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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, 2023, 40(2): 814-824. doi: 10.13801/j.cnki.fhclxb.20220426.001
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, 2023, 40(2): 814-824. doi: 10.13801/j.cnki.fhclxb.20220426.001
CHENG Yan, WANG Zhaotian, LUO Hongjie, et al. Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre[J]. Acta Materiae Compositae Sinica, 2023, 40(2): 814-824. doi: 10.13801/j.cnki.fhclxb.20220426.001
Citation: CHENG Yan, WANG Zhaotian, LUO Hongjie, et al. Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre[J]. Acta Materiae Compositae Sinica, 2023, 40(2): 814-824. doi: 10.13801/j.cnki.fhclxb.20220426.001

水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能

doi: 10.13801/j.cnki.fhclxb.20220426.001
基金项目: 国家自然科学基金(51874093)
详细信息
    通讯作者:

    罗洪杰,博士,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: TQ343

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

Funds: National Natural Science Foundation of China (51874093)
  • 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,本文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323~360℃;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376.0 N,断裂伸长率为2.647%,优于未被浸润纤维(287.8 N、1.932%)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  Zr-SR的合成图

    Figure  1.  Synthesis scheme of Zr-SR

    图  2  Zr-SR的FTIR图谱

    Figure  2.  FTIR spectra of 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  4  25℃、300℃、400℃时BF和Zr-SR/BF的SEM图像

    (a) BF; ((b)-(f)) Zr-SR/BF-1, Zr-SR/BF-2, Zr-SR/BF-3, Zr-SR/BF-4, Zr-SR/BF-5; (g) 300℃ Zr-SR/BF-5; (h) 400℃ Zr-SR/BF-5

    Figure  4.  SEM images of BF and Zr-SR/BF at 25℃, 300℃, 400℃

    图  5  BF和Zr-SR/BF的AFM图像

    Figure  5.  AFM morphologies of BF and Zr-SR/BF

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

    图  6  BF和Zr-SR/BF的表面积值及表面粗糙度值

    Ra—Arithmetic average roughness; Rq—Root mean square roughness

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

    图  7  (a) BF和Zr-SR/BF-4的XPS全谱图;Zr-SR/BF-4的Zr3d (b)、O1s (d) 和Si2p (f);BF的O1s (c)、Si2p (e) XPS分谱图谱

    Figure  7.  (a) XPS spectra of BF and Zr-SR/BF-4; XPS patterns of Zr3d (b), O1s (d), Si2p (f) of Zr-SR/BF-4 and O1s (c), Si2p (e) of BF

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

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

    图  9  BF和Zr-SR/BF断裂机制

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

    表  1  水溶性锆杂化硅树脂(Zr-SR)配方及浸润后玄武岩纤维(BF)的对应样品编号

    Table  1.   Formulas of the water-soluble zirconium hybrid silicone resin (Zr-SR) and the corresponding sample numbers of sized basalt fibres (BF)

    CodeMTES/molKH602/molZrOCl2·8H2O/molH2O/mLCH3COOH/gHDMS/molSolid content/wt%Sample numbers of sized BF
    Zr-SR-1 0.020 0.030 0.0005 2.00 0.6 0.0025 59.67 Zr-SR/BF-1
    Zr-SR-2 0.020 0.030 0.0010 2.00 0.6 0.0025 60.97 Zr-SR/BF-2
    Zr-SR-3 0.020 0.030 0.0015 1.75 0.9 0.0025 61.79 Zr-SR/BF-3
    Zr-SR-4 0.020 0.030 0.0020 0.50 1.0 0.0026 67.36 Zr-SR/BF-4
    Zr-SR-5 0.020 0.030 0.0025 0.70 1.2 0.0026 69.79 Zr-SR/BF-5
    Notes: MTES—Methyltriethoxysilane; KH602—N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane; HDMS—Hexamethyldisiloxane.
    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 andZr-SR/BF samples

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

    表  3  BF和Zr-SR/BF样品的接触角θ及表面能

    Table  3.   Contact angles θ and surface energies of BF and Zr-SR/BF samples


    Sample
    θ/(°)$\gamma _{\rm{s}}^{\rm{p}} $/(mN·m−1)$\gamma _{\rm{s}}^{\rm{d}} $/(mN·m−1)γs/(mN·m−1)
    H2OCH2I2
    BF 119.0 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
    Notes: γs—Surface energy of solid; $\gamma _{\rm{s}}^{\rm{p}} $—Polar component of solid; $\gamma _{\rm{s}}^{\rm{d}} $—Dispersion component of solid.
    下载: 导出CSV
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  • 收稿日期:  2022-01-25
  • 修回日期:  2022-04-09
  • 录用日期:  2022-04-19
  • 网络出版日期:  2022-04-26
  • 刊出日期:  2023-02-15

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