三草酸合铁(Ⅲ)酸钾合成工艺的优化

以硫酸亚铁铵、草酸为主要原料,双氧水为氧化剂合成三草酸合铁(Ⅲ)酸钾。采用响应面法优化三草酸合铁(Ⅲ)酸钾的制备工艺,用XRD、FT-IR、SEM对产物进行表征。结果表明,产物化学式为K[Fe(C_2O_4)_3]·3H_2O,形貌为微米块状颗粒。优化工艺条件:草酸亚铁制备中草酸用量为28.00 m L、反应时间为18.00 min;氧化配位反应中草酸钾用量为17.00 m L、H_2O_2用量为6.00 m L,清除H_2O_2时间为5.00 min;酸溶配位中草酸用量为11.00 m L,在该条件下重复实验,产品均为翠绿色晶体,产率均在89.89%~90.57%之间。

Improvement for the Preparation Technology of Potassium Trioxalatoferrate

Potassium trioxalato ferrate was synthesized by using ammonium ferrous sulfate and oxalic acid as materials,and hydrogen peroxide as the oxidant.The experimental conditions have been optimized by response surface method.The obtained products were confirmed by XRD,SEM,IR and chemical analysis.The results showed that the structure product is K[Fe(C2O4)3]· 3H2O and a micron particle with morphology bulk shape.The improved conditions are oxalic acid dosage is 28.00 mL,the reaction time of 18.00 min during the preparation of ferrous oxalate.Potassium oxalate,H2O2 dosageare17.00 mL,6.00 mL respectively,removal of H2O2 time is 5.00 min during the oxidation of coordination reaction.Oxalic acid dosage is 11.00 mL in acid soluble ligand process.The products are green crystals.The yield are between 89.89％ ～ 90.57％ under the repeated experiment of improved condition.