• Title/Summary/Keyword: 수소 환원

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Oxidation of Benzyl Ethers in Sodium Hypochlorite Mediated Piperidine-1-oxyl System (촉매량의 Piperidine-1-oxyl과 NaOCl계에서 벤질 에테르 유도체들의 산화 반응)

  • Cho, Nam Sook;Park, Chan Heun
    • Journal of the Korean Chemical Society
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    • v.39 no.8
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    • pp.657-665
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    • 1995
  • The oxidation of various benzyl ethers and benzyl alkyl ethers to benzoates has been studied in two-phase system of $CH_3CO_2Et$ and aqueous NaOCl (6.6 mol eq.). The oxidant N-oxo-4-methoxy-2,2,6,6-tetramethylpiperidium bromide (N-oxoammonium salt) was prepared in situ and recycled by addition of 4-methoxy-2,2,6,6-tetramethylpiperidine-1-oxyl (0.03 mol eq., 4-methoxy-TEMPO), co-catalyst KBr (0.03mol eq.) and second oxidant NaOCl. Thus the catalytic amount of 4-methoxy-TEMPO was used. An adjustment of the pH value of below 8.0 was also required for this reaction with 2.5 hr of reaction time at 0∼5$^{\circ}C$. Under these conditions benzyl ethers were oxidized to benzoates. The selectivity of oxidation of benzyl alkyl ethers is dependent on the acidity of hydrogen and steric effect of alkyl group.

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화학적 구조 설계를 통한 수계 Cu-In-S 잉크와 액상셀렌화 법의 개발을 통한 고효율의 CISSe 태양전지 제작

  • O, Yun-Jeong;Yang, U-Seok;Kim, Ji-Min;Mun, Ju-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.428-428
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    • 2016
  • Copper indium sulfide (selenide) (CuIn(S,Se)2,CISSe)는 1.0~1.5 eV의 Direct band gap과 105 cm-1이 넘는 큰 광 흡수 계수를 가지고 있어 박막 태양전지의 흡수층으로써 연구되어 왔다. 최근 대량생산 및 저가 공정에 용이하다는 측면에서 용액 공정 기반 CISSe 태양전지 연구가 크게 주목 받고 있다. 용액공정 기반 중 하이드라진을 사용 한 경우 매우 높은 효율을 기록하였으나, 하이드라진 자체의 유독성과 폭발성 때문에 분위기 제어가 필요하고 여전히 저가화 및 대면적 제작에 한계가 있다. 따라서 알코올 솔젤 기반 CISSe 태양전지 제작 연구가 많이 진행되었으나, 결정립 성장 및 칼코겐 원자를 공급하기 위해 불가피하게 황화/셀렌화 후속 열처리 공정을 요구한다. 후속 열처리 공정은 폭발성의 황화수소/황화셀레늄 기체 분위기 제어와 고가의 장비를 필요로 한다. 본 연구에서는 매우 안정적이며 저가 용매인 물과 아민계 첨가제를 이용하여 Cu, In 전구체와 S, Se 이 포함된 Cu-In-S 잉크와 Se잉크를 제작하였다. 잉크 내에 S, Se을 첨가 함으로써 추가적인 후속공정 없이 비활성 가스 분위기에서 고품질의 CISSe 박막 제작을 가능케 하였다. 또한 Se 잉크 증착 횟수에 따른 결정 구조, 광학적 성질의 차이에 주목하였다. 따라서 수계 잉크를 대기 중에서 스핀코팅으로 박막을 제작한 후, Hot plate에서 건조하여 균일한 박막을 제조하고, 제작된 박막을 tube furnace에서 환원 분위기 및 비활성 가스 분위기에서 열처리 진행하여 $1.3{\mu}m$ 두께의 고품질의 CISSe 흡수층을 제작하였다. 이러한 흡수층에 대해 XRD, SEM, EDS 분석을 진행하여, 결정성, 미세구조, 및 조성을 확인하였으며, 제작된 흡수층 위에 버퍼층/투명전극층을 차례로 증착하여 CISSe 태양전지를 제작하여 셀 성능 및 양자 효율 특성을 파악하였다. 또한 액상 Raman 분석을 통해 결정립 성장 과정 메커니즘을 제시하였다.

