尿素-氯化胆碱低共熔溶剂催化聚酰胺酸亚胺化  

Imidization of polyamide acid catalyzed by urea-choline chloride deep-eutectic solvent

作　　者：冯树波[1] 杨帅 杨依依 孟祥浩 武金亮 张科 FENG Shubo;YANG Shuai;YANGYiyi;MENG Xianghao;WU Jinliang;ZHANG Ke(School of Chemical and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,Hebei,China;Shijiazhuang Hope Hi^h-Technology Co.Ltd.,Shijiazhua昭052160,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 [2]石家庄昊普科技有限公司,河北石家庄052160

出　　处：《精细化工》2022年第4期741-745,782,共6页Fine Chemicals

基　　金：中央引导地方科技发展资金项目(206Z1403G)。

摘　　要：该文报道了以均苯四甲酸二酐(PMDA)和4,4′-二氨基二苯醚(ODA)为单体制备聚酰亚胺(PI)的清洁过程。首先,在N,N-二甲基甲酰胺(DMF)中获得聚酰胺酸(PAA);然后,以尿素-氯化胆碱低共熔溶剂(DES)为催化剂,乙酸酐为脱水剂,协同实现PAA亚胺化。所得产物PI可通过简单过滤分离。用FTIR、TGA-DSC和元素分析对PAA和PI的结构进行了表征。考察了反应时间、反应温度、DES催化剂与脱水剂用量对PAA亚胺化反应的影响。得到亚胺化最佳反应条件为:温度80℃,DES与乙酸酐体积比1∶2、PAA与DES物质的量比1∶2。红外表征结果证实了亚胺键的生成。此外,DES和DMF可重复使用,反应过程绿色,不使用有毒有害的吡啶、咪唑和喹啉类催化剂。A green process of the synthesis of polyimide(PI)from phthalic anhydride(PMDA)and 4,4′-diaminodiphenyl ether(ODA)was reported.Firstly,polyamic acid(PAA)was formed in N,N-dimethylformamide(DMF).Then,imidization of PAA was realized using urea-choline chloride deep eutectic solvent(DES)as catalyst and acetic anhydride as dehydrator.The obtained PI could be isolated by a simple and direct filtration.PAA and PI were characterized by FTIR,TGA-DSC and element analysis.The effects of reaction temperature,reaction time,DES catalyst dosage and acetic anhydride dosage on imidization of PAA were investigated.The optimal conditions for the synthesis of PI were obtained as follows:temperature of 80℃,volume ratio of DES to acetic anhydride 1∶2,molar ratio of PAA to DES 1∶2.The result of FTIR confirmed the formation of imine bonds.In addition,DES and DMF could be reused.This process was green and did not use toxic and harmful pyridine imidazole and quinoline catalyst.

关 键 词：尿素-氯化胆碱低共熔溶剂 聚酰胺酸 化学亚胺化 催化脱水 聚酰亚胺 催化技术 

分 类 号：TQ426[化学工程] TQ323.7