主链含酞和芴结构的无定形聚芳醚酮的合成  

Synthesis of Amorphous Polyaryletherketone Containing Phthalein and Fluorene as Side Groups

作　　者：王志鹏[1,2] 王菲菲[1,2] 王红华[1] 周光远[1] 

机构地区：[1]中国科学院长春应用化学研究所,生态环境高分子材料重点实验室,长春130022 [2]中国科学院大学,北京100049

出　　处：《高等学校化学学报》2014年第11期2487-2493,共7页Chemical Journal of Chinese Universities

基　　金：吉林省科技发展计划项目(批准号:20130204029GX)资助~~

摘　　要：通过共聚改性在酚酞聚芳醚酮（PEK—C）的主链上引入含芴侧基，制备了一系列主链含酞和芴结构的线性高分子量无定形聚芳醚酮无规共聚物．通过傅里叶红外光谱（FTIR）、核磁共振谱（^1H，^13C NMR）等手段确定了共聚物结构．凝胶渗透色谱（GPC）数据表明，共聚物的Mn^-〉6．0×10^4，Mw^-〉1．0×10^5，PDI（Mw^-／Mn^-）范围在1．6—1．7之间．X射线衍射（XRD）数据表明共聚物系无定形结构，差示扫描量热法（DSC）和热重分析（TGA）测试表明聚合物具有良好的耐热性；初始热分解温度高于467℃；700℃时残炭率大于58．9％；共聚物呈现单一的玻璃化转变温度（Tg〉243℃）．当酚酞与双酚芴摩尔比在3：7—5：5范围时，共聚物的弹性模量和断裂伸长率显著提高，可分别达到3．1GPa和58％，是酚酞聚芳醚酮的1．4倍和8．3倍．这类含酞和芴侧基的无定形聚芳醚酮保持了在氯仿、二氯甲烷、四氢呋喃（THF）和甲基吡咯烷酮（NMP）等极性非质子溶剂中良好的溶解性能，并显著提高了聚合物的力学性能和热性能．A series of linear high molecular weight amorphous polyaryletherketone （PAEK） copolymers with phthalein and fluorene side groups was synthesized on the basis of the polyetherketone with phthalein cardo group （PEK-C）. The structures were characterized by FTIR, ^1H NMR, ^13C NMR. Gel permeation chromatog- raphy（GPC） data indicated that the Mn^- and the Mw^- of the copolymer were higher than 6.0×10^4 and 1.0×10^5, respectively, with a polydisperity index （PDI） ranging from 1.6 to 1.7. The X-ray diffraction （XRD） data revealed that the copolymers were amorphous structure. Thermogravimetric analysis （TGA） and differential scanning calorimetry （DSC） tests showed that the copolymers exhibited good heat resistant property. The onset temperature of mass loss was higher than 467 ℃. The char yield at 700 ℃ was more than 58.9%. There was a single glass transition temperature （ Tg） , with Tg 〉243 ℃. The elastic modulus and elongation at break of the copolymer showed a significant increase, up to 3.1 GPa and 58%, respectively, which were 1.4 folds and 8.3 folds compared to that of PEK-C when the feed ratio of phenolphthalein and 9,9-bis （4-hydroxyphenyl） fluorene was between 3 ： 7 and 5 ： 5. Amorphous polyaryletherketone containing phthalein and fluorene as side groups kept good solubility in chloroform, dichloromethane, tetrahydrofuran （ THF）, N-methyl-2-pyrrolidone （NMP） and other aprotie solvents. The mechanical and thermal properties were improved significantly.

关 键 词：无定形聚芳醚酮 共聚物 酚酞 双酚芴 高性能树脂 

分 类 号：O633.1[理学—高分子化学]