• 제목/요약/키워드: Reaction Crystallization

검색결과 249건 처리시간 0.025초

A Novel Synthetic Method for Bepotastine, a Histamine H1 Receptor Antagonist

  • Ha, Tae Hee;Suh, Kwee-Hyun;Lee, Gwan Sun
    • Bulletin of the Korean Chemical Society
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    • 제34권2호
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    • pp.549-552
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    • 2013
  • An efficient and alternative synthesis of enantiomerically pure (+)-(S)-4-(4-((4-chlorophenyl)(pyrid-2-yl)methoxy]piperidin-1-yl)butanoic acid, bepotastine (1) is described. The key resolution of (R/S)-bepotastine l-menthyl ester (3) is achived via diastereomeric salt crystallization using N-benzyloxycarbonyl-L-aspartic acid (NCbzLAA) as the resolving agent to provide (S)-bepotastine l-menthyl ester (S)-3. Hydrolysis of (S)-bepotastine l-menthyl ester (S)-3 afforded the desired bepotastine (1) with good yields and enantiopurity (> 99%). Finally, bepotastine besilate (4) and bepotastine calcium (5) are achived by salt formation of bepotastine (1) with benzene sulfonic acid and calcium salt respectively. The reaction conditions were optimized to make suitable for commercial scale production.

카올리나이트의 상전이반응 과정 연구 (An Investigation of the Transformation Sequence from Kaolinite to Mullite)

  • 이수정;김윤중;문희수
    • 한국광물학회지
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    • 제11권1호
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    • pp.32-44
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    • 1998
  • The transformation sequence of kaolinite to mullite is examined with new electron diffraction data obtained mainly by an energy filtering transmission electron microscope. Kaolinite is transformed finally into mullite and cristobalite through several steps of continuous reactions by heating, which result in metakaolinite, microcrystalline spinel-type phase and amorphous silica. Metakaolinite maintains a short-range order in its structure ven at $920^{\circ}C$. Spinel phase results from a topotactictransformation of metakaolinite apart from the breakdown of metakaolinite structure. the first strong exothermic peak on DTA curve is mainly due to the extraction of amorphous silica from metakaolinite and the gradual nucleation of mullite. Metakaolinite decomposes around$ 940^{\circ}C$ to mullite that doesn't show a clear crystallographic relationship to the parent metakaolinite structure. However, spinel phase produced previously is maintained. The initially formed spinel and mullite phases are suggested to be Al-rich, but progressively gain Si in their structures at higher temperatures. Spinel phase decomposes completely through a second weak exothermic reaction promoting the growth of mullite, and crystallization of amorphous silica to cristobalite.

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Preparation of Mesoporous SiCBN Ceramic Templated by Mesoporous Carbon

  • Nghiem, Quoc Dat;Ryoo, Hyang-Im;Kim, Dong-Pyo
    • 한국세라믹학회지
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    • 제44권7호
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    • pp.358-361
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    • 2007
  • Well-ordered mesoporous SiCBN ceramics have been successfully synthesized by infiltrating a polymeric precursor, which was prepared from borazine and 2,4,6-trimethyl-2,4,6-trivinylcyclotrisilazane via a hydroboration reaction, into a mesoporous carbon (CMK-3) as a hard template. This was followed by pyrolysis at $1400^{\circ}C$ under nitrogen gas and subsequent oxidative removal of the carbon template without chemical etching. The prepared mesoporous SiCBN ceramic was characterized by a small-angle XRD, TEM, and BET surface area. The resulting mesoporous SiCBN ceramic revealed a BET surface area of $275 m^2g^{-1}$ and a pore volume of $0.8 cm^3 g$ with no crystallization.

Peculiarities of amorphous and crystalline dielectric films prepared by sol-gel method

  • Natalya, Korobova;Soh, Dea-Wha
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2005년도 하계학술대회 논문집 Vol.6
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    • pp.401-402
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    • 2005
  • The important parts of material science in the film preparation fields and sol-gel technology are presented. For the present work, a series of amorphous films was prepared in air by sol-gel method without using some alkoxide stabilizer, which reduces the reactivity of the metal alkoxides. The choice of precursors can affect the chemical-reaction kinetics, microstructures and properties of the product. In this report author compared the crystallization behavior of oxide functional films derived from the same precursors, stressing the influence of experiment conditions and where it was possible to obtain the uniform amorphous or crystalline dielectric films. A short analysis of sol-gel technology and thin film methods about development of dielectric materials has been given.

