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Noh, Hye Ran,Lee, Dong Woo,Suh, Kyungwon,Lee, Jeongmook,Kim, Tae-Hyeong,Bae, Sang-Eun,Kim, Jong-Yun,Lim, Sang Ho Korean Radioactive Waste Society 2020 방사성폐기물학회지 Vol.18 No.4
An important property of glass and ceramic solid waste forms is processability. Tellurite materials with low melting temperatures and high halite solubilities have potential as solid waste forms. Crystalline TiTe3O8 was synthesized through a solid-state reaction between stoichiometric amounts of TiO2 and TeO2 powder. The resultant TiTe3O8 crystal had a three-dimensional (3D) structure consisting of TiO6 octahedra and asymmetric TeO4 seesaw moiety groups. The melting temperature of the TiTe3O8 powder was 820℃, and the constituent TeO2 began to evaporate selectively from TiTe3O8 above around 840℃. The leaching rate, as determined using the modified American Society of Testing and Materials static leach test method, of Ti in the TiTe3O8 crystal was less than the order of 10-4 g·m-2·d-1 at 90℃ for durations of 14 d over a pH range of 2-12. The chemical durability of the TiTe3O8 crystal, even under highly acidic and alkaline conditions, was comparable to that of other well-known Ti-based solid waste forms.
Hye Ran Noh,Jong-Yun Kim,Tae-Hyeong Kim,Jeongmook Lee,Jung Hwan Park,Sang Ho Lim 한국방사성폐기물학회 2022 한국방사성폐기물학회 학술논문요약집 Vol.20 No.1
Polyoxometalates (POMs) are nanoclusters composed of transition metals with high oxidation states. Owing to their redox properties and structural diversity, POMs have been applied to broad fields, such as catalysis, materials, and medicine. Among various fields of application, POMs play an important role in radiochemistry. POMs can form complexes with tri- and tetravalent lanthanides and actinides (radioactive elements), which may be good sequestrators or agents for separating nuclear wastes. Among the most prominent POM structures, Anderson-type POMs with a general formula of [Hy(XO6)M6O18]n? (y=0–6, n=2–8, M=addenda atom, X=heteroatom) represent one of the basic topological structures of the POM family. An important feature of Anderson type POMs is incorporating a large number of various heteroatoms with different size and oxidation states, which can lead to tune chemical properties. Interestingly, no example of Anderson type POMs with early transition metal ions in the heteroatom site has been reported to date. Herein, we discovered that the Anderson POM Na2K6Ti0.92W6.08O24·12H2O, which consists of pure inorganic framework built from a central Ti core supported by six WO6 inorganic scaffold, and the crystal structure was confirmed and refined using single-crystal X-ray diffraction (SC-XRD). In addition, structural characterizations, including, Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and Inductively coupled plasma-optical emission spectroscopy (ICP-OES) were performed.
Hye Ran Noh,Suk-Bon Yoon,Tae-Hyeong Kim,Dong-Woo Lee,Sang-hun Lee,Jeongmook Lee,Jong-Yun Kim,Sang Ho Lim 한국방사성폐기물학회 2023 한국방사성폐기물학회 학술논문요약집 Vol.21 No.1
In this study, we evaluated the performance of phosphate-functionalized silica in adsorbing uranium and provided insights into optimizing the initial conditions of the uranium solution (concentration and pH), which are often overlooked in uranium adsorption studies. While most studies take into account the effect of pH on both the surface charge of the adsorbents and the dissolved speciation of uranium in solution, they often overlook the formation of solid phases such as β-UO2(OH)2 (cr) and UO3· 2H2O(cr), leading to an overestimation of the adsorption capacity. To address this issue, we considered the speciation of U(VI) calculated using thermodynamic data. Our findings suggest that it is reasonable to evaluate the adsorption performance at pH 4 and concentration below 1.35 mM. The formation of β-UO2(OH)2 (cr) starts at 23 μM (pH 5) and 1 μM (pH 6) and increases sharply with increasing concentration. To avoid interference from the formation of solid phases, experiments should be conducted at lower concentrations, which in turn require very small msorbent/Vsolution ratios. However, controlling small amounts of sorbent can be challenging, and increasing the volume of the solution can generate significant amounts of radioactive waste. We also used UV-vis spectra analysis to investigate the formation of solid phases. We found that a 100 mg L-1 uranium solution resulted in the formation of colloidal particles in the solid phase after 2.5 hours at pH 6, while at pH 4, no significant changes in absorbance were observed over 120 hours, indicating a stable ion phase. Based on these conditions, we obtained an excellent adsorption capacity of 110 mg g-1.
