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作 者:何伟春[1] 王建明[1] 周利[2] 陈权启[1] 沈报春[1] 张鉴清[1]
机构地区:[1]浙江大学化学系 [2]枣庄学院化学化工系,枣庄277160
出 处:《化学学报》2007年第20期2261-2265,共5页Acta Chimica Sinica
基 金:国家自然科学基金(No.50172041)资助项目.
摘 要:首次提出了一种在浓的NaOH溶液中电合成0.83mol·L-1Na2FeO4溶液进而高纯度合成固态K3Na(FeO4)2的方法.研究了合成条件,并利用多种实验技术研究了该固态样品的性质.实验表明,K3Na(FeO4)2晶体在混合的NaOH-KOH溶液中,其溶解-沉淀平衡曲线符合经验方程式:[Na+][K+]3[FeO24-]2.8=1.4×10-4([K+]≤1.01mol·L-1);在浓的KOH溶液中其溶解度与K2FeO4几乎一致.和K2FeO4晶体不同,所得K3Na(FeO4)2晶体显示3个红外特征峰(787,801~802和858~862cm-1)并具有P■m1(164)空间群的六方晶胞,其粉末在Ar气中直到197℃才分解,热稳定性低于K2FeO4.An electrosynthesis in concentrated NaOH electrolyte is first presented for the synthesis of 0.83 mol·L^- 1 Na2FeO4 solution, and then for the synthesis of solid K3Na(FeO4)2 with high purity and yield. The synthesis conditions have been explored. Many experiment techniques have been used to characterize the obtained solid sample. The experiment results showed that in the mixed NaOH-KOH solutions, the dissolution-precipitation curve of K3Na(FeO4)2 conformed to the empirical foumula of [Na+][K+]^3× [FeO4^2-]2.8= 1.4× 10^-4 ([K^+]≤1.01 mol·L^-1). The measured solubility of K3Na(FeO4)2 in concentrated KOH electrolytes was almost the same as that of K2FeO4. Different from K2FeO4 crystals, the synthesized K3Na(FeO4)2 powders exhibited three characteristic IR absorption peaks (787, 801~802 and 858~862 cm-1) and a hexagonal unit cell with the space group P3 ml (164), The results of TG/DSC experiments showed that the K3Na(FeO4)2 powders would not decompose until 197 ℃in the atmosphere of Ar, but were less stable than K2FeO4.
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