摘要
设计合成了4种负载型离子液体[Silica-Ps-Mor]HSO_4、[Silica-Ps-Mor]PTSA、[Silica-Ps-Mor]H_2PO_4和[Silica-Ps-Mor]BF_4,采用傅里叶变换红外光谱、扫描电镜、热重分析和N_2吸附-脱附等方法对样品进行表征,通过顺丁烯二酸酐和乙醇的酯化反应考察其催化性能。结果表明:当n(C_4H_2O_3)∶n(C_2H_6O)=1∶3.5,催化剂[Silica-Ps-Mor]HSO_4用量为顺丁烯二酸酐质量的5%,带水剂用量为酸酐质量的30%,反应温度为90℃,反应时间为4 h,酯收率可达94.5%。负载型离子液体作为催化剂,反应结束经抽滤便可回收再利用,催化剂循环使用8次,酯收率没有明显地降低。
Four kinds of silica-supported ionic liquid,containing [Silica-Ps-Mor]HSO4、[Silica-PsMor]PTSA、[Silica-Ps-Mor]H2PO4and [Silica-Ps-Mor]BF4 were successfully synthesized. The structures and properties were characterized by Fourier transform infrared spectrometer,scanning electron microscope thermogravimetric analysis and N2 adsorption-desorption technique. The esterification reaction of cis-butenedioic anhydride with ethanol was carried out to investigate the catalytic performance of the liquid ionic. The yield of diethyl maleate reached up to 94. 5% under the optimized conditions： n（ C4H2O3） ∶n（ C2H6O） = 1 ∶ 3. 5,dosage of [Silica-Ps-Mor]HSO4= 5% of cisbutenedioic anhydride,dosage of water carrying agent = 30% of cis-butenedioic anhydride,temperature90 ℃,and reaction time 4 h. The supported catalyst could be easily recovered from the reaction system. The diethyl maleate yield did not significantly lower when the catalyst was recycled for eight times.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2016年第6期648-653,共6页
Fine Chemicals
基金
国家自然科学基金(20576026
21106032)~~
