固化处理对木材液化物碳纤维原丝的微观构造及热稳定性影响

Effects of curing process on microstructure characterization and thermal stability of liquefied wood carbon fiber precursors

  • 摘要: 以木材液化物和六次甲基四胺为原料, 利用熔融纺丝法制备初始纤维。将初始纤维置于甲醛和盐酸混合液中进行固化处理制成木材液化物碳纤维原丝。考察了固化处理对木材液化物碳纤维原丝的孔隙结构、 晶态结构及热稳定性的影响。结果表明: 初始纤维和原丝的吸附等温曲线属于 Ⅱ 型吸附等温线, 初始纤维和原丝比表面积分别为0.517 m2·g-1和0.142 m2·g-1。杉木木粉中具有典型的纤维素 Ⅰ 晶体衍射峰; 初始纤维和原丝中纤维素 Ⅰ 特征峰消失, 且18.8°附近出现新的衍射峰, 说明形成了新的晶态物质; 原丝中18.8°附近的特征衍射峰增强, 结晶度提高。初始纤维失重率为88.3%, 原丝为60%, 初始纤维到原丝表观活化能由31.31 kJ·mol-1增大到39.18 kJ·mol-1, 原丝热稳定性提高。

     

    Abstract: A new carbon fiber precursors was prepared by liquefied wood in phenol. The liquefied wood was modified to spinning solution by adding hexamethylenetetramine, melt-spinning then cured in combined solution of hydrochloric acid and formaldehyde to obtain precursors. The pore structure, microcrystalline structure and thermal stability of liquefied wood carbon fiber precursors were studied. The results show that the adsorption isotherm of N2 for as-spun fibers and precursors belongs to type Ⅱ , the specific surface area of as-spun fibers is 0.517 m2·g-1, and precursors is 0.142 m2·g-1. Wood powder form Chinese fir has typical diffraction peaks of cellulose Ⅰ . The typical diffraction peaks of cellulose Ⅰ in as-spun fibers and precursors disappear, at the same time a new diffraction peak around 18.8° emerges, suggesting that new crystalline structure of as-spun fibers and precursors has formed. The typical diffraction peaks around 18.8° for precursors polymer strengthen, so crystallinity increases. Interestingly, the mass loss of as-spun fibers is 88.3%, and precursors is 60%, simultaneously the apparent activation energy increases from 31.31 kJ·mol-1 of as-spun fibers to 39.18 kJ·mol-1 of precursors, the thermal stability of precursors improves.

     

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