Optimization of Synthetic Conditions for Titanium-containing Anderson-type Polyoxometalate
Hye Ran Noh,Jong-Yun Kim,Tae-Hyeong Kim,Jeongmook Lee,Jung Hwan Park,Sang Ho Lim 한국방사성폐기물학회 2022 한국방사성폐기물학회 학술논문요약집 Vol.20 No.2
Anderson-type polyoxometalate (POM) with general formula of [Hy(XO6)M6O18]n- (y=0-6, n=2-8, M=addenda atom, X=heteroatom) represents one of the basic topological structures among POM-type family. Anderson-type POMs have a planar arrangement and two terminal oxygen atoms attached to each addenda metal atom unlike other type. Thus, the Anderson-type POMs have high reactivity and various coordination modes. The various multifunctional organic-inorganic hybrid materials can be synthesized using the Anderson-type POMs as an inorganic building block. Another important feature of the Anderson-type POMs is the incorporation of the heteroatoms with various sizes and oxidation states, which can lead to tune chemical properties. No Anderson-type POMs with early transition metal ions in the heteroatom site have been reported previously. Recently, we reported the synthesis of titanium-containing Anderson-type POM, Na2K6Ti0.92W6.08O24?12H2O (Ti-POM), which consists of pure inorganic framework built from a central Ti atom surrounded by six WO6 inorganic scaffold. Herein, in-depth studies were conducted to find optimal synthesis conditions such as composition and pH. The success of synthesis was confirmed with Powder X-ray Diffraction that the Ti-POM has a rhombohedral structure with space group of R-3m (No. 166) when the TiOSO4·xH2SO4?yH2O/ Na2WO4?2H2O molar ratio is in the range of 0.07 to 0.33. But outside of this range, other unwanted phases coexist. In a basic condition (pH=12), a single-phase Ti-POM with good crystallinity can be obtained, while a Keggin-type POM, NaxK10-x(H2W12O42), was formed through the decomposition of Ti-POM at pH lower than 7.
Hye Ran Noh,Suk-Bon Yoon,Tae-Hyeong Kim,Dong-Woo Lee,Jeongmook Lee,Sang Ho Lim,Jong-Yun Kim 한국방사성폐기물학회 2023 한국방사성폐기물학회 학술논문요약집 Vol.21 No.2
Bis (2-ethylhexyl)phosphoric acid (HDEHP) is a renowned extractant, favored for its affinity to selectively remove uranium via its P=O groups. We previously synthesized HDEHP-functionalized mesoporous silica microspheres for solid-phase uranium adsorption. Herein, we investigated the kinetic and isothermal behavior of uranyl ion adsorption in mesoporous silica microspheres functionalized with phosphate groups. Adsorption experiments were conducted by equilibrating 20 mg of silica samples with 50 mL of uranium solutions, with concentrations ranging from 10 to 100 mgU L?1 for isotherms and 100 mgU L?1 for kinetics. Three distinct samples were prepared with varying HDEHP to TEOS molar ratios (x = 0.16 and 0.24) and underwent hydrothermal treatment at different temperatures, resulting in distinct textural properties. Contact times spanned from 1 to 120 hours. For x = 0.16 samples, it took around 50 and 11 hours to reach equilibrium for the hydrothermally treated samples at 343 K and 373 K, respectively. Adsorbed quantities were similar (99 and 101 mg g-1, respectively), indicating consistent functional group content. This suggests that the key factor influencing uranium adsorption kinetics is pore size of the silica. The sample treated at 373 K, with a larger pore size (22.7 nm) compared to 343 K (11.5 nm), experienced less steric hindrance, allowing uranium species to diffuse more easily through the mesopores. The data confirmed the excellent fit of pseudo-second-order kinetic model (R2 > 0.999) and closely matched the experimental value, suggesting that chemisorption governs the rate-controlling step. To gain further insights into uranium adsorption behavior, we conducted an adsorption isotherm analysis at various initial concentrations under a constant pH of 4. Both the Langmuir and Freundlich isotherm models were applied, with the Langmuir model providing a superior fit. The relatively high R2 value indicated its effectiveness in describing the adsorption process, suggesting homogenous sorbate adsorption on an energetically uniform adsorbent surface via a monolayer adsorption and constant adsorption site density, without any interaction between adsorbates on adjacent sites. Remarkably, differences in surface area did not significantly impact uranium removal efficiency. This observation strongly suggests that the adsorption capacity is primarily governed by the loading amount of HDEHP and the inner-sphere complexation with the phosphoryl group (O=P). Our silica composite exhibited an impressive adsorption capacity of 133 mg g-1, surpassing the results reported in the majority of other silica literature.