N,N-二甲基脱氢枞基氧化叔胺的制备及其性能

摘要

A new dehydroabietylamine derivative, i. e. , N, N-dimethyl dehydroabietylamine oxide, was synthesized from dehydroabietylamine (99 %) via alkylation and oxidation. Its structure was identified by FT-IR and 1H NMR spectra. The oxidation conditions were optimized by the L16 (45 ) orthogonal test. The results showed that suitable synthesis reaction conditions of the titled compound were as follows:N,N-dimethyl dehydroabietylamine oxide and H2 O2 molar ratio of 1. 5:1, reaction time of 12 h, EDTA of 1. 5 % and reaction temperature of 80 ℃. The GC content of the tertiary amine oxide were above 70 % in repetitive experiments. The surfactivity experiment showed that the critical micelle concentration ( CMC ) can be as low as 0. 2 g/L, and the surface tension is 22. 75 mN/m. And a new type of adsorbent prepared from amine oxide-modified zeolite has better adsorption effect on a certain concentration of humic acid and Congo red. When the initial concentration of 40 mg/L reached equilibrium, the removal rates were 51. 1% and 91. 0 %, respectively.%利用纯度99%的脱氢枞胺原料经烷基化和氧化两步反应合成了一种含松香基三元菲环结构的N,N-二甲基脱氢枞基氧化叔胺。采用红外光谱(FT-IR)、核磁(1H NMR)对其结构进行表征,并通过L16(45)正交试验,对双氧水氧化法合成氧化叔胺的工艺条件进行了优化研究,制备反应的最佳工艺条件：双氧水与叔胺的物质的量比为1.5：1,反应时间12 h,催化剂用量1.5%,反应温度80℃。在优化的工艺条件下重复试验,氧化叔胺的产率为80%,GC含量均大于70%。产物的临界胶束浓度( CMC)为0.2 g/L,表面张力为22.75 mN/m,并且经此氧化叔胺改性得到的新型沸石吸附剂对一定浓度的腐殖酸、刚果红等环境污染物具有较佳的吸附效果,当初始质量浓度达到40 mg/L左右时吸附基本达到平衡,去除率分别为51.1%和91.0%。