气相色谱法分析PPTA粉体中NMP的残留量  

Determination of NMP residue in PPTA powder by gas chromatography

作　　者：苏凤仙 陈建梅 季轩 徐哲峰 Su Fengxian;Chen Jianmei;Ji Xuan;Xu Zhefeng(Research Institute of Sinopec Yizheng Chemical Fibre Co.,Ltd.,Yizheng Jiangsu 211900,China;Jiangsu Key Laboratory of High Performance Fiber,Yizheng Jiangsu 211900,China)

机构地区：[1]中国石化仪征化纤有限责任公司研究院,江苏仪征211900 [2]江苏省高性能纤维重点实验室,江苏仪征211900

出　　处：《合成技术及应用》2024年第3期54-60,共7页Synthetic Technology & Application

摘　　要：N-甲基吡咯烷酮(NMP)作为对苯二甲酰氯和对苯二胺的聚合溶剂,会有部分残留于聚对苯二甲酰对苯二胺(PPTA)产品中,影响PPTA产品质量。国际环保组织协会将NMP列入Standard100限用检测列表,明确提出了NMP残留量的限值。为了测定PPTA粉体中NMP残留量,采用超声萃取-气相色谱法分析PPTA粉体中NMP的残留量,通过探索色谱柱、柱温、柱流速、分流比等,确定合适的色谱条件,通过研究萃取溶剂、萃取温度、萃取时间、称样量等,确定合适的萃取条件。建立的分析方法重复性优于3.0%,再现性优于5.0%,回收率范围为84.81%~103.15%,检出限优于0.0009%,说明本方法的精密度好、准确度高,能满足PPTA粉体中NMP残留量的测试需求。Polyp-phenyl-phthalyl-p-phenylenediamine(PPTA)polymeric solventN-methylpyrrolidone(NMP)will partially linger in PPTA products,impacting their quality.The Standard 100 Limited use test list,published by the International Association of Environmental Organizations,explicitly states the maximum amount of residue that can be left over after using NMP.This study used gas chromatography and ultrasonic extraction to ana-lyze the remaining NMP in PPTA powder.The ideal chromatographic conditions were found by examining the col-umn,temperature,flow rate,split ratio,and other factors.The ideal extraction conditions were found by exami-ning the extraction solvent,temperature,time,and sample weight.The established analytical method has demon-strated better than 3.0%reproducibility,5.0%reproducibility,84.81%~103.15%recovery range,and better than 0.0009%detection limit.These results demonstrate the method's high precision and accuracy,as well as its ability to meet the testing requirements for NMP residue in PPTA powder.

关 键 词：聚对苯二甲酰对苯二胺 N-甲基吡咯烷酮 气相色谱法 萃取 

分 类 号：O657.7[理学—分析化学]