脱氢枞酸蔗糖酯的无溶剂法合成

用精制的脱氢枞酸,在n(硫酸二甲酯)∶n(脱氢枞酸)=1∶1,碳酸钾为催化剂,反应时间为4 h,丙酮回流条件下,得到脱氢枞酸甲酯,产率为75%。脱氢枞酸甲酯与蔗糖在熔融下通过酯交换反应生成脱氢枞酸蔗糖酯,最佳条件为:n(脱氢枞酸甲酯)∶n(蔗糖)=1∶1.5,m(催化剂碳酸钾)∶m(反应物)=0.05∶1,m(乳化剂硬脂肪酸钠)∶m(反应物)=0.1∶1,温度140℃,压强0.5 kPa,反应时间5 h,产率可达32%,测定了其表面张力和乳化能力。临界胶束浓度(CMC)为:9.0×10-3mol/L;此时表面张力为18.42 mN/m。

Synthesis of Sucrose Dehydroabietate by Solvent-free Method

Methyl dehydroabietate was obtained from the purified dehydroabietic acid in 75% yield by reacting dehydroabietic acid and dimethyl sulfate in molar ratio 1∶1,using potassium carbonate as catalyst and acetone as solvent.Sucrose dehydroabietate was synthesized by transesterifion of methyl dehydroabietate and sucrose without solvent.The optimum reaction conditions were n(methyl dehydroabietate)∶n(sucrose)=1∶1.5,m(catalyst)∶m(reactants)=0.05∶1,m(emulsifier)∶m(reactants)=0.1∶1,temperature 140 ℃,pressure 0.5 kPa and reaction time 5 h.Yield of sucrose ester was 32%.The final product had good capability of foaming and emulsification,its CMC was 9.0×10~(-3) mol/L,and the surface tension at this point was 18.42 mN/m.