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文章编号： 1672-6987（2021）02-0037-05； DOI： 10.16351/j.1672-6987.2021.02.005
刘俊宏1， 赵震2， 杨喜生2， 徐基海1， 吴鸿志1， 唐林生1*（1.青岛科技大学 化工学院，山东 青岛 266042；2.山东兄弟科技股份有限公司，山东 寿光 262700）
摘要： 以1-烷氧基-2,2,6,6-四甲基哌啶-4-醇、癸二酸二甲酯为原料，LiOH和四丁基溴化铵（TBAB）为催化剂，正庚烷为溶剂，在反应过程中采用分水器不断地分出甲醇的酯交换方法，制备了系列双（1-烷氧基-2,2,6,6-四甲基哌啶-4-基）癸二酸酯，并通过红外光谱、核磁共振氢谱、核磁共振碳谱和质谱表征了其结构。结果表明:其较佳合成条件为n(癸二酸二甲酯)∶n(1-烷氧基-2,2,6,6-四甲基哌啶-4-醇)∶n（LiOH）∶n(TBAB)=1∶22∶16∶0024,在回流状态下反应6~8 h，粗产品通过m(甲醇)∶m(水)=1∶1的混合溶剂洗涤提纯。在以上条件下，产品的产率大于80%，质量分数大于95%。热重分析表明，以上合成的目标产物热稳定性良好。该方法具有反应条件温和，催化剂便宜，反应设备简单，产品产率及纯度高等优点。
关键词： 1-烷氧基-2,2,6,6-四甲基哌啶-4-醇; 癸二酸二甲酯; 双（1-烷氧基-2,2,6,6-四甲基哌啶-4-基）癸二酸酯; 热稳定性
中图分类号： TQ 225.14文献标志码： A
引用格式： 刘俊宏， 赵震， 杨喜生， 等. 双（1-烷氧基-2,2,6,6-四甲基哌啶-4-基）癸二酸酯的合成及其热稳定性［J］. 青岛科技大学学报(自然科学版), 2021, 42(2): 37-41.
LIU Junhong, ZHAO Zhen, YANG Xisheng, et al. Synthesis and thermal stability of bis(1-alkoxy-2,2,6,6-tetramethylpiperidin-4-yl) sebacate［J］. Journal of Qingdao University of Science and Technology（Natural Science Edition), 2021， 42(2)： 37-41.
Synthesis and Thermal Stability of
Bis(1-alkoxy-2,2,6,6-tetramethylpiperidin-4-yl) Sebacate
LIU Junhong1, ZHAO Zhen2, YANG Xisheng2, XU Jihai1, WU Hongzhi1, TANG Linsheng1
(1.College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;
2.Shandong Brothers Technology Co., Ltd., Shouguang 262700, China)
Abstract: Bis(1-alkoxy-2,2,6,6-tetramethylpiperidin-4-yl)sebacates(NORSs) were synthesized through transesterification by using dimethyl sebacate and 1-alkoxy-2,2,6,6-tetramethylpiperidin-4-ol as raw materials, LiOH and tetrabutyl ammonium bromide as catalysts, n-heptane as a solvent, and constantly separating methanol from the reaction system with a water konckout vessel, and their structures were characterized by IR, 1H NMR,13C NMR and MS. The results revealed that their optimal conditions were as follows: n (dimethyl sebacate)∶n(1-alkoxy-2,2,6,6-tetramethylpiperidine-4-ol)∶n(LiOH)∶n(TBAB)=1∶22∶1.6∶0024, the transesterification time being 6—8 h at the reflux temperature, and the crude products were purified by washing using the mixture of water and methanol with weight ratio of 1∶1. Under the above conditions, the mass fraction of the target products was more than 95%，the yield was more than 80%. The thermogravimetric analysis showed that the above NORSs had good thermal stability. The method has some advantages such as mild reaction conditions, cheap catalyst, simple apparatus and the high yield and purity.
Key words: bis(1-alkoxy-2,2,6,6-tetramethylpiperidine-4-yl)sebacates; dimethyl sebacate; 1-alkoxy-2,2,6,6-tetramethylpiperidin-4-ol; thermal stability
收稿日期： 2020-05-30
基金项目： 山东省教育厅科技计划项目（J16LC21）；山东省自然科学基金项目（ZR2015BL025）.
作者简介： 刘俊宏(1996—)，女，硕士研究生.*通信联系人.
