准确获得聚丙烯腈(PAN)原丝含油率,可有效地控制原丝品质、碳纤维生产稳定及有效地降低生产成本。研究了提取剂、提取方法、纤维状态以及提取方法组合对PAN原丝含油率测定的影响,开发了适用原丝生产企业的简便、准确和稳定性好的原丝含油率测定方法。结果表明:在提取剂相同时,抽提法测试所得PAN原丝含油率均大于回流法0.02%～0.04%,但抽提法CV值为4.2%,而回流法CV值在1%左右,小于数据更稳定;纤维完全松散或棉线绑定,不影响含油率测定,但滤纸包裹纤维会吸附0.01%～0.02%油剂;相同的提取方法,乙醚作为提取剂的含油率测定比二氯甲烷高0.06%～0.07%;经回流提取后再进行二次抽提,仍可获得0.12%～0.21%不等的油剂,上油原丝、二氯甲烷回流提取原丝、再经乙醚二次抽提的原丝进行X射线光电子能谱技术分析,Si相对C的含量 Si 2p/C 1s逐步下降,由48.31%分别下降至17.96%、11.09%,回流法和抽提法结合更能稳定、真实地获取原丝真实含油率,是PAN碳纤维原丝厂家适用的原丝含油率测定方法。

Accurate oil content of PAN precursor can effectively control precursor quality,stabilize carbon fiber production and effectively reduce production cost.The influence of extraction agent,extraction method,fiber state and the combination of extraction methods on the determination of oil content of PAN precursor was studied.A simple,accurate and stable method for determination of oil content of PAN precursor was developed.The results showed that the oil content of PAN precursor obtained by extraction method was higher than that by reflux method by 0.02%～0.04%,but the CV value of extraction method was 4.2%,and the CV value of reflux method was about 1%,which was less than the data more stable.The fiber was completely loose or bound with cotton thread,which did not affect the determination of oil content,but the filter paper wrapped fiber would adsorb 0.01%～0.02% oil agent Compared with dichloromethane,the oil content was 0.06%～0.07% higher than that of dichloromethane,and 0.12%～0.21% oil could still be obtained after the second extraction after reflux extraction.XPS analysis showed that the content of Si relative to C Si 2p/C 1s decreased gradually from 48.31% to 9.31% and 17.96% from 11.09%.The combination of reflux and extraction was more stable and real.It was a suitable method to determine the oil content of PAN carbon fiber precursor.