Metall. Res. Technol.
Volume 114, Number 5, 2017
|Number of page(s)||7|
|Published online||28 August 2017|
Crystalline-selected synthesis of ferrous oxalate dihydrate from spent pickle liquor
Yunnan Provincial Laboratory for Advanced Materials and Batteries Application, Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology,
Yunnan, PR China
2 Research & Development Center, China Tobacco Yunnan Industrial Co. Ltd, 650093 Kunming, PR China
3 State Key Laboratory of Physical Chemistry of Solid Surfaces, Collaborative Innovation Center of Chemistry for Energy Materials, College of Chemistry and Chemical Engineering, Xiamen University, 361005 Xiamen, PR China
4 Yunnan Provincial Energy Investment Group Co. Ltd, 650000 Kunming, PR China
Received in final form: 2 June 2017
Accepted: 8 June 2017
Ferrous oxalate dihydrate with different crystalline structures, polymorphs and sizes have been synthesized through a facile precipitation reaction from spent pickling liquors (SPL) by controlling synthesis conditions. The β-FeC2O4 · 2H2O in orthorhombic phase can be formed at room temperature, whereas α-FeC2O4 · 2H2O with a monoclinic unit cell can be obtained after aging at 80 °C. With the increasing aging temperature, the morphology of samples can be tailored from flower-like to prismatic-like and the particle-sizes are decreased. Innovatively, thermal decomposition behaviors of products have been investigated in details by X-ray diffraction pattern (XRD) and thermal gravimetric-differential scanning calorimetry (TG-DSC). The results show that both FeC2O4 · 2H2O samples can be transformed to α-Fe2O3 in air atmosphere and Fe3O4 in argon atmosphere at T ≧ 400 °C. In air atmosphere, there are two sharp exothermic peaks for β-FeC2O4 · 2H2O (250 °C) and α-FeC2O4 · 2H2O (239.5 °C) correspond to the decomposition reactions. In argon atmosphere, the decomposition end temperatures are 500 °C and 430 °C for β-FeC2O4 · 2H2O and α-FeC2O4 · 2H2O, respectively. This indicates that β-FeC2O4 · 2H2O has higher thermal stability in comparison with α-FeC2O4 · 2H2O.
Key words: resource utilize / spent pickling liquors / ferrous oxalate dihydrate / crystalline control
© EDP Sciences, 2017
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