摘要
在微型反应器(40℃)中,将漆酶加入醋酸缓冲溶液(pH=5.0)中催化4-氨基苯酚聚合,持续反应10 h后得到黑色粉末状聚合物。通过UV-Vis观察了4-氨基苯酚及其聚合物吸收光谱的变化,采用FTIR、1HNMR、MALDI-TOF MS、TGA和DSC对产物的结构和性能进行了表征。结果表明:所得聚合物在氯仿中不溶,在丙酮、四氢呋喃、N,N-二甲基甲酰胺和二甲基亚砜中均有良好的溶解性。UV-Vis、FTIR和1HNMR结果显示:聚合物中酚羟基保留,氨基参与反应,苯环上的氢原子部分参与反应,并且推测了聚合物的结构。MALDI-TOF MS、TGA和DSC结果显示:聚合物为低聚物,相对分子质量分布在300-1 300 Da,聚合度为3-12。聚4-氨基苯酚的分解温度为223℃,具有良好的耐热性能。
Laccase-catalyzed polymerization of 4-aminophenol was conducted in acetate buffer solution(pH = 5. 0) at 40 ℃. After continuous reaction for 10 h,black solid powers were obtained. UV-Vis spectra were used to observe the absorption spectra changes of 4-aminophenol and its polymer. The structure and properties of product were characterized by means of FTIR,1 HNMR,MALDI-TOF MS,TGA and DSC. The results showed that the as-prepared polymer was insoluble in chloroform,and soluble in acetone,tetrahydrofuran,N,N-dimethylformamide and dimethyl sulfoxide. UV-Vis,FTIR and1 HNMR spectra of product revealed that the synthetic polymer contained phenolic hydroxyl groups,the amine group of 4-aminophenol participated in the polymerization reaction,and partial hydrogen atoms on the benzene ring involved in the reaction. The possible structures of polymer were speculated. In addition,the obtained poly(4-aminophenol) was an oligomer with a molecular weight ranging from 300 to 1 300 Da,its degree of polymerization was 3 to 12. The polymer had excellent heat resistance with a decomposition temperature of 223 ℃.
作者
朱洪玲
傅佳佳
许波
王强
Artur Cavaco Paulo
苏静
ZHU Hong-ling1,3, FU Jia-jia2,3, XU Bo1,3, WANG Qiang1,3, Artur Cavaco Paulo1,3, SU Jing1,3(1. International Joint Research Laboratory for Textile and Fiber Bioprocesses, Textile & Garment Institute, Jiangnan University, Wuxi 214122, Jiangsu, China; 2. Jiangsu Engineering Technology Research Center for Funetional Textiles Textile & Garment Institute ,Jiangnan University, Wuxi 214122 ,Jiangsu , China ;3. Key Laboratory of Eco- Textiles Ministry of Education Textile & Garment Institute, Jiangnan University, Wuxi 214122, Jiangsu, China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2018年第4期620-624,共5页
Fine Chemicals
基金
国家自然科学基金(31470509,31201134)
江苏省产学研前瞻性研究项目(BY2016022-23)
中央高校基本科研业务费专项资金资助(JUSRP51622A)
2016年度江苏省普通高校学术研究生科研创新计划项目(KYLX16_0788)~~
关键词
漆酶
4-氨基苯酚
聚合
质谱
催化技术
laccase
4-aminophenol
polymerization
mass spectroscopy
catalysis technology