3-氯-2-羟丙基二甲基脱氢枞基氯化铵的合成研究.doc

3-氯-2-羟丙基二甲基脱氢枞基氯化铵合成研究 摘 要：由脱氢枞胺（DHA）和环氧氯丙烷合成3-氯-2-羟丙基二甲基脱氢枞基氯化铵（CHPDMDHA）。制备过程分三步进行：首先，以脱氢枞胺为主要原料通过Eschweiler-Clarke反应制得N,N-二甲基脱氢枞胺（DMDHA）；第二步是DMDHA与盐酸反应生成N,N-二甲基脱氢枞胺盐酸盐；最后盐酸盐与环氧氯丙烷反应，并用乙酸乙酯与乙醇的复合溶剂重结晶，得到产物CHPDMDHA。用FT-IR和核磁共振表征了原料、中间体及产物的结构；离子色谱法（IC）测定了产物的含量。 结果表明，用以上方法合成CHPDMDHA时，操作简单，得到的CHPDMDHA产品与脱氢枞胺及N,N-二甲基脱氢枞胺相比具有较好的水溶性 关键字：脱氢枞胺； 环氧氯丙烷；临界胶束浓度Study on the synthesis of 3-chloro-2-hydroxypropyl dimethyl dehydroabietyl ammonium chloride Abstract： 3-hloro-2-hydroxypropyl dimethyl dehydroabietyl ammonium chloride (CHPDMDHA) was synthesized from dehydroabietylamine (DHA) and epichlorodrin. The synthesis was done in three steps. First, DHA was transformed into N,N-dimethyl dehydroabietyl amine (DMDHA) through Eschweiler-Clarke Reaction. Second, the DMDHA was reacted with hydrochloric acid and translated into DMDHA hydrochloride. Third, the CHPDMDHA was obtained after the DMDHA hydrochloride had reacted with epichlorodrin and recrystallized using a solvent composed of ethyl acetate and ethanol. The structures of raw materials、intermediates and final products were all characterized by FT-IR and NMR. The content of intermediates and final products was analyzed by IC. The experimental results showed that CHPDMDHA obtained by DMDHA and epichlorodrin had a good quality. The result of FT-IR and IC test showed the content of CHPDMDHA in the product was more than 85% Keywords ： Eschweiler-Clarke reaction； 3-Chloro-2-hydroxypropyl dimethyl dehydroabietyl ammonium chloride (CHPDMDHA)；hydrochloric acid 第一章 绪论 1 1.1课题概述 1 1.1.1松香型表面活性剂的简介 1 1.1.2国内外对松香系列表面活性剂的研究现状、研究进展 1 1.2．CHPDMDHA的制备方法 3 1.2.1 N,N-二甲基脱氢枞胺的制备及其进展 3 1.2.2由中间产物制备CHPDMDHA及其进展 3 1.3 课题的研究目的和研究内容 5 1.3.1 课题的研究目的和意义 5 1.3.2.课题的研究内容 5 1.4课题的研究路线和方案 6 1.4.1课题的研究路线 6 1.4.2 课题的研究方案 6 1.4.2.1合成原理 7 1.4.2.2 研究路线 7 第二章3-氯-2-羟丙基二甲基脱氢枞基氯化铵的制备和结构表征 9 2.1 概述 9 2.2 实验部分 9 2.2.1 主要药品和仪器 9 2.2.2 N,N-二甲基脱氢枞胺的制备 9 2.2.3 N,N-二甲基脱氢枞胺盐酸盐的制备 10 2.2.4 CHPDMDHA的制备 10 2.2.5 原料、中间体及产物结构表征 10 2.2.6 CHPDMDHA的含量分析 11