Precipitation study of CO2-loaded glycinate solution with the introduction of ethanol as an antisolvent
Siming Chen , Yue Wu , Geoffrey W. Stevens , Guoping Hu , Wenshou Sun , Kathryn A. Mumford
Front. Chem. Sci. Eng. ›› 2020, Vol. 14 ›› Issue (3) : 415 -424.
Focused beam reflectance measurement (FBRM) and 13C nuclear magnetic resonance (13C NMR) analysis were used to study the precipitation process of CO2-loaded potassium glycinate (KGLY) solutions at different CO2 loadings, during the addition of ethanol as an antisolvent at a rate of 10 mL·min−1. The volume ratio of ethanol added to the KGLY solution (3.0 mol·L−1, 340 mL) ranged from 0 to 3.0. Three solid-liquid-liquid phases were formed during the precipitation process. The FBRM results showed that the number of particles formed increased with CO2 loading and ethanol addition for CO2-unsaturated KGLY solutions, whilst for CO2-saturated KGLY solution it first increased then decreased to a stable value with ethanol addition. 13C NMR spectroscopic analysis showed that the crystals precipitated from the CO2-unsaturated KGLY solutions consisted of glycine only, and the quantity crystallised increased with CO2 loading and ethanol addition. However, a complex mixture containing glycine, carbamate and potassium bicarbonate was precipitated from CO2-saturated KGLY solution with the maximum precipitation percentages of 94.3%, 31.4% and 89.6%, respectively, at the ethanol volume fractions of 1.6, 2.5 and 2.3.
crystallization / precipitation / glycinate / FBRM / 13C NMR
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Higher Education Press
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