Journal of Textile Research ›› 2022, Vol. 43 ›› Issue (05): 57-62.doi: 10.13475/j.fzxb.20210500406

• Fiber Materials • Previous Articles     Next Articles

Preparation and properties of hexamethylenetetramine cross-linked phenolic fibers

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

  1. 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 Online:2022-05-15 Published:2022-05-30
  • Contact: WANG Liang E-mail:liangwang@tiangong.edu.cn

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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

CLC Number: 

  • TQ342

Fig.1

Schematic diagram of fiber crosslinking process"

Fig.2

Influence of different factors on fiber mechanical properties. (a)Mass fraction of HCl; (b)Heating rate of curing-link bath;(c)Temperature of curing-link bath;(d)Heating-temperature"

Fig.3

SEM images of samples (×5 000).(a)Surface of raw fiber;(b)Surface of cured fiber;(c)Section of raw fiber; (d)Section of cured fiber"

Fig.4

FT-IR spectra of raw fiber, pre-cured fiber and cured fiber"

Fig.5

Curing reaction mechanism of phenolic fiber. (a)Reaction equation of HMTA and HCl;(b)Molecular structure changes of cross-linking process"

Fig.6

TG(a)and DTG(b)curves of fibers before and after curing-linked"

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