含嘧啶杂环聚酰亚胺纤维的湿法纺丝成形及结构性能Fabrication, Structure and Properties of Polyimide Fiber Containing Pyrimidine Moiety Prepared by Wet-Spinning Method
甘锋,董杰,张殿波,谭文军,赵昕,张清华
GAN Feng,DONG Jie,ZHANG Dian-bo,TAN Wen-jun,ZHAO Xin,ZHANG Qing-hua
摘要(Abstract):
以2,5-二(4-氨基苯基)嘧啶与3,3',4,4'-联苯二酐聚合得到高分子质量的聚酰胺酸溶液,采用"两步法"湿法纺丝制备聚酰亚胺纤维,研究了凝固浴组成对纤维成形形貌的影响以及热亚胺化、热牵伸作用对纤维聚集态结构的影响。三元相图与扫描电镜结果显示:过快或过慢的凝固速度均不利于形成规则、致密结构的纤维,以体积比5/5的H2O/DMAc混合溶液为凝固浴时,纤维成形较佳。同步辐射结果显示:热环化、热牵伸均可促进纤维形成更为完善的晶态、取向结构。最终得到聚酰亚胺纤维的最高拉伸强度、模量分别达1.72 GPa与95.1 GPa,此外所得纤维具有优异的耐热稳定性。
An aromatic poly(amic acid) dope was synthesized from 2,5-bis(4-aminophenyl)-pyrimidine and3,3',4,4'-biphenyltetracarboxylic dianhydride. The corresponding polyimide fiber was fabricated via a two-step wet-spinning method. The morphology and aggregation structure of the fiber were investigated by scan-ning electron microscope(SEM) and 2 D-wide angle X-ray diffraction(2 D-WAXD) technology. The SEM re-sults indicate that the as-spun precursor fiber with a regular and dense morphology is obtained in the H2 O/DMAc solution at a volume ratio of 5/5. 2 D-WAXD data reveales that the better-define crystal structure for-mation is mainly induced by the effects of thermal and thermal stretching. The obtained polyimide fibershows excellent thermal oxidative stability and the optimal tensile strength and modulus reaches to 1.72 GPa and 95.1 GPa, respectively.
关键词(KeyWords):
湿法纺丝;聚酰亚胺纤维;聚集态结构;嘧啶杂环
wet-spinning;polyimide fiber;aggregation structure;pyrimidine unit
基金项目(Foundation): 国家自然科学基金项目(编号51233001);; 973计划课题(2014CB643603)
作者(Author):
甘锋,董杰,张殿波,谭文军,赵昕,张清华
GAN Feng,DONG Jie,ZHANG Dian-bo,TAN Wen-jun,ZHAO Xin,ZHANG Qing-hua
DOI: 10.16090/j.cnki.hcxw.20180116.001
参考文献(References):
- [1]AFSHARI M,SIKKEMA DJ,LEE K,et al.High performance fibers based on rigid and flexible polymers[J].Polymer Reviews,2008,48(2):230-274.
- [2]LIAW DJ,WANG KL,HUANG YC,et al.Advanced polyimide materials:syntheses,physical properties and applications[J].Progress in Polymer Science,2012,37(7):907-974.
- [3]BHAT G,SCHWANKE R.J.Thermal properties of a polyimide fiber[J].Journal of Thermal Analysis,1997,49(1):399-405.
- [4]向红兵,陈蕾,胡祖明.聚酰亚胺纤维及其纺丝工艺研究进展[J].高分子通报,2011(1):40-50.
- [5]LUO L,YAO J,WANG X,et al.The evolution of macromolecular packing and sudden crystallization in rigid-rod polyimide via effect of multiple H-bonding on charge transfer(CT)interactions[J].Polymer,2014,55(16):4258-4269.
- [6]LUO L,WANG Y,ZHANG J,et al.The effect of asymmetric heterocyclic units on the microstructure and the improvement of mechanical properties of three rigid-rod co-PI fibers[J].Macromolecular Materials and Engineering,2016,301(7):853-863.
- [7]NIU H,HUANG M,QI S,et al.High-performance copolyimide fibers containing quinazolinone moiety:Preparation,structure and properties[J].Polymer,2013,54(6):1700-1708.
- [8]SUKHANOVA TE,BAKLAGINA YG,KUDRYAVTSEV VV,et al.Morphology,deformation and failure behaviour of homo-and copolyimide fibres:1.Fibres from 4,4′-oxybis(phthalic anhydride)(DPh O)and pphenylenediamine(PPh)or/and 2,5-bis(4-aminophenyl)-pyrimidine(2,5PRM)[J].Polymer,1999,40(23):6265-6276.
- [9]YIN C,DONG J,LI Z,et al.Ternary phase diagram and fiber morphology for nonsolvent/DMAc/polyamic acid systems[J].Polymer Bulletin,2015,72(5):1039-1054.
- [10]DONG R,ZHAO J,ZHANG Y,et al.Morphology control of polyacrylonitrile(PAN)fibers by phase separation technique[J].Journal of Polymer Science Part B Polymer Physics,2009,47(3):261-275.
- [11]DONG J,YIN C Q,LU H X,et al.Morphology control of polyimide fibers by phase separation under different coagulation bath conditions[C]//Materials Science Forum,2014,789:142-147.
- [12]ZIABICKI A,JARECKI L.Potential energy barriers in the kinetic theory of nucleation[J].Journal of Chemical Physics,1984,80(11):5751-5753.
- [13]MURAKAMI S,NISHIKAWA Y,TSUJI M,et al.A study on the structural changes during uniaxial drawing and/or heating of poly(ethylene naphthalene-2,6-dicarboxylate)films[J].Polymer,1995,36(2):291-297.
- [14]YIN C,DONG J,TAN W,et al.Strain-induced crystallization of polyimide fibers containing 2-(4-aminophenyl)-5-aminobenzimidazole moiety[J].Polymer,2015,75:178-186.