接枝法制备聚丙烯腈-聚偕胺肟纤维 及其结构与性能研究  

Study on structure and properties of polyacrylonitrile-polyamidoxime fibers prepared via grafting method

作　　者：薛娟 孙世操 刘彦洋 白亚楠 苗雷 樊亚玲 黄国庆 范海明 陈兆文 XUE Juan;SUN Shicao;LIU Yanyang;BAI Yanan;MIAO Lei;FAN Yaling;HUANG Guoqing;FAN Haiming;CHEN Zhaowen(The 718th Research Institution of CSSC,Handan 056027)

机构地区：[1]中国船舶集团有限公司第七一八研究所,河北邯郸056027

出　　处：《合成纤维工业》2024年第5期38-43,共6页China Synthetic Fiber Industry

摘　　要：通过聚合、改性、接枝三步法制备聚丙烯腈-聚偕胺肟(PAN-PAO)纤维。首先利用自由基聚合制备低相对分子质量聚丙烯腈(PAN),然后通过盐酸羟胺对PAN进行偕胺肟化改性制备可溶性聚偕胺肟(PAO),最后将PAO接枝到PAN羧酸(PAN-COOH)纤维上制备PAN-PAO纤维;研究了聚合反应时间和温度对PAN相对分子质量的影响,以及PAN相对分子质量、接枝反应时间和温度对PAN-PAO纤维偕胺肟(AO)基含量的影响,并对PAN-PAO纤维的结构及力学性能进行表征。结果表明:较佳的聚合反应条件为反应时间30 min、反应温度80℃,得到的PAN数均相对分子质量为29300;较佳的接枝反应条件为PAN数均相对分子质量小于30000、反应时间6 h、反应温度70℃,制备的PAN-PAO纤维AO基含量为1.09 mmol/g;红外光谱中C=N和N=O特征峰的出现证实通过接枝法成功制备了PAN-PAO纤维;在AO基含量均为1.1 mmol/g的条件下,PAN-PAO纤维的断裂强度为3.06 cN/dtex,高于直接法制备的聚丙烯腈-偕胺肟(PAN-AO)纤维的断裂强度(2.73 cN/dtex)。Polyacrylonitrilated-polyamidoxime(PAN-PAO)fibers were prepared through a three-step method involving polymerization,modification and grafting.Firstly,low-relative molecular mass PAN was prepared by free radical polymerization;then soluble PAO was prepared by amidoxime modification of PAN with hydroxylamine hydrochloride;finally,PAO was grafted onto carboxylated polyacrylonitrile(PAN-COOH)fibers to prepare PAN-PAO fibers.The effects of polymerization reaction time and temperature on the relative molecular mass of PAN were studied,as were the effects of PAN relative molecular mass,grafting reaction time and temperature on the content of amidoxime(AO)groups in PAN-PAO fibers.The structure and mechanical properties of PAN-PAO fibers were characterized.The results showed that the optimal polymerization reaction conditions were a reaction time of 30 min and reaction temperature of 80℃,resulting in a PAN number average relative molecular mass of 29300;the optimal grafting reaction conditions were a PAN number average relative molecular mass lower than 30000,reaction time of 6 h and reaction temperature of 70℃,contributing an AO group content of 1.09 mmol/g to the prepared PAN-PAO fibers;the presence of C=N and N=O characteristic peaks in infrared spectra confirmed the successful preparation of PAN-PAO fibers by grafting method;and the breaking strength of PAN-PAO fibers was 3.06 cN/dtex when the AO content was 1.1 mmol/g,which was higher than that of polyacrylonitrile-amidoxine(PAN-AO)fibers(2.73 cN/dtex)prepared by direct method.

关 键 词：聚丙烯腈纤维 偕胺肟纤维 自由基聚合 偕胺肟化 接枝法 

分 类 号：TQ342.84[化学工程—化纤工业]