纺织学报 ›› 2021, Vol. 42 ›› Issue (10): 34-40.doi: 10.13475/j.fzxb.20201205207

• 纤维材料 • 上一篇    下一篇

星型无卤阻燃剂改性粘胶纤维的制备及其性能

何聚1, 刘晓辉1(), 苏晓伟1, 林生根1, 任元林2   

  1. 1.天津工业大学 材料科学与工程学院, 天津 300387
    2.天津工业大学 纺织科学与工程学院, 天津 300387
  • 收稿日期:2020-12-18 修回日期:2021-06-01 出版日期:2021-10-15 发布日期:2021-10-29
  • 通讯作者: 刘晓辉
  • 作者简介:何聚(1995—),男,硕士生。主要研究方向为阻燃纤维素纤维。
  • 基金资助:
    国家重点研发计划项目(2017YFB0309000)

Preparation and properties of viscose fibers modified with star-shaped halogen-free flame retardants

HE Ju1, LIU Xiaohui1(), SU Xiaowei1, LIN Shenggen1, REN Yuanlin2   

  1. 1. School of Material Science and Engineering, Tiangong University, Tianjin 300387, China
    2. School of Textile Science and Engineering, Tiangong University, Tianjin 300387, China
  • Received:2020-12-18 Revised:2021-06-01 Published:2021-10-15 Online:2021-10-29
  • Contact: LIU Xiaohui

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摘要：

针对粘胶纤维的可燃性带来安全隐患的问题,优选含有六元环结构的六氯环三磷腈作为功能单体,设计合成了一种同时含有磷、氮、硅三元阻燃元素的星型无卤阻燃剂。将该阻燃剂添加到粘胶中,采用湿法纺丝工艺制备了阻燃改性粘胶纤维。借助傅里叶红外光谱仪、X射线光电子能谱仪、热重分析仪、热重-质谱联用系统等对阻燃改性粘胶纤维的结构和性能进行分析。结果表明:改性后粘胶纤维的阻燃性能明显提高,且具有一定的耐洗性;与未改性粘胶纤维相比,其在氮气氛围下800 ℃时的残炭量从12.5%提高到31.2%;在改性粘胶纤维燃烧过程中,可燃性气体释放量明显降低并产生大量膨胀炭层,说明阻燃剂在气相和凝聚相发挥阻燃作用。

关键词: 粘胶纤维, 共混改性, 湿法纺丝, 阻燃剂, 六氯环三磷腈, 热稳定性, 阻燃机制

Abstract:

Aiming at the potential safety hazard caused by the flammability of viscose fibers, phosphonitrilic chloride trimer containing a ring structure was selected as a functional monomer to design a star-shaped halogen-free flame retardant that combines phosphorus, nitrogen, silicon ternary flame retardant elements. The flame retardant was added to the viscose, and then the flame retardant modified viscose fibers was prepared through wetting spinning. The structures and properties of the modified viscose fibers were characterized by means of Fourier infrared spectroscopy, X-ray photoelectron spectroscopy, thermogravimetric analyzer, and thermogravimetric-mass spectrometry system. The results show that the flame retardancy of the modified viscose fibers was improved while the fibers maintaining the durability. In nitrogen atmosphere, its char residue rate at 800 ℃ increased from 12.5% to 31.2% compared with the unmodified viscose fibers. During the combustion process of the modified fibers, the release of combustible gas was significantly reduced and abundant expanded carbon layer was produced. The flame retardant operated in condensed phase and gas phase.

Key words: viscose fiber, blending modification, wetting spinning, flame retardant, phosphonitrilic chloride trimer, thermal stability, flame retardant mechanism

中图分类号: 

  • TS102.6

图1

阻燃剂的制备流程图"

图2

阻燃剂的核磁共振氢谱图"

图3

粘胶纤维和阻燃粘胶纤维的红外光谱图"

图4

粘胶纤维、阻燃粘胶纤维和水洗后阻燃粘胶纤维的XPS图"

图5

粘胶纤维、阻燃粘胶纤维和阻燃粘胶纤维燃烧后残炭的扫描电镜照片"

图6

粘胶纤维、阻燃粘胶纤维和水洗后阻燃粘胶纤维在氮气中的TG和DTG曲线"

图7

粘胶纤维、阻燃粘胶纤维和水洗后阻燃粘胶纤维在空气中的TG和DTG曲线"

图8

粘胶纤维和阻燃粘胶纤维的垂直燃烧图"

图9

粘胶纤维和阻燃粘胶纤维的TG-MS图"

图10

阻燃粘胶纤维燃烧后的拉曼光谱图"

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