• Title/Summary/Keyword: Catalyst-free

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A Green and Highly Efficient Solvent-free Synthesis of Novel Calicx[4]resorcinarene Derivatives Using Tungstate Sulfuric Acid

  • Karami, Bahador;Khodabakhshi, Saeed;Safikhani, Niloofar;Arami, Afsaneh
    • Bulletin of the Korean Chemical Society
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    • v.33 no.1
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    • pp.123-127
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    • 2012
  • A facile and simple procedure for the synthesis of novel and known calix[4]resorcinarene derivatives were developed via a reaction of arylaldehydes with resorcinol in the presence of catalytic amounts of tungstate sulfuric acid (TSA) under solvent-free conditions. This eco-friendly method has many appealing attributes, such as excellent yields, short reactions times, use of safe and recoverable catalyst, and simple work-up procedures. TSA was characterized by powdered X-ray diffraction (XRD), X-ray fluorescence (XRF) and FTIR spectroscopy.

Rapid and Ecofriendly Esterification of Alcohols with 2-Acylpyridazinones

  • Kim, Bo Ram;Sung, Gi Hyeon;Ryu, Ki Eun;Kim, Jeum-Jong;Yoon, Yong-Jin
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3410-3414
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    • 2013
  • Atom-economical esterification is of great importance in green chemistry. In this work, we demonstrated the catalyst and additive free esterification of alcohols by their reaction with 2-acyl-4,5-dichloropyridazin-3(2H)-ones without solvent at $100^{\circ}C$. Aliphatic and aromatic alcohols were converted into the corresponding esters in good to excellent yields. It is noteworthy that the reaction is solvent-free, atom-economic, easy-workup, and rapid and that the process is inexpensive.

Ultrasound Mediated, Sodium Bisulfite Catalyzed, Solvent Free Synthesis of 6-Amino-3-methyl-4-substitued-2,4-dihydropyrano[2,3-c]pyrazole-5-carbonitrile

  • Darandale, Sunil N.;Sangshetti, Jaiprakash N.;Shinde, Devanand B.
    • Journal of the Korean Chemical Society
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    • v.56 no.3
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    • pp.328-333
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    • 2012
  • A simple, convenient and practical green synthetic protocol for sodium bisulfite catalyzed multicomponent reaction of ethyl acetoacetate, hydrazine hydrate, malononitrile, and various aldehydes for the synthesis of 6-amino-4-phenyl-3-methyl-2,4-ihydropyrano[2,3-c]pyrazole-5-carbonitriles using ultrasound irradiations in solvent free condition. This method provides the advantage of operational simplicity, shorter reaction time and excellent yields making the protocol environment friendly and economically lucrative.

Optimum Synthesis and Characterization of Precursor Solution for a Hard Coating Silica Film Prepared by Sol-Gel Process

  • Kim, Seon Il;Kim, Gu Yeol;Im, Hyeong Mi;Lee, Bong U;Na, Jae Un
    • Bulletin of the Korean Chemical Society
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    • v.21 no.8
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    • pp.817-822
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    • 2000
  • Crack-free hard coating siIica films were prepared by sol-gel processfrom twokinds of silicon alkoxide (tetra-ethoxysilane and methyltrimethoxysilane) and two kinds of alcohol (methanol and isopropyl alcohol) with an acid catalyst,acetic acid. A silicate framework of the precursor solution was investigated by infrared spectros-copy (IR) in the process of hydrolysis and condensation. Theextent of the condensation in the intermediates was elucidated by gel permeation chromatography (GPC) and 29Si-NMR spectroscopy. The hard coating films werecharacterized by IR,scanning electron microscope (SEM), thermo gravimetric analyzer (TGA) and dif-ferential scanning calroimeter (DSC). The synthetic condition for the crack-free and transparent silica film for-mation was optimized interms of starting materials for the precursor solution as well as preparation method of the silica film.

