化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2014年
2期
561-569
,共9页
赵地顺%葛京京%翟建华%张娟%刘猛帅%李俊盼
趙地順%葛京京%翟建華%張娟%劉猛帥%李俊盼
조지순%갈경경%적건화%장연%류맹수%리준반
离子液体%Lewis酸%酯化%丁二酸二异丙酯%催化剂
離子液體%Lewis痠%酯化%丁二痠二異丙酯%催化劑
리자액체%Lewis산%지화%정이산이이병지%최화제
ionic liquid%Lewis acid%esterification%diisopropyl succinate%catalyst
采用两步法制备了9种不同的Lewis酸性离子液体,采用1H NMR、FT-IR对离子液体的结构进行了表征,并系统地考察了其对丁二酸和异丙醇酯化反应的催化性能。结果表明,离子液体随着卤化物用量增加表现出更强的酸性。其中[Bmim]Br-Fe2Cl6催化合成丁二酸二异丙酯效果良好,催化剂用量为丁二酸质量的10.0%,反应温度100℃,反应时间4 h,酸醇摩尔比为1:5,丁二酸二异丙酯收率为88.9%,酯化率达92.7%。离子液体重复使用6次后,产品收率下降1.7%。
採用兩步法製備瞭9種不同的Lewis痠性離子液體,採用1H NMR、FT-IR對離子液體的結構進行瞭錶徵,併繫統地攷察瞭其對丁二痠和異丙醇酯化反應的催化性能。結果錶明,離子液體隨著滷化物用量增加錶現齣更彊的痠性。其中[Bmim]Br-Fe2Cl6催化閤成丁二痠二異丙酯效果良好,催化劑用量為丁二痠質量的10.0%,反應溫度100℃,反應時間4 h,痠醇摩爾比為1:5,丁二痠二異丙酯收率為88.9%,酯化率達92.7%。離子液體重複使用6次後,產品收率下降1.7%。
채용량보법제비료9충불동적Lewis산성리자액체,채용1H NMR、FT-IR대리자액체적결구진행료표정,병계통지고찰료기대정이산화이병순지화반응적최화성능。결과표명,리자액체수착서화물용량증가표현출경강적산성。기중[Bmim]Br-Fe2Cl6최화합성정이산이이병지효과량호,최화제용량위정이산질량적10.0%,반응온도100℃,반응시간4 h,산순마이비위1:5,정이산이이병지수솔위88.9%,지화솔체92.7%。리자액체중복사용6차후,산품수솔하강1.7%。
Nine kinds of different Lewis acid ionic liquids were synthesized by two-step process and their structures were characterized with 1H NMR and FT-IR. Lewis acid ionic liquids prepared were used to catalyze the esterification reaction of succinic acid and isopropyl alcohol. With the increase of dosage of halide, the ionic liquids showed stronger acidity. [Bmim]Br-Fe2Cl6 had the best catalytic performance, and optimal conditions for the synthesis of succinic acid diisopropyl ester were obtained as follows, amount of catalyst 10.0%(g/g)of succinic acid, reaction temperature 100℃ and reaction time 4 h, succinic acid and isopropyl alcohol ratio 1:5. Under the optimal conditions, the yield of succinic acid diisopropyl ester was up to 88.9%, esterification rate was 92.7%.The catalyst was recycled 6 times, and the yield of succinic acid diisopropyl ester only decreased by 1.7%.