全文下载: 202204002.pdf
文章编号: 1672-6987(2022)04-0014-06; DOI: 10.16351/j.1672-6987.2022.04.002
张坤, 纪聪聪, 王广浩, 于世涛, 刘仕伟*(青岛科技大学 化工学院,山东 青岛 266042)
摘要: 制备并表征了Brnsted-Lewis双酸型离子液体3-磺酸丙基三乙基铵氯锌酸盐[HO3S·(CH2)3NEt3]Cl-ZnCl2(x(ZnCl2)=060),并用于催化合成松香甘油酯。考察了原料配比、催化剂用量、反应时间和反应温度等条件对反应结果的影响。结果表明:所合成的离子液体具有可调变的Brnsted与Lewis酸性特征,且两酸性间兼有的协同催化效应显著提高了反应的催化性能;在n(松香)∶n(甘油)=1∶08、松香150 g和催化剂03 g、反应温度230 ℃、反应时间5 h、真空度40 kPa的较佳实验条件下,产物松香甘油酯的软化点为1045 ℃、酸值(KOH)为92 mg·g-1、色泽为10~11(Fe-Co)。且反应后分离所得催化剂重复使用6次后,其催化性能未见降低,具有较好的可重复使用性。
关键词: 松香; 松香甘油酯; 双酸型离子液体; 酯化反应; 催化
中图分类号: O 629.9文献标志码: A
引用格式: 张坤, 纪聪聪, 王广浩, 等. 双酸型离子液体[HO3S(CH2)3NEt3]Cl-ZnCl2 (x(ZnCl2)=060)催化合成松香甘油酯[J]. 青岛科技大学学报(自然科学版), 2022, 43(4): 14-19.
ZHANG Kun, JI Congcong, WANG Guanghao, et al. Synthesis of rosin glyceride catalyzed by double acidic ionic liquid [HO3S(CH2)3NEt3]Cl-ZnCl2(x(ZnCl2)=060)[J]. Journal of Qingdao University of Science and Technology(Natural Science Edition), 2022, 43(4): 14-19.
Synthesis of Rosin Glyceride Catalyzed by Double Acidic Ionic
Liquid [HO3S(CH2)3NEt3]Cl-ZnCl2 (x(ZnCl2)=060)
ZHANG Kun, JI Congcong, WANG Guanghao, YU Shitao, LIU Shiwei
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)
Abstract: Brnsted-Lewis double acidic ionic liquid [HO3S(CH2)3NEt3]Cl-ZnCl2 (x(ZnCl2)=060) was prepared, characterized, and used for catalytic synthesis of rosin glyceride. The influences of reaction conditions, such as kinds of catalysts, amounts of catalyst, reaction time and temperature were examined. The optimum reaction conditions for esterification were obtained as follows:n(rosin)∶n(glycerinum)=1∶08, rosin 150 g, catalyst 03 g, reaction temperature 230 ℃, reaction time 4 h, and vacuum degree 40 kPa. Under the above reaction conditions, the softening point of rosin glyceride was 1045 ℃, the acid value (KOH) was 92 mg·g-1, the color was 10—11 (Fe-Co). The recyclability of the catalyst was also investigated. When the catalyst [HO3S(CH2)3NEt3]Cl-ZnCl2 (x=060) was repeatedly used for six times, it′s catalytic performance had not been reduced, so it had good reusability.
Key words: rosin; rosin glyceride; diacid type ionic liquid; esterification reaction; catalysis
收稿日期: 2021-06-10
基金项目: “十三五”国家重点研发计划项目(2016YFD0600804);山东省泰山学者工程项目(ts201511033);全国大学生创新创业训练计划项目(S202010426038).
作者简介: 张坤(1994—),女,硕士研究生.*通信联系人.