干喷湿纺聚丙烯腈凝固丝的表征方法研究

Characterization method of polyacrylonitrile coagulated fiber by dry-jet wet spinning

以干喷湿纺聚丙烯腈(PAN)凝固丝为研究对象,通过优化试样处理方法和测试条件,建立了一套表征PAN凝固丝组成、形貌、结晶、取向及可拉伸性的方法。结果表明:采用擦拭法擦拭4次以上,PAN凝固丝的溶剂残留率保持稳定,萃取3 h以上可完全除去PAN凝固丝内的残留溶剂;在偏光显微镜和扫描电子显微镜下可分别观察PAN凝固丝的皮芯结构及截面的细微网状结构;PAN凝固丝的结晶度可直接使用X射线衍射仪分析计算,水洗温度对PAN凝固丝取向程度的测试结果影响较小;PAN凝固丝在空气中的自然拉伸比与在水浴中的最大拉伸倍数存在正相关性,自然拉伸比可作为衡量PAN凝固丝可拉伸性的参数。

Using polyacrylonitrile(PAN)coagulated fiber prepared by dry-jet wet spinning process as the research object,a set of methods for characterizing the composition,morphology,crystallization,orientation and stretchability of PAN coagulated fiber was established by optimizing sample treatment methods and testing conditions.The results showed that the solvent residual rate of PAN coagulated fiber remained stable after wiping more than 4 times,and the residual solvent in PAN coagulated fiber could be completely removed by extraction for more than 3 h;the skin-core structure and the fine network structure of the cross section of the PAN coagulated fiber could be observed repectively with polarizing microscope and scanning electron microscope;the crystallinity of PAN coagulated fiber could be directly analyzed and calculated with X-ray diffractometer,and the washing temperature had little effect on the test results of the orientation degree of PAN coagulated fiber;there was a positive correlation between the natural stretch ratio of PAN coagulated fiber in air and the maximum stretch ratio in water bath,and the natural stretch ratio could be used as a parameter to measure the stretchability of PAN coagulation fiber.