以DBU/甲醇为开关溶剂,大豆油代替藻类油脂,在无水条件下通过条件实验确定了开关溶剂提取油脂、开关溶剂循环利用两个实验的较好条件。提取大豆油:VDBU/V甲醇:1∶1;V开关溶剂:21 m L;V大豆油:7 m L;通CO_2t:35 min;T:室温;CO_2连续鼓泡...以DBU/甲醇为开关溶剂,大豆油代替藻类油脂,在无水条件下通过条件实验确定了开关溶剂提取油脂、开关溶剂循环利用两个实验的较好条件。提取大豆油:VDBU/V甲醇:1∶1;V开关溶剂:21 m L;V大豆油:7 m L;通CO_2t:35 min;T:室温;CO_2连续鼓泡;转速:540 r/min。大豆油的收率91.43%。开关溶剂循环:加热温度:130℃;冷凝回流1.5 h;N2连续鼓泡;转速:540 r/min。由L9(33)正交试验得出各因素对反应的影响强弱顺序为:V开关溶剂/V大豆油>通CO_2的温度>VDBU/V甲醇。开关溶剂循环次数可达到6次以上。展开更多
Switchable ionic compounds have wide applications in chemical processes.A switchable ionic compound based on 1,8-diazabicyclo-[5.4.0]-undec-7-ene(DBU),CH_3OH and CO_2 was synthesized and characterized.DBU/CH_3OH/CO_2 ...Switchable ionic compounds have wide applications in chemical processes.A switchable ionic compound based on 1,8-diazabicyclo-[5.4.0]-undec-7-ene(DBU),CH_3OH and CO_2 was synthesized and characterized.DBU/CH_3OH/CO_2 ionic compound was prepared in the presence of excess methanol,and then the excess methanol was removed by reduced pressure distillation in CO_2 atmosphere.The product yield(100%) reached the theoretical maximum for the first time.Its structure was identified by NMR,FT-IR,and XRD.The crystal product shows 8strong peaks in XRD at 2θ values of 16.0547°,16.4308°,16.7651°,18.8714°,19.2140°,21.9471°,22.0780°,and25.5661°.Its decomposition onset temperature(53 ℃) was affirmed by TGA,which is lower than its melting point.And its ionic switch point was measured by conductivity.展开更多
文摘以DBU/甲醇为开关溶剂,大豆油代替藻类油脂,在无水条件下通过条件实验确定了开关溶剂提取油脂、开关溶剂循环利用两个实验的较好条件。提取大豆油:VDBU/V甲醇:1∶1;V开关溶剂:21 m L;V大豆油:7 m L;通CO_2t:35 min;T:室温;CO_2连续鼓泡;转速:540 r/min。大豆油的收率91.43%。开关溶剂循环:加热温度:130℃;冷凝回流1.5 h;N2连续鼓泡;转速:540 r/min。由L9(33)正交试验得出各因素对反应的影响强弱顺序为:V开关溶剂/V大豆油>通CO_2的温度>VDBU/V甲醇。开关溶剂循环次数可达到6次以上。
基金Supported by the Doctoral Fund of Ministry of Education of China(20130181130006)the Key Program of National Natural Science Foundation of China(21336008)the National Natural Science Foundation of China(21476150)
文摘Switchable ionic compounds have wide applications in chemical processes.A switchable ionic compound based on 1,8-diazabicyclo-[5.4.0]-undec-7-ene(DBU),CH_3OH and CO_2 was synthesized and characterized.DBU/CH_3OH/CO_2 ionic compound was prepared in the presence of excess methanol,and then the excess methanol was removed by reduced pressure distillation in CO_2 atmosphere.The product yield(100%) reached the theoretical maximum for the first time.Its structure was identified by NMR,FT-IR,and XRD.The crystal product shows 8strong peaks in XRD at 2θ values of 16.0547°,16.4308°,16.7651°,18.8714°,19.2140°,21.9471°,22.0780°,and25.5661°.Its decomposition onset temperature(53 ℃) was affirmed by TGA,which is lower than its melting point.And its ionic switch point was measured by conductivity.
