Page 130 - 《精细化工》2020年第1期

·116· 精细化工 FINE CHEMICALS
a—SS; b—OS max
图 4 OS max 与 SS 的 FTIR 谱图
Fig. 4 FTIR spectra of OS max and SS
–1
由图 4 可知，SS 在 3318 cm 处有强烈的羟基
v(—OH)吸收峰，而 OS 在此处的吸收峰明显减弱，表
示 SS 中的羟基 v(—OH)大幅减少 [16] 。在 1734 cm 处
OS 出现峰，该峰为醛基 v(C==O)的吸收峰，而 SS 在此
处未出现峰，表明 OS max 中出现了醛基(C==O)
–1
且在 3550 cm 处出现羧基吸收峰，这与实验测得结果
吻合，证明 SS 的羟基(—OH)被电氧化成醛基(C==O) 。
根据 SS 电解过程的氧化方程式（见 1.2.1 节），
羟基(—OH)被氧化成醛基(C==O)官能团，使分子之
间氢键被破坏，从而使 OS max 的结晶度改变
5 为糊化 OS 与糊化未氧化 SS 的 XRD 谱图。
由图 5 可知，尽管 OS max 氧化后含有微量醛基
及羧基，但其在 2θ=21°处的峰接近消失。而 SS 在
[19]
2θ=16°、18°、21°和 23°位置衍射峰明显
SS 在电解氧化之后结晶度降低。
a—SS; b—OS max
图 5 OS max 与 SS 的 XRD 谱图
Fig. 5 XRD patterns of OS max and SS
3 结论
（1）采用电化学分析系统结合单电流阶跃法制
备 OS，得到最佳条件为：电流密度 20 mA/cm ，SS
质量分数 10%，NaCl 质量分数为 2%，电解时间为
20 min，在此条件下测得醛基质量分数为 0.432%。
（2）对 SS 与 OS max 进行 FTIR 及 XRD 对比分
第 37 卷
析，FTIR 显示 OS max 中出现醛基和羧基吸收峰，XRD
显示 OS max 结晶度降低。表明该电氧化方法效果明显。
（3）采用单电流阶跃法可以直观地根据电势变
化来确定氧化时间，以获得实验系统最高醛基质量
分数，这是一种很直观、方便的电解方法。可以为
电氧化提供参考。
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