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Syntheses of New Nitrogen-Oxygen Multidentate Ligands and Their Stability Constants of Transition Metal(Ⅱ) Ions (새로운 질소-산소계 여러 자리 리간드의 합성 및 전이금속(Ⅱ)이온 착물의 안정도상수)

  • Kim, Sun Deuk;Jang, Ki Ho;Kim, Jun Kwang
    • Journal of the Korean Chemical Society
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    • v.42 no.5
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    • pp.539-548
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    • 1998
  • Multidentate N,O-containing ligands, such as N,N'-bis(2-hydroxybenzyl)-ethylenediamine(BHED), N,N'-bis(2-hydroxybenzyl)-propylenediamine(BHPD), N,N'-bis(2-hydroxybenzyl)-diethylenetriamine(BHDT), N,N'-bis(2-hydroxybenzyl)-triethylenetriamine(BHTT) and N,N'-bis(2-hydroxybenzyl)-tetraethylenepentaamine (BHTP) were synthesized by reduction of the imine group of Bis(salicylidene)-ethylendiamine(BSED), Bis (salicylidene)-propylenediamine(BSPD), Bis(salicylidene)-diethylentriamine(BSDT), Bis(salicylidene)-triethylenetetraamine(BSTT) and Bis(salicylidene)-tetraethylenepentaamine(BSTP). Proton dissociation constants of the ligands and stability constants of transition metal(Ⅱ) ion complexes with BHED, BHPD, BHDT, BHTT, and BHTP were determined by potentiometic titration. The sequence of stability constants $(logK_{ML})$ of complex increases as BHED Zn(Ⅱ) which follows the Irving-Williams series.

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Synthesis and Electrochemical Characteristics of Carbon added Li3V2(PO4)3 (탄소첨가한 Li3V2(PO4)3의 합성 및 전기화학적 특성)

  • Jo, Yeong-Im;Na, Byung-Ki
    • Journal of the Korean Electrochemical Society
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    • v.15 no.2
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    • pp.101-108
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    • 2012
  • The purpose of this study was to improve the conductivity of $Li_3V_2(PO_4){_3}$ by adding carbon source so that the discharge rate and cyclic properties were improved. Glucose and CNT were added to $Li_3V_2(PO_4){_3}$ and the structure and electrochemical properties were studied. $Li_3V_2(PO_4){_3}$, $Li_3V_2(PO_4){_3}$/C and $Li_3V_2(PO_4){_3}$/CNT were synthesised by solid state reaction using hydrogen reduction method at 600, 700, 800, $900^{\circ}C$. The cathode materials were assembled to coin cell type 2032 with Lithium metal as a counter electrode. The coin cell was galvanostatically evaluated in the voltage range of 3.0~4.8 V.

A Comparison Study on the Separation Process of TaCl5 from the Chlorinated Reaction Product (염화반응법으로 제조된 TaCl5의 분리공정에 관한 비교 연구)

  • Cho, Jung-Ho;Park, So-Jin;Choi, Young-Yoon
    • Korean Chemical Engineering Research
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    • v.44 no.3
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    • pp.259-264
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    • 2006
  • The separation and purification of $TaCl_5$is indispensable in the synthetic process of $TaCl_5$by chlorination of tantalum oxide. The reaction products are mainly $TaCl_5$, $NbCl_5$, $TiCl_4$ and $FeCl_2$. However, we need to separate $TaCl_5/NbCl_5$ mixture from the reaction product, because $TaCl_5$ and $NbCl_5$ are easily separated each other by distillation or hydrogen reduction process. In this work, a comparison study was carried out between direct sequence and indirect sequence to obtain $TaCl_5/NbCl_5$ mixture from the reaction product by removing light component, $TiCl_4$ and heavy component, $FeCl_2$ using two distillation columns. It was concluded that the direct sequence gave better results than indirect sequence in the aspect of initial capital costs and the associative operating costs.

