采用光学显微镜和紫外可见分光光度计研究了聚丙烯腈(PAN)纤维的溶胀、溶解过程,采用旋转流变仪和激光粒度仪研究了不同组成PAN溶液的流变特性及对PAN溶液相转变的影响。结果表明:增大与溶剂的接触面积和延长时间,有利于PAN废丝的溶胀、溶解;PAN含量越多,大分子缠结作用力越大,分子间相互作用越强烈,PAN溶液的复数黏度、储能模量和损耗模量越大,在沉淀剂水中形成较大和较多的聚合物颗粒;可以用PAN废丝制备用于碳纤维原丝用的纺丝溶液。
The swelling and dissolution of polyacrylonitrile (PAN) fibers were studied by optical microscopy and ultraviolet-visible spectrophotometer.The rheological properties of PAN solutions with different compositions and their effects on the phase transition of PAN solutions were studied by rheometer and laser particle size analyzer.The results shown that increasing the contact area and prolonging time was beneficial to swelling and dissolution of waste PAN fiber.The more PAN content was,the greater the entanglement force of macromolecules,the stronger the intermolecular interaction.The greater the complex viscosity,storage modulus and loss modulus of PAN solution,the larger and more polymer particles will form in precipitating water.The waste PAN fiber was used to prepare spinning solution for carbon fiber precursor.
[1] 程卫平.聚丙烯腈基碳纤维在航天领域应用及发展[J].宇航材料工艺,2015,45(6):11-16.
[2] 向小波,蒋永凡,程勇.聚丙烯腈基碳纤维及其在固体火箭发动机壳体上的应用[J].纤维复合材料,2015,32(3):23-28.
[3] Alarifi I M,Alharbi A,Khan W S,et al.Mechanical and thermal properties of carbonized PAN nanofibers cohesively attached to surface of carbon fiber reinforced composites[J].Macromolecular Symposia,2016,365(1):140-150.
[4] 季敏霞,王成国.聚丙烯腈基碳纤维制备过程中微观结构的演变[J].材料导报,2007,21(5):111-114.
[5] 陈洞,张顺,王晓丽,等.废聚丙烯腈纤维制备高性能碳纤维研究[J].化工新型材料,2019,47(11):209-212.
[6] 吴嵩义,黄翔宇.碳纤维用聚丙烯腈聚合体溶解工艺的研究[J].石油化工技术与经济,2016,32(3):18-22.
[7] 滕宪忠.PAN聚合物一次性溶解新技术[J].炼油与化工,2003,4(1):13-15.
[8] 宋文迪.聚丙烯腈溶解行为的研究[J].石油化工技术与经济,2017,33(1):24-29.
[9] Wood H,Sourirajian S.The effect of additives,solvent type,and polymer concentration on macromolecule dimensions[J].Journal of Applied Polymer Science,1991,43(1):213-217.
[10] Wood H,Sourirajian S.The effect of polymer solution composition and film-forming procedure on aromatic polyamide membrane skin layer structure[J].J Colloid Interface Sci,1992,149(1):105-113.
[11] 莫高明,王艳菲,张若愚,等.流变和光学法研究PAN/DMSO/H2O体系的凝胶化和相分离行为[J].高分子通报,2016(9):162-170.
[12] Qian Baojun,Lin Weiping,He Jianming,et al.The role of macromolecular entanglements in the gel spinning process and properties of high performance polyacrylonitrile fiber[J].Journal of Polymer Engineering,1995,15(3-4):327-335.
[13] Beckmann J,Zenke D.Thermoreversible gelation of polyacrylonitrile/dimethylformamide-solution[J].Colloidand Polymer Science,1993,271(5):436-445.