前驱体法合成PPESK-b-PEDEK及其性能  

Synthesis of Block Copolymer PPESK-b-PEDEK by Precursor Method and Its Properties

作　　者：林显泷 郭皓[2] 鲍锋 王锦艳[2] 蹇锡高[2] Xianlong Lin;Hao Guo;Feng Bao;Jinyan Wang;Xigao Jian(School of Ocean Science and Technology Panjin Campus,Dalian University of Technology,Panjin 124221,China;Department of Polymer Science & Materials,College of Chemical Engineering,Dalian University of Technology,Dalian 116024,China)

机构地区：[1]大连理工大学盘锦校区海洋科学与技术学院,辽宁盘锦124221 [2]大连理工大学化工学院高分子材料系,辽宁大连116024

出　　处：《高分子材料科学与工程》2019年第8期30-35,41,共7页Polymer Materials Science & Engineering

摘　　要：从分子设计的角度出发,采用前驱体法成功制备了3种含杂萘联苯结构嵌段共聚物PPESK-b-PEDEK。首先,设计合成了一种新型双卤单体4,4′-二氟二苯酮亚胺(Ketimine),代替4,4′-二氟二苯酮(DFK)与联苯二酚(BP)进行亲核取代反应,制备了3种酚氧盐封端的可溶性聚醚醚酮PEDEK(P)低聚物。然后与F/Cl封端的含杂萘酮联苯结构聚芳醚砜酮O-PPESK低聚物进行嵌段共聚制备可溶性前驱体PPESK-b-PEDEK(P),水解得到嵌段共聚物PPESK-b-PEDEK。红外、乌氏黏度及索提测试证明了嵌段共聚物的成功制备。热重分析、差示扫描量热分析、X射线衍射测试表明,随着PEDEK链段长度的增加,嵌段共聚物的玻璃化转变温度(Tg)降低,而热氧稳定性和结晶性却有所增加。溶解性测试表明,前驱体具有优异的溶解能力,嵌段共聚物的溶解性能有所降低。From the point of molecular design, three different block copolymers PPESK-b-PEDEK with phthalazinone moiety were successfully synthesized via precursor method. Firstly, a novel double halide monomer, 4, 4′-two fluorine diphenyl ketone imide(Ketimine), was designed and prepared. It replaced DFK and performed nucleophilic substitution with BP to prepare three soluble poly(ether ether ketone) oligomers PEDEK(P) with high molecular weight. Then, the PEDEK(P) reacted with O-PPESK to prepare soluble block copolymer precursors(Block(P)). The precursors were hydrolyzed under acidic conditions, the block copolymers were obtained. The structures of blocks were confirmed by Fourier transform infrared spectrometer(FT-IR) and wide-angle X-ray diffractometer(WAXD). The results of thermal gravimetric analyzer(TGA), differential scanning calorimeter(DSC) and WAXD show that as the length of the PEDEK segment increases, the glass transition temperature(T_g) of the block copolymers decreases, while the thermal oxygen stability and crystallinity increase. The solubility test shows that the precursor has an excellent solubility while the solubility of block copolymers is decreased.

关 键 词：嵌段聚合物 二氮杂萘酮联苯 前驱体 耐热性 溶解性 

分 类 号：TQ316.61[化学工程—高聚物工业]