六次甲基四胺交联酚醛纤维的制备及其性能  

Preparation and properties of hexamethylenetetramine cross-linked phenolic fibers

作　　者：赵波波 王亮[1] 李敬毓 万刚 夏兆鹏[1] 刘雍[1] ZHAO Bobo;WANG Liang;LI Jingyu;WAN Gang;XIA Zhaopeng;LIU Yong(School of Textile Science and Engineering, Tiangong University, Tianjin 300387, China;Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China;Qingdao Jifa Group Co. , Ltd. , Qingdao, Shandong 266299, China)

机构地区：[1]天津工业大学纺织科学与工程学院,天津300387 [2]中国科学院化学研究所,北京100190 [3]青岛即发集团股份有限公司,山东青岛266299

出　　处：《纺织学报》2022年第5期57-62,共6页Journal of Textile Research

基　　金：天津市自然科学基金项目(18JCQNJC71600)。

摘　　要：针对在制备酚醛纤维过程中醛类交联剂对人体及环境危害较大的问题,采用六次甲基四胺(HMTA)作为交联剂在盐酸溶液中制备酚醛纤维,探讨了交联浴配比、升温速率、交联浴温度以及热处理温度对纤维力学性能、耐热性能的影响。结果表明:与初生纤维相比,交联酚醛纤维的力学性能、热稳定性均得到了较大改善;在盐酸和HMTA质量比为1.2∶1,交联浴以15℃/h的升温速率升至120℃后恒温1.5 h条件下制得预交联酚醛纤维,然后于200℃真空氛围下处理2 h,得到的交联酚醛纤维的断裂强度为3.63 cN/dtex,断裂伸长率为7.7%,初始分解温度高达386℃,氮气氛围下900℃处理1 h后质量保留率为60.7%。本文提出的以HMTA为交联剂制备酚醛纤维的方法对建立酚醛纤维的绿色环保生产工艺路线具有指导意义。Aiming at the problem that the aldehyde crosslinking agent is harmful to the human body and the environment during the preparation of phenolic fibers,hexamethylenetetramine(HMTA)was used as crosslinking agent to prepare phenolic fiber in hydrochloric acid solution.The effects of crosslinking bath ratio,heating rate,crosslinking bath temperature and heat treatment temperature on the fiber mechanical properties and heat resistance were studied.The results show that the mechanical properties and thermal stability of phenolic fiber are greatly improved after crosslinked.The pre-crosslinked phenolic fiber was prepared under the condition that the mass ratio of HCl and HMTA is 1.2,the temperature of cross-linking bath is raised to 120℃at a heating rate of 15℃/h and constant temperature for 1.5 h,and the cross-linked phenolic fiber obtained by treating at 200℃in a vacuum atmosphere for 2 h.The maximum breaking strength of the cross-linked phenolic fibers reaches to 3.63 cN/dtex and breaking elongation is 7.7%respectively.The initial decomposition temperature reaches to 386℃and the mass retention rate at 900℃in a nitrogen atmosphere is 60.7%.The method used in this research for preparing phenolic fiber with HMTA as cross-linking agent has guiding significance for establishing the green and environmentally friendly production process route.

关 键 词：酚醛纤维 六次甲基四胺 交联固化 力学性能 热稳定性能 

分 类 号：TQ342[化学工程—化纤工业]