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1 2023

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Shortening synthesis process of zirconium hydroxide as a hydrolysis product of sodium zirconate

Muzakky, Poernomo Herry, Prabasiwi Devi Swasti, Amiliana Rahmatika Alfia

Physicochemical Problems of Mineral Processing

2023

Vol. 59, iss. 3

art. no. 167965

This research was focusing on shortening the process of Zirconium hydroxide (Zr(OH)4) synthesis to get a more efficient process. In the earlier method, Zr(OH)4 was produced through ZOC, which was the product of Na2ZrO3 reacted with HCl. While this study offers a new method to synthesize Zr(OH)4 through the hydrolysis process of sodium zirconate (Na2ZrO3), removing the leaching step of Na2ZrO3 with HCl. The hydrolysis process of Na2ZrO3 was carried out in a multistage stirred reactor at 70°C. The multistage hydrolysis process occurred in 13 stages with 4000 grams of feed and 890 liters of water. This process produced 2500 grams of Zr(OH)4. Then the impurities analysis was done using UV-Vis and atomic absorption spectroscopy (SAA). The UV-Vis analysis was done to analyze Si concentration, while the atomic absorption spectroscopy (SAA) was done to analyze Na concentration. Si and Na concentrations could decrease to 23.98 μg/ml and 1.05 μg/ml, respectively. The Zr(OH)4 contained in the residue was characterized using X-Ray Diffractometer (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). Then, the calcination process of Zr(OH)4 was done at 300°C and 400°C for 1 hour, and characterized using XRD. The XRD result shows crystals of zirconium titanium oxide or srilankite, and SiO2 crystals that are separated from ZrO2 or TiO2 crystals. Surface analysis was done using Scanning Electron Microscope - Energy Dispersive X-Ray (SEM-EDX), the result shows that the hydrolysis process at the 3rd, 7th, and 13th stages have different amorphous crystals with bright colors. At the 13th hydrolysis stage, Zr concentration increased to 63.38%, and Si concentration decreased. Thus, the shorter process of Zr(OH)4 synthesis has been done successfully.