合成纤维工业2024,Vol.47Issue(5) :38-43.

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

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
合成纤维工业2024,Vol.47Issue(5) :38-43.

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

薛娟 1孙世操 1刘彦洋 1白亚楠 1苗雷 1樊亚玲 1黄国庆 1范海明 1陈兆文1
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作者信息

  • 1. 中国船舶集团有限公司第七一八研究所,河北邯郸 056027
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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29 300;较佳的接枝反应条件为PAN数均相对分子质量小于30 000、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—0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).

Abstract

Polyacrylonitrilated-polyamidoxime(PAN-PAO)fibers were prepared through a three-step method involving poly-merization,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 re-action time and temperature on the content of amidoxime(AO)groups in PAN-PAO fibers.The structure and mechanical proper-ties 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 29 300;the op-timal grafting reaction conditions were a PAN number average relative molecular mass lower than 30 000,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 pres-ence of C=N and N—O characteristic peaks in infrared spectra confirmed the successful preparation of PAN-PAO fibers by graft-ing 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

Key words

polyacrylonitrile fiber/amidoxime fiber/free radical polymerization/amidoxime modification/grafting method

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出版年

2024
合成纤维工业
中国石化集团巴陵石油化工有限责任公司 中国石化集团公司合成纤维科技情报中心站

合成纤维工业

CSTPCD
影响因子:0.417
ISSN:1001-0041
参考文献量10
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