-butylamine 1 ： 1.25 ： 3, and the yield of 2,2＇-thiobis （4- t-octylphenolato） - n- butylamine nickel was 97.6 %. Total yield of the products in the two steps was 83.4 %. The structures of the intermediate and object product were verified by IR spectrum and elementary analysis.