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本文观察了分子氮与过量格氏试剂C_2H_5MgBr和二氯钛茂(C_5H_5)_2TiCl_2乙醚悬浮混合物在-80℃、无氧、无水条件下的反应。 由二氯钛茂不同还原价态的紫外可见光谱表明活性物质为(C_5H_5)_2Ti或[(C_5H_5)_2Ti]_2,它和N_2分子生成双核钛络合物[(C_5H_5)_2Ti]_2N_2。结合不同价态钛的顺磁共振谱和在-80℃下反应的顺磁共振谱随时间的变化,提出了固氮反应的机理,并讨论了失活的原因和影响反应进行的因素。
In this paper, we observed the reaction of molecular nitrogen with an excess of Grignard reagent C_2H_5MgBr and dichloro-titanocene (C_5H_5) _2TiCl_2 ether suspension at -80 ℃ under anaerobic and anhydrous conditions. The UV-Vis spectra of different reduction valence states of dichlorotitanium showed that the active material is (C_5H_5) _2Ti or [(C_5H_5) _2Ti] _2, which forms binuclear titanium complex [(C_5H_5) _2Ti] _2N_2 with N_2. Combined with the paramagnetic resonance spectra of titanium with different valences and the paramagnetic resonance spectrum of the reaction at -80 ℃ with time, the mechanism of nitrogen fixation reaction was proposed. The reasons for the deactivation and the factors affecting the reaction were discussed.