The Phase Morphology of Citrogypsum Waste Controlled by a Hydrothermal Process in Ethylene Glycol/Water Solutions

Abstract

The acid purification of calcium citrate from citric acid production using sulfuric acid as a reagent resulted in citrogypsum waste. The identification of citrogypsum by XRD technique indicates that the main component consists of CaSO4∙2H2O (DH). Furthermore, the comparison of the colours between citrogypsum and natural gypsum are also different. Hence, this research mainly focused on the phase transformation of DH to α-CaSO4 ∙0.5H2O (α-HH) due to high strength and heat resistant. The preparation of α-HH carry out in different volume ratios of ethylene glycol (EG): water solutions at 95oC for 7 hrs under atmospheric pressure. The FT-IR spectra of DH and α-HH results reveal that the absorption frequencies at 1700 and 1800 cm-1 of –OH group are 0.5 and 1.5 water molecule in CaSO4 respectively. TGA thermograms show the theoretical crystal water content of DH approximately 20.1 wt% and the converted α-HH about 4-5 wt%. DSC thermograms of the citrogypsums show two endothermic peaks regarding to two steps of water molecule loss at 151.2oC and 168.5oC respectively. In addition, the α-HH shows exothermic peak at 238.7oC. The morphology of citrogypsum and α-HH are observed by SEM, showing the plate-like shape of citrogypsum and hexagonal shape of α-HH. Moreover, the products could be applied to several other industries for increasing the value and reducing the environmental concerns.