从甲醇溶液中沉淀Ni(II)配合物的阴离子效应和配体偏好:酒石酸盐和吡嗪的例子

Yenni Finisia, Siti Mutrofin, Yuniar Ponco Prananto
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引用次数: 1

摘要

本研究旨在结合吡嗪合成Ni(II)-酒石酸盐-吡嗪金属有机骨架或Ni(II)-T-P MOF作为多孔材料的候选材料。在甲醇溶液中,将Ni(II)溶液、l -酒石酸(T)、吡嗪(P)溶液按不同的摩尔比(Ni(II):T:P = 1:1:0;1:0:2;1:2:2;和1:2:4)使用两种不同的Ni(II)盐(氯化物和硝酸盐)。固体产物通过红外光谱、定性阴离子鉴定、熔点测试和扫描电镜进行了表征。结果表明,镍盐类型对Ni(II)络合物的析出有影响,只有在氯化反应(1:0:2、1:2:2和1:2:4)中才析出淡蓝色固体。1:2:2和1:2:4反应的IR和SEM分析结果与1:0:2反应的结果一致,而定性阴离子鉴定测试结果表明氯离子与Ni(II)不配位。目标Ni(II)-T-P未能成功获得,取而代之的产物是[Ni(pyrazine)x(H2O)(6-x)]Cl2。虽然酒石酸被加倍并首先与Ni(II)反应,吡嗪仍然比酒石酸配体更倾向于与Ni(II)中心配位。
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Anion Effect and Ligand Preference in the Precipitation of Ni(II) Complex from Methanolic Solution: Case of Tartrate vs Pyrazine
This research aims to incorporate pyrazine in the synthesis of Ni(II)-tartrate-pyrazine metal organic frameworks or Ni(II)-T-P MOF as candidate of porous material. Synthesis of the targeted MOF was conducted at room temperature in a methanolic solution by mixing Ni(II) solution, L-tartaric acid (T), and pyrazine (P) solutions sequentially in various molar ratios (Ni(II):T:P = 1:1:0; 1:0:2; 1:2:2; and 1:2:4) using two different Ni(II) salts (chloride and nitrate). Solid products were characterized by infrared spectroscopy, qualitative anion identification test, melting point test, and scanning electron microscopy. The result shows that type of nickel salt affects the precipitation of Ni(II) complex, in which pale blue solids were precipitated out only from the chloride reactions (1:0:2, 1:2:2, and 1:2:4). IR and SEM analyses from the 1:2:2 and 1:2:4 reactions show identical result as also shown by the 1:0:2 reaction, whereas qualitative anion identification test result suggests that the chloride is uncoordinated to the Ni(II). The targeted Ni(II)-T-P is unsuccessfully obtained, instead the product is proposed to be [Ni(pyrazine)x(H2O)(6-x)]Cl2. although the tartaric acid was doubled and firstly reacted with the Ni(II), the pyrazine still has higher preference to coordinate to the Ni(II) center than the tartrate ligand.
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