N-(3-十八烷氧基-2-羟基丙基)-N,N-二羟乙基氧化胺制备

Synthesis of N-(3-Octadecanoxy-2-Hydroxy-Propyl)-N,N-Dihydroxyethyl Amine Oxide

本文以十八醇、环氧氯丙烷、二乙醇胺和双氧水等为原料,通过三步反应合成N-(3-十八烷氧基-2-羟基丙基)-N,N-二羟乙基氧化胺,探索反应温度、投料比、反应时间、催化剂等因素对产物收率的影响,确定最佳反应条件。3-十八烷氧基-2-羟基-1-氯丙烷生成的最佳工艺条件:催化剂选用氢氧化钠,反应物摩尔比1:1.1,滴加环氧氯丙烷的温度是65℃,滴加时间1.5 h,反应温度95℃,反应时间5 h;N-(3-十八烷氧基-2-羟基丙基)-N,N-二羟乙基叔胺生成的最佳工艺条件:反应温度85℃,反应物摩尔比为1:1.2,反应时间4 h;N-(3-十八烷氧基-2-羟基丙基)-N,N-二羟乙基叔胺与双氧水反应的最佳工艺条件:60℃滴加双氧水1.5 h,80℃反应2 h,反应物摩尔比为1:1.1。在最佳工艺条件下终产物收率达到93.4%;对产物进行红外光谱表征,测定其临界胶束浓度为7.9 mmol/L时,水溶液的表面张力为23.2 mN/m,产物具有较好的表面活性。

In this paper,using octadecanol,epichlorohydrin,diethanolamine and hydrogen peroxide as raw materials,N-(3-octadecyloxy-2-hydroxypropyl)-N-N-dihydroxyethyl amine was synthesized by three-step reaction.The effects of reaction time,catalyst and other factors on the yield of the product were determined,and the optimum reaction conditions were determined.The optimum conditions for the formation of 3-octadecyloxy-2-hydroxy-1-chloropropane were as follows:sodium hydroxide was used as catalyst;the molar ratio of reactants is 1:1.1;the temperature of dropping epichlorohydrin is 65?C;the time of dropping is 1.5 h;the reaction temperature is 95?C and the reaction time is 5 h.The optimum conditions for the formation of N-(3-octadecyloxy-2-hydroxypropyl)-N-N-dihydroxyethyl tertiary amine were as follows:reaction temperature 85?C;molar ratio of reactants 1:1.2;reaction time 4 h.The optimum reaction condi-tions of N-(3-octadecyloxy-2-hydroxypropyl)-N-(N-dihydroxyethyl)amine and hydrogen peroxide were as follows:1:1.1 mol ratio of reactants was 1:1.1 when hydrogen peroxide was dripped at 60?C for 1.5 h or 80?C for 2 h.The yield of the final product reached 93.4 under the optimum conditions.When the critical micelle concentration of the product was 7.9 mmol/L,the surface tension of the aqueous solution was 23.2 mN/m,with good surface activity.