杂多酸催化合成氰乙酸乙酯的研究  

SYNTHESIS OF ETHYL CYANOACETATE CATALYZED BY HETEROPOLY ACID

作　　者：尚会建[1] 康丽娜[1] 赵叶[1] 高攀[1] 王丽梅[1] 王少杰[1] 郑学明[1] 

机构地区：[1]河北科技大学化工学院,河北石家庄050000

出　　处：《精细石油化工》2012年第3期48-51,共4页Speciality Petrochemicals

摘　　要：采用自制的磷钨酸(PW12)、硅钨酸(SiW12)、活性炭负载的磷钨酸(PW12/C)为催化剂,以甲苯为带水剂,催化氰乙酸与无水乙醇合成氰乙酸乙酯。确定了反应的最适条件:n(氰乙酸)∶n(无水乙醇)=1∶3.5,反应时间3h,带水剂用量为28%,PW12、SiW12催化剂用量为原料的0.6%时,酯化率分别为96.5%、95.4%。PW12/C催化剂用量为原料的5%,酯化率为94.3%。但两种纯杂多酸的使用寿命3次左右,而负载后的磷钨酸可重复使用7次,酯化率下降缓慢,表明PW12/C催化剂更有利于氰乙酸的酯化反应。Ethyl cyanoacetate was synthesized using cyanoacetic acid and absolute ethanol as reactants, three heteropolyacids as catalysts and methylbenzene as water entrainer. The optimum process condi- tions were obtained as follows： n（cyanoacetic acid） ： n（absolute ethyl alcohol）= 1 .＂ 3.5, reaction time 3 h, entrainer mass fraction 28% based on cyanoacetic acid, mass ratio of heteropolyacid PW12 and SiWl~ to cyanoacetic acid 0.6%, with the esterification yield reached 96.5% and 95.4~, respectively. The catalyst could be repeatedly used for three times. With PW12/C catalyst at 5% loadings based on cyanoacetic acid, the esterifieation yield reached 94.3% and the catalyst could be used for 7 times, showing that PW12/C catalyst is more suitable for the esterification reaction of cyanoacetic acid.

关 键 词：氰乙酸 杂多酸 氰乙酸乙酯 酯化 

分 类 号：TQ225.241[化学工程—有机化工]