Characteristics of Low Temperature De-NOx Process with Non-thermal Plasma and NH3 Selective Catalytic Reduction (I) (저온 플라즈마 및 암모니아 선택적 환원공정을 활용한 저온 탈질공정의 특성(I))

  • Lee, Jae-Ok;Song, Young-Hoon
    • Applied Chemistry for Engineering
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    • v.17 no.4
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    • pp.409-413
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    • 2006
  • An experimental study on a combined $De-NO_x$ process of non-thermal plasma and $NH_{3}$ SCR, which can be operated under low temperature conditions, i.e. $150{\sim}200^{\circ}C$, has been conducted. The test results confirmed feasibility of fast SCR reaction, which shows faster reactivity compared with typical SCR reaction under the low temperature conditions. The test showed that pre-oxidation step to convert NO to $NO_2$ is necessary for the fast SCR reaction, and the appropriate ratio of $NO_{2}/NO_{x}$ ranges from 0.3 to 0.5. Ammonium salts produced under low temperature conditions, effects of hydrocarbons on the combined process, the operation power of the process are discussed in the present study.

투명전극용 박막의 제작과 전기적인 특성에 대한 연구

  • O, Teresa
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.42.1-42.1
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    • 2011
  • 박막형 디스플레이구서에 있어서 투명전극은 필수적이다. 투명전극은 정보를 표시하기 위해 빛을 외부로 방출시키거나 태양광 등을 소자 내부로 입사시켜야 한다. 또한 전극을 형성하는 박막은 높은 광투과율과 ${\sim}10-4{\Omega}cm$ 정도의 낮은 전기비저항을 가져야 한다. 가장 널리 사용되는 투명전극으로 ITO (Indium Tin Oxide)는 인듐의 독성, 저온증착의 어려움, 스퍼터링시 음이온 충격에 의한 막 손상으로 저항의 증가 및 액정디스플레이의 투명전극으로 사용될 경우 $400^{\circ}C$정도의 높은 온도와 수소플라즈마 분위기에서 장시간 노출시 열화로 인한 광학적 특성변화가 문제로 지적된다. 이러한 문제 해결의 대안으로 ZnO 산화물 반도체가 있는데 ITO 박막에 비해 비저항이 높기 때문에 도핑을 이용한 비저항을 ${\sim}10-4{\Omega}cm$ 정도로 낮추어야 한다. 투명전도막으로는 ITO, FTO 등과 더블어 체적 저항율은 다소 높으나 환원성 분위기에 대한 내성, 가시광 영역에서의 높은 광투과율과 저렴한 가격 등의 장점 등으로 AZO 박막이 주목 받고 있다. ZnO는 ITO 나 FTO에 비해서 700 kJ/mol의 큰 분해에너지를 가지므로 코팅 때 발생하는 전도도 및 투과율이 나빠지는 현상이 발생하지 않는 특징이 있으며, 위의 두 재료에 비해 밴드갭도 가장 낮아서 자외선 투과율이 낮다. 그러나 내습성이 약하기 때문에 이를 보완하기 위하여 내습성향상과 전도성 향상을 위해서 3족 원소인 B, In, Al, Ga 등을 도핑한 ZnO 투명전도막의 연구가 진행되고 있다. 이러한 원소들 중에서 Al로 도핑했을 때 가장 낮은 비저항을 얻을 수 있다고 알려져 있다. 본 연구에서는 SiOC 박막위에 AZO 박막을 제조하기 위하여 RF 마그네트론 스퍼터링법을 이용하여 박막을 성장시켰으며, 박막의 전기적 및 광학적 특성을 조사하였다. AZO 박막은 rf power가 5~200 W인 RF 마그네트론 스퍼터 방법에 의해서 제작되었다. SiOC 박막은 산소와 DMDMOS 전구체의 유량비를 다르게 하여 플라즈마 발생 화학적 기상 증착방법으로 증착되었다. 증착된 SiOC박막은 UV visible spectroscopy에 의해서 분석하였다. 투명전극의 비저항은 rf 전력이 작을 수록 낮았으며, SiOC 절연막 위에 AZO를 증착시킨 후 반사률은 반대로 바뀌는 것을 확인하였다.

