Heterophase Synthesis of Zirconium Hydroxide from Zirconium Oxychloride

Zhukov, A. V.; Chizhevskaya, S. V.; Phyo, Pyae; Panov, V.A.

doi:10.1134/s0020168519080193

Cited by 5 publications

(3 citation statements)

References 6 publications

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“…Then the NH4OH is used for hydrolysis process of ZOC to produce Zr(OH)4. (Aghazadeh et al, 2012;Mondal & Ram, 2004;Subuki et al, 2020;Zhang & He, 2012;Zhukov et al, 2019). As there are a lot of steps, thus this process takes a lot of processing time.…”

Section: Introductionmentioning

confidence: 99%

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

Muzakky¹,

Poernomo²,

Prabasiwi³

et al. 2023

Physicochem. Probl. Miner. Process.

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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.

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Section: Introductionmentioning

confidence: 99%

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

Muzakky¹,

Poernomo²,

Prabasiwi³

et al. 2023

Physicochem. Probl. Miner. Process.

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“…Precipitation from aqueous solutions of salts is the main method for the synthesis of ZrO 2 , during which nanosized X-ray amorphous hydrous zirconia (ZrO 2 • nH 2 O) is formed. This is an effective method for the preparation of t-ZrO 2 nanocrystallites with a developed mesoporous structure, which is formed during thermal treatment at 350 -450 • C. There are other methods: hydrolysis of aqueous solutions of salts [6][7][8][9], hydrothermal treatment [10], solution combustion [11], thermal decomposition of salts [12], heterophase conversion [13], etc. Matsui et al [6][7][8][9] showed that a sol consisting of m-ZrO 2 nanoparticles (crystallites 2.2 -4.9 nm, agglomerates 100 -200 nm) is formed upon the long-term maintenance of a ZrOCl 2 solution at 100 • C during complete hydrolysis of the salt.…”

Section: Introductionmentioning

confidence: 99%

The effect of hydrolysis duration on the phase composition, texture, aggregation and agglomeration of ZrO2 nanoparticles

Omarov¹

2021

Nanosystems: Phys. Chem. Math.

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In this work, a number of ZrO 2 • nH 2 O and ZrO 2 samples were synthesized by direct precipitation and hydrolysis with different duration (36 and 61 h) followed by neutralization and thermal treatment. The prepared samples were analyzed using DT-TGA, PXRD, N 2 physisorption and LD methods. The dependence of the size of crystallites and secondary particles, phase composition, texture, and particle morphology on the amount of zirconium hydrolyzed to form m-ZrO 2 is shown. The possibility of regulating the phase composition of ZrO 2 has been established while maintaining the specific surface area (110 -120 m 2 /g), as well as creating a hierarchical system of micro-mesopores. The mechanism of the ZrO 2 • nH 2 O formation during hydrolysis and precipitation is considered. The size of the critical nucleus is estimated (1.5 -2 nm).

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“…And in this case, it is necessary to change in a wide range the temperature, pressure, concentration and acidity of the solutions used. Nano-dispersed zirconium dioxide is obtained by its heterophase synthesis from zirconium oxychloride with the participation of solutions of different bases (for example, from the compound ZrOCl 2 •8H 2 O in aqueous solutions of KOH, NaOH or ammonia [5]). So, the methods described above make it possible to obtain nanodispersed zirconium dioxide using aqueous solutions of acids, alkalis and alcohols.…”

mentioning

confidence: 99%

Thermal-Vacuum Method for Obtaining Nanodispersed Zirconium Dioxide

Kutovyi

Malykhin

Virych

et al. 2021

EEJP

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An energy-efficient thermal-vacuum method for continuous production of nanodispersed powder of amorphous zirconium dioxide from zirconium hydroxide has been developed. This approach is based on a principle of creating an aerodynamic flow with an initial powder-like material in the cavity of the heating element of a thermal-vacuum installation. In this way, short-term contacts of particles of zirconium hydroxide with the inner surface of the heating element made in the form of the winding helical are created. As a result, the crushing of the particles is carried out due to the high thermal stresses in the particles contacted. This process is aggravated by the presence of residual moisture in the original powdery material. Transformations of the zirconium hydroxide in the process of thermal-vacuum treatment have been investigated. Amorphous dioxide has been obtained. The study of structural composition of the material in the initial state and processed in a thermal-vacuum installation was carried out using X-ray analysis and scanning microscopy. Experimental data on the structural-phase composition of the original material and data on the closest structural prototypes of crystalline-impurity compounds are presented. They are also given data on the volume of crystal cells and estimates of the molar concentration of the components. A mass spectrometric assessment of the elemental composition of the obtained zirconium dioxide is given. Thermal-vacuum method allows toobtain highly dispersed zirconium dioxide in its amorphous state directly from zirconium hydroxide without using liquid media and, moreover, in a short time – within 15...20 s.

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Heterophase Synthesis of Zirconium Hydroxide from Zirconium Oxychloride

Cited by 5 publications

References 6 publications

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

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

The effect of hydrolysis duration on the phase composition, texture, aggregation and agglomeration of ZrO2 nanoparticles

Thermal-Vacuum Method for Obtaining Nanodispersed Zirconium Dioxide

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