• Title/Summary/Keyword: Microwave synthesis

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Microwave Synthesis of Hydrotalcite by Urea Hydrolysis

  • Yang, Zhiqiang;Choi, Kwang-Min;Jiang, Nanzhe;Park, Sang-Eon
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.2029-2033
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    • 2007
  • Hydrotalcite, layered double hydroxides (LDH), with hexagonal morphology has been rapidly synthesized by microwave reaction within 1 hour by urea hydrolysis from homogeneous solution. Different synthesis parameters, Mg/Al molar ratio, microwave reaction temperature and microwave power were systematically investigated. Pure hydrotalcite phase was obtained for Mg/Al ratios of 2:1 and 3:1, and higher reaction temperature gave higher crystallinity. The hydrotalcite synthesized at 600W power shows the highest crystallinity and more homogeneous crystal size distribution. The hydrotalcite samples were characterized by powder X-ray diffraction (XRD), simultaneous thermogravimetric/differential thermal analysis (TG/DTA), Fourier Transform Infrared (FT-IR) and Scanning electron micrograph (SEM).

Nanosulfated Silica as a Potential Heterogeneous Catalyst for the Synthesis of Nitrobenzene

  • Khairul Amri;Aan Sabilladin;Remi Ayu Pratika;Ari Sudarmanto;Hilda Ismail;Budhijanto;Mega Fia Lestari;Won-Chun Oh;Karna Wijaya
    • Korean Journal of Materials Research
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    • v.33 no.7
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    • pp.265-272
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    • 2023
  • In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H2SO4/SiO2 as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO2 was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 ℃. SiO2 with a 200-mesh size was impregnated with 98 % H2SO4 by mixing for 1 h. The resulting 33 % (w/w) H2SO4/SiO2 catalyst was separated by centrifugation, dried, and calcined at 600 ℃. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 ℃ for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H2SO4/SiO2 could generate an average benzene conversion of 40.33 %.

Design of broad-band impedance matching networks for hybrid microwave amplifier applications (하이브리드 마이코로파 광대역 증폭기용 임피던스 정합회로 설계)

  • 김남태
    • Journal of the Korean Institute of Telematics and Electronics D
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    • v.35D no.5
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    • pp.11-17
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    • 1998
  • In this paper, the synthesis procedufe of impedance matching network is presented for broad-band microwave amplifier design, whereby amplifier operating in the octave bandwidth is designed and fabricated in detail. The transfer function of the matching netowrks is synthesized by chebyshev approximation and element values for the networks of specified topology are calculatd for various MILs and ripples. After the transistor is modeled by negative-image device model, the synthesis procedure for matching networks is applied to broad-band amplifier design which has electrical performance of about 12dB gain in 4 to 8GHz range. Experimental results obtained from the fabricated amplifier are shown to approach the electrical performance designed in the given frequency range. Construction of the impedance matching networks by transfer function synthesis is very useful method for the design of broad-band microwave amplifiers.

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Solid-state metathetic synthesis of MWO4 (M=Zn, Co) particles assisted by microwave irradiation

  • Lim, Chang-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.6
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    • pp.295-300
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    • 2010
  • Metathetic route for the $MWO_4$ (M=Zn, Co) particles is a simple method of synthesis and a viable alternative method in a short time. $MWO_4$ (M=Zn, Co) particles were synthesized using solid-state metathetic (SSM) method with microwave irradiation. The $MWO_4$ (M=Zn, Co) particles were formed completely at $600^{\circ}C$ for 3 h. The crystallization process, thermal decomposition and morphology of the $MWO_4$(M= Zn, Co) particles were evaluated. The characteristics of the SSM reaction and the formation of a high lattice energy by-product NaCl were discussed.

Microwave-Assisted One-Pot Synthesis of Octahydroquinazolinone Derivatives Catalyzed by Thiamine Hydrochloride Under Solvent-free Condition

  • Badadhe, Pravin V.;Chate, Asha V.;Hingane, Dattatraya G.;Mahajan, Pravin S.;Chavhan, Namdev M.;Gill, Charansingh H.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.936-939
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    • 2011
  • Thiamine hydrochloride (VB1) has been used as an acid catalyst in organic synthesis. One pot three component Biginelli condensation of dimedone, urea/thiourea and substituted aromatic aldehydes catalyzed by 10 mol % of thiamine hydrochloride (VB1) in solvent free condition under microwave irradiation in good to excellent yields has been investigated. Utilization of microwave irradiation, simple reaction conditions, short reaction time, ease of product isolation, and purification makes this manipulation very interesting from an economic and environmental perspective.

Synthesis and characterization of AlN nanopowder by the microwave assisted carbothermal reduction and nitridation (CRN)

  • Chun, Seung-Yeop;Chun, Myoung-Pyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.5
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    • pp.223-228
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    • 2017
  • Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.

Microwave Syntheses of Subphthalocyanine Derivatives and Their Properties (서브프탈로시아닌 유도체의 마이크로파 합성 및 이의 특성)

  • Kim, Jae Hwan;Heo, Jin;Kang, Boo Min;Son, Dae-Hee;Lee, Geun-Dae;Hong, Seong-Soo;Park, Seong-Soo
    • Applied Chemistry for Engineering
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    • v.20 no.2
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    • pp.154-158
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    • 2009
  • Subphthalocyanine (SubPc) derivatives with different kind of substitute groups were synthesized successfully from various precursors using conventional and microwave heating sources. The chemical structure of precursor and product was determined by $^{1}H-NMR$ and FT-IR spectrometer. Also, spectroscopic property was measured by UV-Vis spectrometer. Compared to the conventional synthesis, it was found that SubPc derivatives were synthesized for a shorter reaction time with a higher synthetic yield in the microwave synthesis.

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.3
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

Synthesis of Forsterite with High Q and Near Zero TCf for Microwave/Millimeterwave Dielectrics

  • Ohsato, Hitoshi;Ando, Minato;Tsunooka, Tsutomu
    • Journal of the Korean Ceramic Society
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    • v.44 no.11
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    • pp.597-606
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    • 2007
  • With the advent of ubiquitous age, the high quality dielectric materials have been required for the wireless communications available to the millimeterwave as well as microwave frequencies. The utilizable region for the frequency has been expanding to the millimeter-wave region because of the shortage of radio frequency (RF) resources. These high frequencies would be expected for ultra high speed LAN, ETS and car anti-collision system on the intelligent transport system (ITS) and so on. Silicates are good candidates for microwave/millimeterwave dielectrics, because of their low dielectric constant ${\epsilon}_r$ and high quality factor (High Q). Forsterite ($Mg_2SiO_4$) is one of the silicates with low ${\epsilon}_r$ of 6.8 and Q f of 240000 GHz. In this paper, we reviewed following three categories for synthesis of forsterite: (1) Synthesis of high Q forsterite (2) Adjust the temperature coefficient of resonant frequency $TC_f$ (3) Diffusion of $SiO_{4^-}$ and Mg-ions on the formation of forsterite.