Study on Reesterification of Rice Bran Oil Containing High Free Fatty Acids and Glycerol (유리지방산을 많이 함유한 미강유와 글리세린의 에스테르화 반응에 관한 연구)

  • Moon, Sung-Hoon;Rhee, Joon-Shick
    • Korean Journal of Food Science and Technology
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    • v.12 no.3
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    • pp.193-199
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    • 1980
  • A series of tests were conducted on the reesterification of rice bran oil containing high free fatty acids (acid value=119.7) with theoretical equivalent of glycerol. Test results showed that reaction rate (in terms of decrease in acid value) was increased as the reaction temperature was increased regardless of the presence of the catalyst and reaction time (42.7, 21.5 and 10.0 at $170^{\circ}C,\;210^{\circ}C\;and\;250^{\circ}C$, respectively) and as the reaction time was increased regardless of the temperature and the presence of the catalyst (31.1 vs 18.3 for 3 hrs vs 6 hrs). The presence of the catalyst (0.2% tin chloride) also accelerated the rate regardless of the reaction temperature and time (36.9 vs 12.5). Analysis by column chromatography showed that content of triglyceride in the oil was increased to 72.9% and 61.1% from 10.4% and content of free fatty acids in the oil was decreased to 1.4% and 6.1% from 60.2%, when the degummed oil was esterified at $250^{\circ}C$ for 6 hrs in the presence of and in the absence of the catalyst, respectively. The results estimated from the iodine values indicate that polymer formation was not significant, when the oil was esterified for 6 hrs at temperatures up to $210^{\circ}C$. However, it was somewhat significant for the oil esterified at $250^{\circ}C$ for 6 hrs. The catalyst did not affect the polymer formation. Analysis by high performance liquid chromatography showed that oleic acid (42.5%), linoleic acid (29.0%) and palmitic acid (20.3%) were the major fatty acid components of the rice bran oil.

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catalyst-free 유기금속 화학증착법을 이용한 InN nanorods의 성장

  • Kim, Min-Hwa;Hong, Yeong-Jun;Jeong, Geon-Uk;Park, Seong-Hyeon;Lee, Geon-Hun;Mun, Dae-Yeong;Jeon, Jong-Myeong;Kim, Mi-Yeong;Lee, Gyu-Cheol;Yun, Ui-Jun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.126-126
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    • 2010
  • 본 연구에서는 catalyst-free 유기금속 화학증착법 (MOCVD)를 이용하여 사파이어 (0001)면 위에 직접 InN nanorods를 성장하였다. InN 박막의 성장에서 TMIn과 $NH_3$를 전구체로 사용하였으며, 캐리어 가스로는 질소를 사용하였다. 성장 전, 기판에 $1100^{\circ}C$에서 3분간 nitridation 처리를 거친 후 온도를 낮춰 $630{\sim}730^{\circ}C$의 온도범위 에서 InN 박막을 성장하였다. 이때 $710^{\circ}C$의 온도에서 박막은 columnar growth의 특성을 보였으며 동일조건에서 80분간 성장시킨 결과 InN nanorods가 성장되었다. 성장시킨 InN nanorod는 X-선 회절 측정법, 주사 전자 현미경 그리고 투과 전자 현미경을 이용하여 그 특성을 분석하였다. 투과 전자 현미경을 통한 분석결과 지름이 150~200 nm이며 그 길이는 수 ${\mu}m$인 InN nanorod가 성공적으로 성장되었음을 확인하였다. 또한 X-선 회절 측정법과 주사 전자 현미경을 통한 분석에서 이들 nanorods가 대부분 c 방향으로 수직하게 정렬되어 있음을 확인하였다. 또한 Ti/Au (120/80 nm)를 전극으로 사용하여 개개의 nanorod의 전기적 특성을 분석한 결과 linear한 I-V특성이 관찰되었으며 비저항은 평균적으로 $0.0024\;{\Omega}cm$ 이었다. transfer 특성의 측정결과 -50V까지 게이트 전압을 인가하여도 드레인 전류의 변화는 매우 적어 doping level이 상당히 높다고 예상가능하다. 또한 mobility는 $133\;cm^2/Vs$로 도출되었다.

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A Density-Functional Theory Study on Mechanisms of the Electrochemical Nitrogen Reduction Reaction on the Nickel(100) Surface (범밀도함수이론에 기초한 니켈(100) 표면에서의 전기화학적 질소환원반응 메커니즘에 관한 연구)

  • Minji Kim;Sangheon Lee
    • Korean Chemical Engineering Research
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    • v.61 no.4
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    • pp.604-610
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    • 2023
  • The nitrogen reduction reaction (NRR), which produces NH3 by reducing N2 under ambient conditions, is attracting attention as a promising technology that can reduce energy consumption in industrial processes. We investigated the adsorption behaviors at various active sites on the Ni (100) surface, which is widely used among catalytic metal surfaces capable of adsorbing and activating N2, based on density-functional theory calculations. We also investigated two N2 adsorption structures, so-called end-on and side-on structures. We find that for the end-on case, N2 is adsorbed on a top site, and the reaction proceeded in a distal pathway, while for the side-on case, N2 is adsorbed on a bridge site, and the reaction proceeded with enzymatic pathway. Finally, this study provides insight into the adsorption of metal catalyst surfaces for the NRR reactions based on the calculated Gibbs free energy profiles of the thermodynamically most favorable pathways.