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Shallow gas origin in the sediment near coastal area of Busan (부산 주변 해역 해저 퇴적물 내 공기층 가스 기원)

  • Kim, Ji-Hoon;Han, Hyun-Chul;Cheong, Tae-Jin;Lee, Young-Joo
    • The Korean Journal of Petroleum Geology
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    • v.13 no.1
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    • pp.24-29
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    • 2007
  • The main purpose of this study is to identify the shallow gas origin in the KSSM zone. Based on the results of gas composition and isotope in the headsapace gas, the shallow gas is mainly composed of methane and carbon and deuterium isotopes (${\delta}^{13}CCH_4$ and ${\delta}DCH_4$) of methane has ranged from -93.4%o to -70.9%, and from -228%o to -199%o in each. These results imply that shallow gas has predominately biogenic source by $CO_2$ reduction rather than thermogenic. The carbon isotopic separation (${\varepsilon}_c$) between methane and carbon dioxide $(CO_2)$ has a range of 54.4 to 72.2, it also supports biogenic origin of shallow gas.

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Fabrication of Porous Mo by Freeze-Drying and Hydrogen Reduction of MoO3/Camphene Slurry (MoO3/camphene 슬러리의 동결건조 및 수소환원에 의한 Mo 다공체 제조)

  • Lee, Wonsuk;Oh, Sung-Tag
    • Journal of Powder Materials
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    • v.19 no.6
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    • pp.446-450
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    • 2012
  • In order to fabricate the porous Mo with controlled pore characteristics, unique processing by using $MoO_3$ powder as the source and camphene as the sublimable material is introduced. Camphene-based 15 vol% $MoO_3$ slurries, prepared by milling at $50^{\circ}C$ with a small amount of dispersant, were frozen at $-25^{\circ}C$. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was hydrogen-reduced at $750^{\circ}C$, and sintered at $1000-1100^{\circ}C$ for 1 h. After heat treatment in hydrogen atmosphere, $MoO_3$ powders were completely converted to metallic W without any reaction phases. The sintered samples showed large pores with the size of about $150{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal wall of large pores and near bottom part of specimen had relatively small pores due to the difference in the camphene growth rate during freezing process. The size of small pores was decreased with increase in sintering temperature, while that of large pores was unchanged. The results are strongly suggested that the porous metal with required pore characteristics can be successfully fabricated by freeze-drying process using metal oxide powders.

Synthesis and Biological Activity Test of the Sex Pheromone of the Diamond Back Moth (배추좀나방의 성 페로몬의 합성과 생물활성시험)

  • Suk-Ku Kang;Chul-Hee Lee;Jung Han Kim;Jeong-Oon Lee
    • Journal of the Korean Chemical Society
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    • v.32 no.1
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    • pp.60-64
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    • 1988
  • Synthesis and biological activity test are described for the (Z)-11-hexadecen-1-ol, (Z)-11-hexadecen-1-yl acetate, and (Z)-11-hexadecen-l-al, the sex pheromone of the diamond back moth, Plutella xylostella L.. Lithium acetylide was alkylated with 10-bromodecan-1-ol THP ether to give 11-hexadecyn-l-ol THP ether. 11-Hexadecyn-l-ol THP ether was stereoselectively reduced over Pd/BaSO4to yield (Z)-11-hexadecen-l-ol THP ether, which was in turn deprotected to provide (Z)-11-hexadecen-l-ol. (Z)-11-Hexadecen-l-ol was acetylated and oxidized to afford (Z)-11-hexadecen-1-yl acetate and (Z)-11-hexadecen-l-al, respectively. Biological activity test of the synthetic compounds, (Z)-11-hexadecen-l-ol, (Z)-11-hexadecen-1-yl acetate, and (Z)-11-hexadecen-l-al in the ratio of 0.1 : 5 : 5 was tested in the field using polyethylene capsules as containers. The numbers of moth trapped with pheromone vials were counted.

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