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水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能

程岩 王诏田 罗洪杰 吴林丽 陈曦平 姜昊

程岩, 王诏田, 罗洪杰, 等. 水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能[J]. 复合材料学报, 2022, 40(0): 1-11
引用本文: 程岩, 王诏田, 罗洪杰, 等. 水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能[J]. 复合材料学报, 2022, 40(0): 1-11
Yan CHENG, Zhaotian WANG, Hongjie LUO, Linli WU, Xiping CHEN, Hao JIANG. Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre[J]. Acta Materiae Compositae Sinica.
Citation: Yan CHENG, Zhaotian WANG, Hongjie LUO, Linli WU, Xiping CHEN, Hao JIANG. Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre[J]. Acta Materiae Compositae Sinica.

水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能

基金项目: 国家自然科学基金资助项目(51874093)
详细信息
    通讯作者:

    罗洪杰,教授,博士生导师,研究方向为多孔材料制备与固废回收 E-mail:neuhjluo@sina.com

  • 中图分类号: 文献标志码:A

Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre

  • 摘要: 现有玄武岩纤维制成的高温烟气滤袋工作温度为280℃,难以在300℃甚至更高的温度下长期工作。为了提高玄武岩纤维的耐热性能,本研究合成了一种水溶性锆杂化硅树脂浸润剂,并用于玄武岩纤维表面改性。用FTIR、TG-DSC、SEM、AFM、DCA及拉伸实验对锆杂化硅树脂及改性纤维进行了微观结构和性能表征。结果表明:锆杂化硅树脂的初始热分解温度为320~360℃;浸润后的玄武岩纤维表面包裹着一层致密、均匀的硅树脂膜,这层膜增大了纤维表面的粗糙度和表面积,提高了纤维的表面能,改变了纤维的表面结构,修复了纤维的表面微缺陷;力学测试表明:浸润后的纤维在300℃热处理2 h后,最优断裂强力值为376 N,强力保持率91.30%,断裂伸长率为2.64%,优于未被浸润纤维(287 N、69.24%、1.93%)的相关性能。因此,锆杂化硅树脂浸润剂可显著提高玄武岩纤维的耐热性能。

     

  • 图  1  水溶性锆杂化硅树脂合成图

    Figure  1.  Synthesis scheme of water-soluble zirconium hybrid silicone resin

    图  2  锆杂化硅树脂(Zr-SR)的FTIR图谱

    Figure  2.  FTIR spectra of zirconium hybrid silicone resin (Zr-SR)

    图  3  Zr-SR的TG曲线(a)和DSC曲线(b)

    Figure  3.  TG curves (a) and DSC curves (b)of Zr-SR

    图  5  BF和Zr-SR/BF-1~Zr-SR/BF-5的AFM图

    Figure  5.  AFM morphologies of basalt fibre BF and Zr-SR/BF-1~Zr-SR/BF-5

    BF (a); Zr-SR/BF-1 (b); Zr-SR/BF-2 (c); Zr-SR/BF-3 (d); Zr-SR/BF-4 (e); Zr-SR/BF-5 (f)

    图  6  BF和Zr-SR/BF的表面积值及表面粗糙度值

    Figure  6.  Surface roughness and surface area values of BF and Zr-SR/BF

    图  7  BF和Zr-SR/BF-4的XPS全谱图(a);Zr-SR/BF-4的Zr3 d(b)、O1 s(d)和Si2 p(f),BF的O1 s(c)、Si2 p(e)XPS分谱图Fig 7 XPS spectra of BF and Zr-SR/BF-4 (a); XPS patterns of Zr3 d (b), O1 s(d), Si2 p(f) of Zr-SR/BF-4 and O1 s(c)、Si2 p(e) of BF

    图  8  玄武岩纤维热处理力学性能图:温度-断裂强力图(a)、温度-断裂伸长率(b)、时间-断裂强力(c)

    Figure  8.  Mechanical properties of basalt fibre after heat treatment: Temperature-breaking force (a); Temperature-breaking elongations (b); Time-breaking force (c)

    图  9  BF和Zr-SR/BF断裂机制图

    Figure  9.  Fracture mechanism of BF and Zr-SR/BF

    表  1  水溶性锆杂化硅树脂配方

    Table  1.   Formulas of the water-soluble zirconium hybrid silicone resin

    CodeMTES/molKH602/molZrOCl2·8 H2O/molH2O/mLCH3COOH/gHDMS/molSolid Content /wt%
    Zr-SR-1 0.020 0.030 0.0005 2 0.6 0.0025 59.67
    Zr-SR-2 0.020 0.030 0.0010 2 0.6 0.0025 60.97
    Zr-SR-3 0.020 0.030 0.0015 1.75 0.9 0.0025 61.79
    Zr-SR-4 0.020 0.030 0.0020 0.5 1 0.0026 67.36
    Zr-SR-5 0.020 0.030 0.0025 0.7 1.2 0.0026 69.79
    下载: 导出CSV

    表  2  25℃时BF及Zr-SR/BF样品测试液体的性能参数

    Table  2.   Properties of the testing liquids at 25℃ of BF and Zr-SR/BF samples.

    Parameters$ {\gamma _l} $/(mN·m−1)$ {\gamma _l}^p $/(mN·m−1)$ {\gamma _l}^d $/(mN·m−1)
    H2O 72.8 51.0 21.8
    CH2I2 50.8 2.3 48.5
    Notes: $ {\gamma _l} $—Surface energy; $ {\gamma _l}^p $—polar component; $ {\gamma _l}^d $—dispersion component of solution
    下载: 导出CSV

    表  3  BF和Zr-SR/BF样品的接触角及表面能

    Table  3.   The contact angles and the surface energies of BF and Zr-SR/BF samples.


    Sample
    Contact angle/(°)γsp/(mN·m−1)γsd/(mN·m−1)γs/(mN·m−1)
    H2OCH2I2
    BF 119 35.9 9.54 22.85 32.39
    Zr-SR/BF-1 106.7 29.0 0.95 43.94 44.90
    Zr-SR/BF-2 107.8 53.1 0.10 33.80 33.91
    Zr-SR/BF-3 110.2 45.5 0.83 36.25 36.25
    Zr-SR/BF-4 111.7 32.7 1.88 41.17 43.06
    Zr-SR/BF-5 117.9 45.7 2.43 34.27 36.71
    下载: 导出CSV
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  • 收稿日期:  2022-01-25
  • 录用日期:  2022-04-19
  • 修回日期:  2022-04-09
  • 网络出版日期:  2022-05-11

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