The Effects of Glycerol Aftertreatment for Low-Formaldehyde Finishing (Glycerol 후처리에 의한 Free-formaldehyde 발생 억제 효과)

  • Choi Suk-Chul;Kim Ho-Jung
    • Journal of the Korean Society of Clothing and Textiles
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    • v.10 no.2
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    • pp.59-67
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    • 1986
  • To control the amounts of formaldehyde released from the cotton fabric finished with N-methylol compounds, glycerol was used as a formaldehyde-scavenging agent. It was observed the effects of catalysts and curing conditions when aftertreated with glycerol on melamine resin finished fabric. The effects of Different processes of glycerol treatment, and different resins, urea resin and melamine resin, were compared. The conclusions obtained from the results are as follows: 1) It was shown hatt the aftertreatment with glycerol (treated without catalyst) was more effective than treated with catalysts in controlling free formaldehyde. 2) The optimum curing temperature and curing time for the glycerol aftertreatment without adversely affecting the other properties of fabric was about $160^{\circ}C$, 3 min. 3) According to the increase of glycerol concentration in both aftertreatment and simultaneous treatment the amounts of free formaldehyde was reduced. The rate of decrease was manifest within the limits of $6\%$ in the case of simultaneous treatment with glycerol ana resins, and $3\%$ in the case of glycerol aftertreatment on resin finished fabrics. 4) Dry wrinkle recovery angle was decreased the increase of glycerol concentration. Melamine resin had a little adverse effect than urea resin, particulary glycerol aftertreatment. 5) The breaking strength was increased with the increase of glycerol concentration.

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Three Component Solvent-free Synthesis of Chroman-2,4-dione-based Heterocyclic Ketene Aminal (HKA) Derivatives by "GAP" Chemistry

  • Yu, Fu-Chao;Hao, Xiao-Pan;Jiang, Xiu-Yang;Yan, Sheng-Jiao;Lin, Jun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1625-1632
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    • 2014
  • A concise and efficient one-pot synthesis of chroman-2,4-dione-based HKA derivatives by three component reaction of HKAs, triethoxymethane and 4-hydroxycoumarin derivatives under solvent-free and catalyst-free conditions is described. This protocol has many advantages, in that the GAP (Group-Assistant-Purification) chemistry process is involved in this method. As a result, the experimenter can avoid cumbersome process steps such as traditional chromatography and recrystallization purifications. The desired products can be easily obtained by washing the crude products with 95% EtOH.

Hydrogen production by catalytic decomposition of methane over carbon black catalyst in a fluidized bed (카본블랙 촉매를 이용한 유동층 반응기에서 메탄의 직접 열 분해에 의한 수소생산 연구)

  • Jung, Jae-Uk;Nam, Woo-Seok;Yun, Ki-Jun;Lee, Dong-Hyun;Han, Gui-Young
    • 한국신재생에너지학회:학술대회논문집
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    • 2005.06a
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    • pp.284-287
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    • 2005
  • A fluidized bed reactor made of quartz with 0.055 m I.D. and 1.0 m in height was employed for the thermocatalytic decomposition of methane to produce $CO_2 - free$ hydrogen. The fluidized bed was proposed for the continuous withdraw of product carbons from the reactor. The methane decomposition rate with the carbon black N330 catalyst was quickly reached a quasi-steady state rate and remained for several hour. The methane decomposition reaction was carried out at the temperature range of $850-925^{\circ}C$, methane gas velocity of $1.0U_{mf}\;3.0U_{mf}$ and the operating pressure of 1.0 atm. Effect of operating parameters such as reaction temperature, gas velocity on the reaction rates was investigated. The produced carbon by the methane decomposition was deposited on the surfaces of carbon catalysts and the morphology was observed by SEM image.

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