六次甲基四胺交联酚醛纤维的制备及其性能

doi:10.13475/j.fzxb.20210500406

纺织学报 ›› 2022, Vol. 43 ›› Issue (05): 57-62.doi: 10.13475/j.fzxb.20210500406

六次甲基四胺交联酚醛纤维的制备及其性能

赵波波¹, 王亮¹(), 李敬毓², 万刚³, 夏兆鹏¹, 刘雍¹

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

收稿日期:2021-05-06 修回日期:2022-01-17 出版日期:2022-05-15 发布日期:2022-05-30
通讯作者: 王亮
作者简介:赵波波(1997—),男,硕士生。主要研究方向为酚醛树脂纤维。
基金资助:
天津市自然科学基金项目(18JCQNJC71600)

Preparation and properties of hexamethylenetetramine cross-linked phenolic fibers

ZHAO Bobo¹, WANG Liang¹(), LI Jingyu², WAN Gang³, XIA Zhaopeng¹, LIU Yong¹

1. School of Textile Science and Engineering, Tiangong University, Tianjin 300387, China
2. Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China
3. Qingdao Jifa Group Co., Ltd., Qingdao, Shandong 266299, China

Received:2021-05-06 Revised:2022-01-17 Published:2022-05-15 Online:2022-05-30
Contact: WANG Liang

摘要/Abstract

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。

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

Abstract:

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.

Key words: phenolic fiber, hexamethylenetetramine, curing, mechanical property, thermal stability

中图分类号:

TQ342

赵波波, 王亮, 李敬毓, 万刚, 夏兆鹏, 刘雍. 六次甲基四胺交联酚醛纤维的制备及其性能[J]. 纺织学报, 2022, 43(05): 57-62.

ZHAO Bobo, WANG Liang, LI Jingyu, WAN Gang, XIA Zhaopeng, LIU Yong. Preparation and properties of hexamethylenetetramine cross-linked phenolic fibers[J]. Journal of Textile Research, 2022, 43(05): 57-62.

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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

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