摘要
以正十八胺为核的1.0代超支化大分子和β-(3,5-二叔丁基-4-羟基苯基)丙酰氯为原料,通过酰胺化缩合反应,合成了一种具有长链烷基和2个受阻酚基团的新型超支化分子桥联受阻酚类抗氧化剂.通过正交实验确定了超支化分子桥联受阻酚类抗氧化剂的最佳合成体系为:3,5-丙酰氯为酰化剂、K_2CO_3为缚酸剂、苯和水为反应溶剂.通过条件优化实验确定了超支化分子桥联受阻酚类抗氧化剂的最佳合成条件为:3,5-丙酰氯与1.0代超支化大分子的物质的量比为6∶1、反应温度为25 ℃、反应时间为12 h、体系苯与水体积比为6∶1、3,5-丙酰氯与缚酸剂K_2CO_3的物质的量比为1∶1,在此条件下,超支化分子桥联受阻酚类抗氧化剂的收率高达75.5%.FT-IR和1H NMR证实了合成抗氧化剂的化学结构与其理论结构相符.超支化分子桥联受阻酚类抗氧化剂在聚乙烯树脂中的抗氧化性能优于抗氧化剂1076,且随着烷基链长度的增加,抗氧化性能增强.
Hyperbranched hindered phenol antioxidant with long-chain alkyl structure and two hindered phenols groups was synthesized by amidation condensation reaction using 3-（3,5-diterbutyl-4-hydroxyphenyl） propionyl chloride and 1.0 generation hyperbranched polymer as raw materials. The synthetic systems and synthetic conditions of hyperbranched hindered phenol antioxidant were studied by orthogonal design and conditional experiment. The optimal synthetic systems were confirmed that 3,5-propionyl chloride, K_2CO_3, toluene and water acts as acylating agent, acid-binding agent, and solvents, respectivety. The optimal synthetic conditions is： the mole ratio of 3,5-propionyl chloride and 1.0 generation hyperbranched polymer was 6∶1, the reaction temperature was 25 ℃, the reaction time was 12 h, the volume ratio of toluene and water was 3∶1 and the mole ratio of 3,5-propionyl chloride and K_2CO_3 was 1∶1. Under these conditions, the yield of the product was up to 75.5%. IR and 1H NMR results further confirmed that the product was the desired one. Antioxidant activities of hyperbranched molecule bridged hindered phenol antioxidants in polyethylene were superior than that of antioxidant 1076, and were strengthened with increasing of the length of alkyl chain.
出处
《分子科学学报》
CAS
CSCD
北大核心
2017年第1期30-36,共7页
Journal of Molecular Science
基金
国家自然科学基金资助项目(51303020)
