3-松香胺基-2-羟丙基三甲基氯化铵的合成研究

Study on the Synthesis of 3-Rosinamino-2-hydroxypropyl Trimethylammonium Chloride

以松香胺(RA)和3-氯-2-羟丙基三甲基氯化铵(CTA)为原料,在碱性助剂作为催化剂和缚酸剂的条件下合成了3-松香胺基-2-羟丙基三甲基氯化铵(RAHPTMA);探讨了反应介质类型、催化剂类型、反应时间、nCTA/nRA值和催化剂用量对产物收率的影响,用电导滴定法分析了产品含量,元素分析、熔点测定、FTIR及1H NMR方法对产物进行了表征。结果表明甲醇、乙醇等低碳醇是较好的反应介质,经重结晶处理后的产品中RAHPTMA的含量在97%以上,固载催化剂的使用能明显改善产品的收率。RAHPTMA适宜的合成条件为:乙醇为反应介质,固载碳酸钾(碳酸钾含量为20%)作为催化剂和缚酸剂且nK2CO3/nRA=1.5,nCTA/nRA=1.4,反应时间为12 h;在此条件下RAHPTMA的收率可达87.4%。

In the presence of a basic promoter, 3-rosinamino-2-hydroxypropyl trimethyl ammonium chloride （RAHPTMA） was synthesized with rosin amine （RA） and 3-chloro-2-hydroxypropyl trimethylammonium chloride （CTA） as starting material. The effect of solvent,catalyst, reaction time and nCTA/nRA value on the yield of RAHPTMA was investigated. The content of RAHPTMA in product was determined by conductometric titration. The product was characterized by elemental analysis, melting point determination, FT IR and ^1H NMR. The results indicated that alcohols with low carbon number such as methanol and ethanol, are good reaction solvent. The content of RAHPTMA in product was more than 97% after recrystallization, and the utilization of solid-loading catalyst could improve the yield of RAHPTMA. The suitable conditions for the synthesis of RAHPTMA were as follows, ethanol as reactive medium, potassium carbonate loading on solid carrier （content of potassium carbonate was 20%） as catalyst and acid-binding agent, nK2CO3/nRA= 1. 5, nCTA/nRA = 1. 4, reaction time of 12 h. The yields of RAHPTMA could reach 87.4% under these conditions.