• Title/Summary/Keyword: Solvothermal method

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Sonochemical Synthesis of UiO-66 for CO2 Adsorption and Xylene Isomer Separation (초음파 합성법을 이용한 UiO-66의 합성 및 이산화탄소 흡착/자일렌 이성체 분리 연구)

  • Kim, Hee-Young;Kim, Se-Na;Kim, Jun;Ahn, Wha-Seung
    • Korean Chemical Engineering Research
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    • v.51 no.4
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    • pp.470-475
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    • 2013
  • Zr-benzendicarboxylate structure, UiO-66 was prepared in 1-L batch scale by using a unique sonochemical-solvothermal combined synthesis method. The produced UiO-66 showed uniform particles of ca. $0.2{\mu}m$ in size with the BET surface area of $1,375m^2/g$ in high product yield (>95%). The UiO-66 showed 198 and 84 mg/g $CO_2$ adsorption capacity at 273 K and 298 K, respectively, with excellent $CO_2$ selectivity ($CO_2:N_2=32:1$) at ambient conditions. The isosteric heat of $CO_2$ adsorption varied from 33 to 25 kJ/mol as the adsorption progressed. The UiO-66 tested for xylene isomer separation in a liquid-phase batch mode confirmed preferential adsorption of the adsorbent for o-xylene over m-, and p-xylene.

Adsorption and Photocatalytic Degradation of Dyes Using Synthesized Metal-Organic Framework NH2-MIL-101(Fe) (합성 금속-유기 골격체 NH2-MIL-101(Fe)를 이용한 염료의 흡착 및 광분해 제거)

  • Lee, Joon Yeob;Choi, Jeong-Hak
    • Journal of Environmental Science International
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    • v.27 no.7
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    • pp.611-620
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    • 2018
  • In this study, a metal-organic framework (MOF) material $NH_2$-MIL-101(Fe) was synthesized using the solvothermal method, and characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), UV-visible spectrophotometry, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), and surface area measurements. The XRD pattern of the synthesized $NH_2$-MIL-101(Fe) was similar to the previously reported patterns of MIL-101 type materials, which indicated the successful synthesis of $NH_2$-MIL-101(Fe). The FT-IR spectrum showed the molecular structure and functional groups of the synthesized $NH_2$-MIL-101(Fe). The UV-visible absorbance spectrum indicated that the synthesized material could be activated as a photocatalyst under visible light irradiation. FE-SEM and TEM images showed the formation of hexagonal microspindle structures in the synthesized $NH_2$-MIL-101(Fe). Furthermore, the EDS spectrum indicated that the synthesized material consisted of Fe, N, O, and C elements. The synthesized $NH_2$-MIL-101(Fe) was then employed as an adsorbent and photocatalyst for the removal of Indigo carmine and Rhodamine B from aqueous solutions. The initial 30 min of adsorption for Indigo carmine and Rhodamine B without light irradiation achieved removal efficiencies of 83.6% and 70.7%, respectively. The removal efficiencies thereafter gradually increased with visible light irradiation for 180 min, and the overall removal efficiencies for Indigo carmine and Rhodamine B were 94.2% and 83.5%, respectively. These results indicate that the synthesized MOF material can be effectively applied as an adsorbent and photocatalyst for the removal of dyes.

Preparation and Characterization of Carbon Nanofiber from Liquid Phase Carbon Source (액상법에 의한 Carbon Nanofiber 제조 및 특성 분석)

  • Lee, Won-Woo;Shin, Chae-Ho;Park, Han-Sung;Choi, Young-Min;Ryu, Beyong-Hwan
    • Korean Journal of Materials Research
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    • v.18 no.10
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    • pp.564-570
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    • 2008
  • Nanostructured carbon materials have been found to have applications in fuel cell electrodes, field emitters, electronic devices, sensors and electromagnetic absorbers, etc. Especially, the CNF (carbon nanofiber) can be expected to play an important role in catalyst supporters for fuel cell electrodes and chemical reactions. In this study, we synthesized CNF from a liquid phase carbon source by a solvothermal method. In addition, we studied the parameters for the preparation of CNF by controlling heating and cooling rates, synthesis temperature and time. We characterized the CNF by SEM/TEM, XRD, Raman spectroscopy and EDS. We found that the heating and cooling rate have strong effects on the CNF formation and growth. We were able to prepare the best CNF at the heating rate of $10^{\circ}$/min, at $450^{\circ}$ for 60 minutes, and at the cooling rate of $4^{\circ}$/min. As a result of Raman spectra, we found that the sample showed two characteristic Raman bands at ${\sim}1350cm^{-1}$ (D band) and ${\sim}1600cm^{-1}$ (G band). The G band indicates the original graphite feature, but the D band has been explained as a disorder feature of the carbon structure. The diameter and length of the CNF was about $15{\sim}20nm$, and over $1{\mu}$, respectively.

