星型高效复合主抗氧剂的合成与抗氧化性能

 以β-(3,5-二叔丁基-4-羟基苯基)丙酰氯(简称3,5-丙酰氯， 3,5-Propionyl chloride)和星型聚合物1.0代聚酰胺-胺(1.0G PAMAM)为原料，通过酰胺化缩合反应合成了结构新颖的星型高效复合主抗氧剂，并通过优化实验确定了该抗氧剂的最佳合成条件。采用元素分析、FT-IR、¹H NMR 和¹³C NMR 对星型高效复合主抗氧剂进行表征，并考察了该抗氧剂在聚烯烃树脂中的抗氧化性能。结果表明，当n(3,5-Propionyl chloride)/n(1.0G PAMAM)=5、 三氯甲烷为溶剂、 反应时间12 h、 滴加1.0G PAMAM的温度为15℃、反应温度为45℃时，星型高效复合主抗氧剂收率在65%以上，熔程为204.5~206.5℃。星型高效复合主抗氧剂在聚烯烃树脂中具有很好的抗氧化作用，在聚丙烯树脂(PP)中的抗氧化性能与市售抗氧剂1010和3114相近，在聚乙烯树脂(LLDPE)中的抗氧化性能优于抗氧剂1010和3114。

Synthesis and Antioxidant Activity of a Star Highly Efficient Complex Primary Antioxidant

A star highly efficient complex primary antioxidant with novel structure was synthesized by condensation reaction with β-(3,5-diterbutyl-4-hydroxyphenyl) propionyl chloride and 1.0 generation poly(amidoamine) (1.0G PAMAM) as raw materials, and characterized by elemental analysis, FT-IR, ¹H NMR and ¹³C NMR. The antioxidant activity of the star highly efficient complex primary antioxidant in polyolefins was evaluated by oxidation induction time. The results showed that the optimum reaction conditions for this antioxidant synthesis were the molar ratio of β-(3,5-diterbutyl-4-hydroxyphenyl) propionyl chloride to 1.0G PAMAM of 5, chloroform as the solvent, the reaction time of 12 h, the adding temperature for 1.0G PAMAM of 15℃ and the reaction temperature of 45℃,under which the yield of the star highly efficient complex primary antioxidant was above 65% and the melting point was in the range of 204.5-206.5℃. The star highly efficient complex primary antioxidant had excellent oxidation resistance behavior in polyolefins, whose oxidation resistance was far superior to antioxidant 1010 and antioxidant 3114 in polyethylene and equal to the two antioxidants in polypropylene.