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微波辐射纳米氧化钐催化合成草酸二丁酯
引用本文:邓斌,章爱华,徐安武.微波辐射纳米氧化钐催化合成草酸二丁酯[J].精细化工中间体,2008,38(3).
作者姓名:邓斌  章爱华  徐安武
作者单位:1. 湘南学院,化学与生命科学系,湖南,郴州,423000;中国科技大学,合肥微尺度物质科学国家实验室,安徽,合肥,230026
2. 吉首大学,化学化工学院,湖南,吉首,416000
3. 中国科技大学,合肥微尺度物质科学国家实验室,安徽,合肥,230026
摘    要:采用微波辐射技术,以纳米氧化钐为酯化反应催化剂合成草酸二丁酯。利用正交实验设计和单因素实验考察了微波辐射功率、微波辐射时间、催化剂用量、醇酸摩尔比等因素对酯化反应的影响。结果表明,纳米氧化钐催化剂在草酸二丁酯的合成中显示出良好的催化性能,而且该方法具有操作简便、反应速率快、节约能源等优点。在草酸用量为0.2mol、微波输出功率350W、辐射时间12min、催化剂用量为反应物总质量的1.0%、醇酸摩尔为4.0∶1的优化条件下,酯化率可达98.3%。

关 键 词:微波辐射  纳米氧化钐  草酸二丁酯  正交实验设计

Catalytic Synthesis of Dibutyl Oxalate by Nanometer Sm2O3 under Catalyst by Microwave Radiation
DENG Bin,ZHANG Ai-hua,XU An-wu.Catalytic Synthesis of Dibutyl Oxalate by Nanometer Sm2O3 under Catalyst by Microwave Radiation[J].Fine Chemical Intermediates,2008,38(3).
Authors:DENG Bin  ZHANG Ai-hua  XU An-wu
Abstract:Dibutyl oxalate was synthesized on nanometer Sm2O3 catalyst accelerated by microwave irradiation. Effects of microwave power,microwave irradiation time,mass fraction of catalyst and n(n-butanol) ∶ n(oxalic acid) on esterification reaction were investigated using orthogonal experimental design and single factor experiment. The experiment results showed that nanometer Sm2O3 had good catalytic activity for preparation of dibutyl oxalate. Esterification on the catalyst also took advantages of easy operation,rapid reaction rate and saving energy. Under optimum conditions of microwave power 350 W,microwave irradiation time,12 min;catalyst mass fraction 1.0%;and mole ratio of n(n-butanol) ∶ n(oxalic acid)=4.0 ∶ 1(for 0.2 mol of oxalic acid),esterifications rate could reach 98.3%.
Keywords:microwave irradiation  nanometer Sm_2O_3  dibutyl oxalate  orthogonal experimental design
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