Electrocatalytic properties of Te incorporated Ni(OH)2 microcrystals grown on Ni foam

  • Lee, Jung-Il;Oh, Seong Gyun;Kim, Yun Jeong;Park, Seong Ju;Sin, Gyoung Seon;Kim, Ji Hyeon;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.2
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    • pp.96-101
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    • 2021
  • Developing effective and earth-abundant electrocatalyst for oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) is critical for the commercialization of a water splitting system. In particular, the overpotential of the OER is relatively higher than the HER, and thus, it is considered that one of the important methods to enhance the performance of the electrocatalyst is to reduce the overpotential of the OER. We report effects of incorporation of metalloid into Ni(OH)2 microcrystal on electrocatalytic activities. In this study, Te incorporated Ni(OH)2 (��Te-Ni(OH)2) were grown on three-dimensional porous NF by a facile solvothermal method with �� = 1, 3 and 5. Homogeneous microplate structure on the NF was clearly observed for the Ni(OH)2/NF and ��Te-Ni(OH)2/NF samples. However, irregular and collapsed nanostructures were found on the surface of nickel foam when Te precursor ratio is (��) over 3. Electrocatalytic OER properties were analysed by Linear sweep voltammetry (LSV) and Electrochemical impedance spectroscopy (EIS). The amount of Te incorporation used in the electrocatalytic reaction was found to play a crucial role in improving catalytic activity. The optimum Te amount (��) introduced into the Ni(OH)2/NF was discussed with respect to their OER performance.

Electrochemical Synthesis of Metal-organic Framework (전기화학적 방법을 통한 금속 유기 골격체 합성)

  • Moon, Sanghyeon;Kim, Jiyoung;Choi, Hyun-Kuk;Kim, Moon-Gab;Lee, Young-Sei;Lee, Kiyoung
    • Applied Chemistry for Engineering
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    • v.32 no.3
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    • pp.229-236
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    • 2021
  • During the last two decades, metal-organic frameworks (MOFs) have been drawn attention due to their high specific surface area, porosity, and catalytic activities that allow to use in many applications such as sensor, catalysis, energy storage, etc. To synthesize MOFs hydrothermal or solvothermal method were generally used. However, these methods require high-cost equipment and long time-spend for the synthesis with multi-step process. In contrast, electrochemical synthesis has been considered as a simple and easy process under the ambient conditions. In this review, we described the mechanism of electrochemical MOFs synthesis by the number of configured electrodes system, with the recent reports of various applications.

One-pot synthesis of silica-gel-based adsorbent with Schiff base group for the recovery of palladium ions from simulated high-level liquid waste

  • Wu, Hao;Kim, Seong-Yun;Ito, Tatsuya;Miwa, Misako;Matsuyama, Shigeo
    • Nuclear Engineering and Technology
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    • v.54 no.10
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    • pp.3641-3649
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    • 2022
  • A simple solvothermal reaction was used to prepare a 3-aminopropyl-functionalized silica-gel-based adsorbent for adsorbing Pd(II) from the nitric acid solution. Scanning electron microscopy, fourier transform infrared spectroscopy, and thermogravimetry analysis were performed on the as-synthesized adsorbent to demonstrate the successful introduction of Schiff base groups. Batch experiments were used to investigate the effects of contact time, nitric acid concentration, solution temperature, and adsorption capacity. It is worth noting that the prepared adsorbent exhibited a higher affinity toward Pd(II) with the uptake approximately 100% even in a 2 M HNO3 solution. At an equilibrium time of 5 h, the maximum adsorption capacity of Pd(II) was estimated to be 0.452 mmol/g. The adsorbed Pd(II) could be completely eluted by dissolving 0.2 M thiourea solution in 0.1 M HNO3. Using a combination of particle-induced X-ray emission analysis and an X-ray photoelectron spectrometer, the adsorbed Pd was found to be uniformly distributed on the surface of the prepared adsorbent and the existing species were Pd(II) and zero-valent Pd(0). Due to the desirable performances, facile preparation method, and abundant raw material source, the prepared adsorbent demonstrated a high application potential in the recovery of Pd(II) from simulated high-level liquid waste treatment.

Highly catalysis Zinc MOF-loaded nanogold coupled with aptamer to assay trace carbendazim by SERS

  • Jinling Shi;Jingjing Li;Aihui Liang;Zhiliang Jiang
    • Advances in nano research
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    • v.14 no.4
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    • pp.313-327
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    • 2023
  • Zinc metal organic framework (MOFZn)-loaded goad nanoparticles (AuNPs) sol (Au@MOFZn), which was characterized by TEM, Mapping, FTIR, XRD, and molecular spectrum, was prepared conveniently by solvothermal method. The results indicated that Au@MOFZn had a very strong catalytic effect with the nanoreaction of AuNPs formation between sodium oxalate (SO) and HAuCl4. AuNPs in the new indicator reaction had a strong resonance Rayleigh scattering (RRS) signal at 370 nm. The indicator AuNPs generated by this reaction, which had the most intense surface enhanced Raman scattering (SERS) peak at 1621 cm -1. The new SERS/RRS indicator reaction in combination with specific aptamer (Apt) to fabricate a sensitive and selective Au@MOFZn catalytic amplification-aptamer SERS/RRS assay platform for carbendazim (CBZ), with SERS/RRS linear range of 0.025-0.5 ng/mL. The detection limit was 0.02 ng/mL. Similarly, this assay platform has been also utilized to detect oxytetracycline (OTC) and profenofos (PF).