Bronsted-Lewis双酸性离子液体催化合成乙酸正丁酯  

Synthesis of n-butyl acetate catalyzed by Bronsted-Lewis diacidic ionic liquids

作　　者：高鹏翔 王亚婷 赵地顺[1] 翟建华[1] GAO Pengxiang;WANG Yating;ZHAO Dishun;ZHAI Jianhua(College of Chemical and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,Hebei,China)

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018

出　　处：《精细化工》2020年第10期2053-2059,共7页Fine Chemicals

摘　　要：以3-氨基-1-丙磺酸、氯化锌、盐酸为原料制备了一系列Bronsted-Lewis双酸性离子液体。离子液体中磺酸基提供Bronsted酸性,阴离子提供Lewis酸性。采用FTIR、1HNMR、13CNMR、元素分析对合成的离子液体进行了结构表征;对离子液体的Bronsted酸性、Lewis酸性、腐蚀性进行了测定。使用该离子液体催化合成了乙酸正丁酯并利用响应曲面法考察了最佳反应条件。结果表明,在反应温度103℃,催化剂[NH3C3H6SO3H]Cl/0.75ZnCl2(0.75代表3-氨基-1-丙磺酸盐酸盐与氯化锌物质的量比为1.00∶0.75)用量为正丁醇质量的10.03%,n(乙酸)∶n(正丁醇)=1.00∶1.22,反应时间4.92 h,带水剂环己烷用量为正丁醇质量的20%条件下,乙酸正丁酯收率可达97.28%。[NH3C3H6SO3H]Cl/0.75Zn Cl2重复使用5次后,催化剂活性没有明显降低。A series of Bronsted-Lewis diacidic ionic liquids were synthesized from 3-amino-1-propanesulfonic acid,zinc chloride and hydrochloric acid,wherein the sulfonic acid groups in cations in ionic liquids provide Bronsted acidity,while the anions provide Lewis acidity.The ionic liquids were characterized by FTIR,1 HNMR,13 CNMR and EA.The Bronsted acidity,Lewis acidity and corrosiveness of ionic liquids were tested.These ionic liquids were used as catalysts to synthesize n-butyl acetate and the optimal conditions were explored by response surface method.The results showed that under the conditions of reaction temperature 103℃,[NH3C3H6SO3H]Cl/0.75 ZnCl2[0.75 means that n(3-amino-1-propanesulfonic acid hydrochloride)∶n(zinc chloride)=1.00∶0.75]dosage being 10.03%of the mass of n-butanol,n(acetic acid)∶n(n-butanol)=1.00∶1.22,reaction time 4.92 h,cyclohexane dosage being 20%of the mass of n-butanol,the yield of n-butyl acetate could reach 97.28%.Furthermore,even if[NH3C3H6SO3H]Cl/0.75 ZnCl2 was reused for 5 times,it still kept high catalytic activity.

关 键 词：Bronsted-Lewis双酸性离子液体 3-氨基-1-丙磺酸 酯化反应 乙酸正丁酯 响应曲面法 催化技术 

分 类 号：O643.32[理学—物理化学]