CAJ | 학술논문

以H-732阳离子交换树脂为催化剂进行了酯化反应研究,合成了丁二酸单乙酯和乙酰水杨酸,通过单因素实验和正交实验优化了反应工艺。单因素实验结果表明：催化剂用量为丁二酸酐质量的20%、乙醇与丁二酸酐的摩尔比1.8∶1、反应时间2 h、反应温度90℃时,丁二酸单乙酯产率最高为68.76%;在丁二酸单乙酯的合成体系中加入分离出的副产物丁二酸二乙酯可以抑制副反应的发生,大大提高单酯的产率（90.79%）。正交实验结果表明：乙酸酐与水杨酸的摩尔比为3∶1,催化剂用量为水杨酸质量的14.50%,反应时间2 h、反应温度60℃时,乙酰水杨酸产率最高为77.57%;催化剂连续使用5次时,催化能力才有明显下降,对连续使用过5次的催化剂重新活化后催化能力无明显降低。
이H-732양리자교환수지위최화제진행료지화반응연구,합성료정이산단을지화을선수양산,통과단인소실험화정교실험우화료반응공예。단인소실험결과표명：최화제용량위정이산항질량적20%、을순여정이산항적마이비1.8∶1、반응시간2 h、반응온도90℃시,정이산단을지산솔최고위68.76%;재정이산단을지적합성체계중가입분리출적부산물정이산이을지가이억제부반응적발생,대대제고단지적산솔（90.79%）。정교실험결과표명：을산항여수양산적마이비위3∶1,최화제용량위수양산질량적14.50%,반응시간2 h、반응온도60℃시,을선수양산산솔최고위77.57%;최화제련속사용5차시,최화능력재유명현하강,대련속사용과5차적최화제중신활화후최화능력무명현강저。
Catalytic ability of cation exchange resin H-732 for esterification reaction was investigated,and monoethyl ester of succinic acid and acetylsalicylic acid were synthesized by esterification reaction,and the optimum experimental conditions were optimized by single factor experiment and orthogonal experiment.The results of single factor experiment showed that under the following condition：the quantity of the resin ：20% of succinic anhydride,n（ethanol）∶n（succinic anhydride）= 1.8∶1,reaction time 2 h,reaction temperature 90 ℃,the yield was 68.67%;.The yield of monoethyl ester of succinic acid was greatly improved by adding diethyl ester of succinate acid（side product）,and the yield was 90.79%.The results of orthogonal experiment show that under the following condition：n（acetic anhydride）∶n（salicylic acid）= 3∶1,the quantity of the resin is 14.50% of salicylic acid,reaction time 2 h,reaction temperature 60℃,the yield was 77.57%.The catalyst lost its activity after reuse 5 times and its activity could be restored by re-activation.