Separation Behavior of Various Metal Chelates by the Vacuum Sublimation Method = 진공승화법에 의한 금속킬레이트의 분리거동

국문 초록 (Abstract)

진공승화법의 주류를 이루는 온도구배로를 이용하여 승화성금속킬레이트화합물을 진공승화 시킬 때 분리거동을 연구하기 위하여 아세틸아세톤의 금속킬레이트화합물인 Be(Ⅱ), Mg(Ⅱ), Cu(Ⅱ), Ni(Ⅱ), Zn(Ⅱ), Co(Ⅱ), Co(Ⅲ), Fe(Ⅲ), Al(Ⅲ)등 9종의 금속아세틸아세토네이트의 정확한 진공응축점(VCP)을 측정하였다.
측정된 VCP 값의 순서는 MgA₂>CoA₃>NiA₂>CuA₂>FeA₃>AlA₃=CoA₂>ZnA₂>BeA₂로서의 이 순서는 승화성의 난이 판정에 지침이 될 수 있었다.
이들 금속킬레이트 화합물들의 VCP 값의 차이를 이용하여 2성분 및 3성분 혼합물을 분별승화시켜 그 분리거동을 검토하였다.

다국어 초록 (Multilingual Abstract)

Among the metalacetylacetonates, there are many which are both sublimable and stable with respect to heat. For this reason, an investigation was made of the separation of these compounds by sublimatography. First, the VCP's of 9 metal chelates of acetylacetone were measured. Next two and three component mixtures were made from among these compounds, and the separability of these mixtures investigated.
Among the two-component mixtures, a mixture of [Cu(acac)₂] and [Be(acac)₂] was perfectly separated. However, a similar mixture of [Cu(acac)₂]and [Zn(acac)₂] could not be separated. Among the three-component mixtures used, the mixture of [Mg(acac)₂], [Al(acac)₃] and [Be(acac)₂] was perfectly separated. However, a similar mixture of [Ni(acac)₂] [Fe(acac)₃] and [Be(acac)₂] could not be separated. These results were in good agreement with expectations based on the values of the VCP's of the components of the mixtures.
A mixture of [Co(acac)₂] and [Co(acac)₃] was used as an example of a separation of two different complexes of the same metal. This same experiment was performed using commercial [Co(acac)₃] in a attempt to further purify it. In a simply one step operation, the [Co(acac)₂], which was present as an impurity to the extent of about 1% was completely removed.