1-(3-磺酸基)丙基-3-甲基咪唑磷钨酸盐的制备及其催化性能  

Preparation and Catalytic Properties of 1-(3-Sulfonic Group) Propyl-3-Methyl Imidazolium Phosphotungstate

作　　者：许妍[1] 万辉[1] 管国锋[1] 

机构地区：[1]南京工业大学化学化工学院,南京江苏210009

出　　处：《石油化工》2009年第12期1270-1275,共6页Petrochemical Technology

基　　金：江苏省自然科学基金项目(BK2005121)

摘　　要：以N-甲基咪唑、1,3-丙烷磺内酯、磷钨酸为原料,采用两步法合成了1-(3-磺酸基)丙基-3-甲基咪唑磷钨酸盐([MIMPS]_3PW_(12)O_(40))催化剂。利用X射线衍射、傅里叶变换红外光谱(FTIR)、热重-示差扫描量热分析对催化剂进行了表征,表征结果显示,[MIMPS]_3PW_(12)O_(40)催化剂中有8个结晶水,具有磷钨酸的Keggin结构和良好的热稳定性。将该催化剂用于合成乙二醇丁醚醋酸酯(BAC),在最佳工艺条件(反应时间2.0 h,乙二醇丁醚与醋酸的摩尔比1.2:1,反应温度120℃,催化剂与反应物的质量比0.04,带水剂环己烷与反应物的质量比0.3)下,BAC收率可达99.3%。反应后催化剂易分离,重复使用9次后BAC收率为86.8%。FTIR表征结果显示,产物为BAC,没有副产物生成。A novel environmental friendly catalyst, 1-（ 3-sulfonic group ） propyl-3-methyl imidazolium phosphotungstate （ [ MIMPS ] 3PW12O40 ） for synthesis of 2-butoxyethyl acetate （BAC） from 2-butoxyethanol and acetic acid was prepared from N-methylimidazolium, 1,3-propanesultone and phosphotungstic acid by a two-step method and was characterized by XRD, FTIR and TG-DSC. The [ MIMPS ] 3 PW12O40 catalyst existed in Keggin structure, possessed eight molecules of crystalline-water and was thermally stable. Under the optimum reaction conditions for synthesis of BAC： reaction temperature 120℃, reaction time 2.0 h, mole ratio of 2-butoxyethanol to acetic acid 1.2 ： 1, mass ratio of catalyst to reactants 0.04 and mass ratio of cyclohexane as water entrainer to reactants 0.3, the yield of BAC was 99.3%. The catalyst could be separated easily. After the catalyst was reused 9 times, yield of BAC remained at 86.8%. The product was identified by FTIR and no any by-product was observed.

关 键 词：磷钨酸 1-(3-磺酸基)丙基-3-甲基咪唑磷钨酸盐 离子液体催化剂 酯化反应 

分 类 号：TQ426.91[化学工程]