化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2014年
12期
3270-3275
,共6页
郭剑桥%虞宁%丁嘉%黄媛媛%汪青松%李工
郭劍橋%虞寧%丁嘉%黃媛媛%汪青鬆%李工
곽검교%우저%정가%황원원%왕청송%리공
合成%单核及双核离子液体%催化%化学反应%柠檬酸三丁酯
閤成%單覈及雙覈離子液體%催化%化學反應%檸檬痠三丁酯
합성%단핵급쌍핵리자액체%최화%화학반응%저몽산삼정지
synthesis%uni-nuclear and bi-nuclear ionic liquids%catalysis%chemical reaction%tributyl citrate
合成了具有 Bronsted 酸性的单核叔铵盐离子液体1-(丙酸基)高哌啶硫酸氢盐[HMILS]HSO4和双核叔铵盐离子液体双-(1-高哌啶)亚丁基双硫酸氢盐HMIBL[HSO4]2,用红外、核磁、元素分析及热分析等方法对合成的产物进行表征。把合成的单核及双核酸性离子液体作为催化剂用于催化柠檬酸和正丁醇的酯化反应,考察其催化活性。结果表明,离子液体的催化活性与其酸强度呈相关性,其中双核离子液体HMIBL[HSO4]2具有较强的酸性和较高的催化活性,当反应条件为n(正丁醇)∶n(柠檬酸)∶n(HMIBL[HSO4]2)=5∶1∶0.05、120℃、反应时间3h,柠檬酸的转化率和柠檬酸三丁酯的选择性分别为98.91%和99.53%,反应后的酸性离子液体可以回收,稳定性好,重复使用10次后仍有较高的催化活性。
閤成瞭具有 Bronsted 痠性的單覈叔銨鹽離子液體1-(丙痠基)高哌啶硫痠氫鹽[HMILS]HSO4和雙覈叔銨鹽離子液體雙-(1-高哌啶)亞丁基雙硫痠氫鹽HMIBL[HSO4]2,用紅外、覈磁、元素分析及熱分析等方法對閤成的產物進行錶徵。把閤成的單覈及雙覈痠性離子液體作為催化劑用于催化檸檬痠和正丁醇的酯化反應,攷察其催化活性。結果錶明,離子液體的催化活性與其痠彊度呈相關性,其中雙覈離子液體HMIBL[HSO4]2具有較彊的痠性和較高的催化活性,噹反應條件為n(正丁醇)∶n(檸檬痠)∶n(HMIBL[HSO4]2)=5∶1∶0.05、120℃、反應時間3h,檸檬痠的轉化率和檸檬痠三丁酯的選擇性分彆為98.91%和99.53%,反應後的痠性離子液體可以迴收,穩定性好,重複使用10次後仍有較高的催化活性。
합성료구유 Bronsted 산성적단핵숙안염리자액체1-(병산기)고고정류산경염[HMILS]HSO4화쌍핵숙안염리자액체쌍-(1-고고정)아정기쌍류산경염HMIBL[HSO4]2,용홍외、핵자、원소분석급열분석등방법대합성적산물진행표정。파합성적단핵급쌍핵산성리자액체작위최화제용우최화저몽산화정정순적지화반응,고찰기최화활성。결과표명,리자액체적최화활성여기산강도정상관성,기중쌍핵리자액체HMIBL[HSO4]2구유교강적산성화교고적최화활성,당반응조건위n(정정순)∶n(저몽산)∶n(HMIBL[HSO4]2)=5∶1∶0.05、120℃、반응시간3h,저몽산적전화솔화저몽산삼정지적선택성분별위98.91%화99.53%,반응후적산성리자액체가이회수,은정성호,중복사용10차후잉유교고적최화활성。
Bronsted acidic ionic liquid 1-(propionyloxy) high piperidine hydrogen sulfate ([HMILS] HSO4) and bis-(1-high piperidine) butylidene double hydrogen sulfate (HMIBL[HSO4]2) were synthesized and characterized by FT-IR,1H NMR,elemental analysis and thermal analysis. As uni-nuclear and bi-nuclear tertiary ammonium ionic liquids,they were used in the esterification reaction of citric acid with n-butyl alcohol for investigating their catalytic activity. The catalytic activity of ionic liquids was related to its acidity,and HMIBL[HSO4]2 had higher acidity and catalytic activity. Conversion of citric acid and selectivity to TBC were 98.91%and 99.53%respectively under the reaction conditions of n(alcohol)∶n(acid)∶n(IL)=5∶1∶0.05,temperature 120℃,reaction time 3h. Acidic ionic liquid could be recycled and exhibit high stability upon reusage. It still remained highly active even after being resued for ten times.