基于干法纺丝的含二氮杂萘酮结构聚芳醚酮纤维制备及其性能

doi:10.13475/j.fzxb.20200501006

纺织学报 ›› 2020, Vol. 41 ›› Issue (12): 1-6.doi: 10.13475/j.fzxb.20200501006

• 纤维材料 • 下一篇

基于干法纺丝的含二氮杂萘酮结构聚芳醚酮纤维制备及其性能

董大林¹, 宾月珍¹(), 蹇锡高¹^,²

1.大连理工大学化工学院, 辽宁大连 116024
2.辽宁省高性能树脂工程技术研究中心, 辽宁大连 116024

收稿日期:2020-05-06 修回日期:2020-09-04 出版日期:2020-12-15 发布日期:2020-12-23
通讯作者: 宾月珍
作者简介:董大林(1992—),男,博士生。主要研究方向为聚芳醚酮纤维制备及其结构。
基金资助:
国家自然科学基金项目(21374014);国家自然科学基金项目(U1663226)

Preparation and properties of poly(phthalazinone ether ketone) fibers by dry spinning

DONG Dalin¹, BIN Yuezhen¹(), JIAN Xigao¹^,²

1. School of Chemical Engineering, Dalian University of Technology, Dalian, Liaoning 116024, China
2. Liaoning Province Engineering Technology Center of High Performance Resins, Dalian, Liaoning 116024, China

Received:2020-05-06 Revised:2020-09-04 Online:2020-12-15 Published:2020-12-23
Contact: BIN Yuezhen

摘要/Abstract

摘要：

为拓展含二氮杂萘酮结构的聚芳醚酮(PPEK)高性能树脂在纤维材料领域的应用,采用对氯苯酚与1,1',2,2'-四氯乙烷(二者体积比为1:1)混合溶剂溶解PPEK制备纺丝液,通过干法纺丝得到PPEK纤维。借助旋转流变仪、差示扫描量热仪、偏光显微镜、拉伸试验机、X射线衍射仪以及声速取向仪等对PPEK纺丝液以及PPEK纤维的结构与性能进行表征。结果表明:PPEK质量分数为40%时,最优纺丝温度为140 ℃;初生PPEK纤维经1.43倍热拉伸后,其断裂强度为167.6 MPa,弹性模量为4.6 GPa,声速取向因子为0.570 5;经热拉伸后,PPEK纤维保持无定形态,且玻璃化转变温度均高于250 ℃,具有良好的耐热性能。

关键词: 聚芳醚酮, 二氮杂萘酮, 混合溶剂, 干法纺丝, 耐高温性能

Abstract:

To expand applications of poly(phthalazinone ether ketone) (PPEK) in fiber preparation, PPEK fibers were prepared by dry spinning with PPEK and mixed solvent of p-chlorophenol and 1,1',2,2'-tetrachloroethane (volume ratio is 1:1). PPEK solution and PPEK fibers were characterized by rotating rheometer, differential scanning calorimeter, polarizing microscope, universal tensile tester, X-ray diffractometer and fiber sound velocimeter. The results show that optimal spinning temperature of 40% PPEK solution is 140 ℃. After being elongated by 1.43 times, breaking strength, elastic modulus and sonic orientation factor of PPEK fibers reach 167.6 MPa, 4.6 GPa and 0.570 5, respectively. Hot elongated PPEK fibers has good heat resistance and remains amorphous with glass transition temperature of higher than 250 ℃.

Key words: poly(aryl ether ketone), diazanaphthalene, mixed solvent, dry spinning, high temperature resistance performance

中图分类号:

TQ342

董大林, 宾月珍, 蹇锡高. 基于干法纺丝的含二氮杂萘酮结构聚芳醚酮纤维制备及其性能[J]. 纺织学报, 2020, 41(12): 1-6.

DONG Dalin, BIN Yuezhen, JIAN Xigao. Preparation and properties of poly(phthalazinone ether ketone) fibers by dry spinning[J]. Journal of Textile Research, 2020, 41(12): 1-6.

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样品编号	喷丝孔直径/mm	喷丝孔长径比	柱塞直径/ mm	加热料桶温度/ ℃	柱塞下降速度/ (mm·s^-1)	纺丝液喷出速度/ (cm·s^-1)	热甬道7 温度/ ℃	热甬道9 温度/ ℃	收丝辊线速度/ (cm·s^-1)	牵伸比	线密度/tex
1^#	0.5	2.0	14.89	140	0.044 9	3.98	—	—	—	—	516.4
2^#	0.5	2.0	14.89	140	0.065 1	5.77	160	280	14.56	2.52	45.0

拉伸倍数	屈服强度/MPa	屈服应变/%	断裂强度/MPa	断裂应变/%	弹性模量/GPa
未拉伸	53.6±0.2	6.0±0.3	49.5±0.2	170.7±4.4	2.0±0.1
0.50	102.8±0.1	6.9±0.4	97.6±0.3	93.1±1.2	2.8±0.3
1.00			151.3±0.2	9.2±0.5	4.3±0.1
1.43			167.6±0.1	8.8±0.3	4.6±0.1

拉伸倍数	C/(m·s^-1)	f_s
未拉伸	2 490 ± 30	0.268 3
0.50	2 720 ± 20	0.386 8
1.00	3 050 ± 10	0.512 3
1.43	3 250 ± 10	0.570 5

基于干法纺丝的含二氮杂萘酮结构聚芳醚酮纤维制备及其性能

Preparation and properties of poly(phthalazinone ether ketone) fibers by dry spinning

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