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Preparation of TiO2 Nanotube Arrays from Thin Film Grown by RF Sputtering

  • Kim, Chang Woo
    • Applied Science and Convergence Technology
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    • 제27권5호
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    • pp.105-108
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    • 2018
  • Transparent $TiO_2$ nanotube arrays are successfully prepared by a two-step approach involving electrochemical anodization and RF magnetron sputtering. First, a Ti film is deposited on an FTO substrate by RF magnetron sputtering at room temperature. The morphologies of the Ti film are controlled by the working distance, Ar flow, and DC power. Second, an anodization treatment is electrochemically performed for the formation of nanotube arrays from the deposited Ti film, followed by post-annealing treatment in air for the formation of $TiO_2$ crystallization. The back side of the crystallized $TiO_2$ nanotube arrays is illuminated with solar light to characterize the photoelectrochemical reaction, and their photoelectrochemical properties are investigated. This work provides information on application of a thin film deposited by RF sputtering in the field of photoelectrochemical water splitting.

유기 템플레이트 배제하의 ZSM-5 결정화에 따른 영향인자 (Influencing Factors on the Crystallizations of ZSM-5 in the Absence of Organic Template)

  • 김화중;임창환;이승애;이명철;정찬이
    • 공업화학
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    • 제4권4호
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    • pp.776-784
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    • 1993
  • 유기 템플레이트인 $TPA^+$ 이온의 배제 하에 pentasil 계열의 제올라이트인 ZSM-5를 $210^{\circ}C$에서 합성하였다. 본 연구에서 얻어진 결론에 의하면 유기 템플레이트가 사용되지 않는 합성조건 하에서는 기존의 방법으로는 합성이 되지 않는 것을 알 수 있었다. 결과에 의하면 유기 템플레이트 배제 하에서 ZSM-5의 결정화 반응에 적합한 조성영역은 매우 좁고 $Na_2O/SiO_2$$SiO_2/Al_2O_3$몰비 조절에 세심한 주의를 요해야 하는 것을 보여주고 있다. 이외에도 ZSM-5 결정화 반응에 미치는 혼합방법, 숙성 및 반응시간의 영향이 매우 큰 것을 알 수 있었다.

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대두유로부터 Lipase를 이용한 재구성 지질의 합성 및 특성 (Lipase-Catalyzed Synthesis of Structured Lipids with Capric and Conjugated Linoleic Acid in a Stirred-Batch Type Reactor)

  • 신정아;이기택
    • 한국식품영양과학회지
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    • 제33권7호
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    • pp.1175-1179
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    • 2004
  • Scale-up하기 위하여 24시간동안 1:2:2의 몰 비율로 stirred-batch type reactor에서 합성된 재구성지질은 capric acid와 CLA를 각각 4.9 mol%와 4.1 mot% 함유하였다. 기능성 지방산인 capric acid와 CLA는 주로 TAG의 sn-1,3 position에 분포하였고, sn-2 position에는 linoleic acid가 대부분을 차지하였다. 재구성지질과 대두유의 요오드가는 각각 126와 114이었고, 비누화가는 각각 190과 194로 측정됨으로써, 재구성 지질의 TAG에서 capric acid의 함유를 확인할 수 있었다. 대두유와 재구성지질의 tocopherol함량은 각각 74.6 mg/100 g과 18.2 mg/100 g으로, 재구성지질의 tocopherol 함량은 대두유보다 약 76% 감소하였다. 색도분석 결과, 재구성 지질과 대두유간에 백색도(L*)와 적색도(a*)에서는 유의적 차이가 없었으나(p<0.05),황색도(b*)에서 재구성지질이 대두유보다 좀더 yellowness를 보이며 유의적 차이를 보였다. (p<0.05). Reversed-phase HPLC 분석 결과, 재구성지 질에서 capric acid를 함유하고 있는 TAG형태의 partition number (PN)는 25∼37로 약 12.57 area%이었음을 확인하였다. 대두유의 주된 crystallization peak는 -57.86$^{\circ}C$C이었으나, capric acid를 4.9 mol% 함유하고 있는 재구성지질의 crystallization peak는 -52.78$^{\circ}C$로 대두유보다 결정화가 좀더 고온에서 일어났다.

갈리실리케이트(Ga-MFI)의 합성 및 ZSM-5와의 비교 (Synthesis of Gallosilicate(Ga-MFI} and Its Comparison with ZSM-5)

  • 김영국;황재영;김명수;박홍수;함현식
    • 한국응용과학기술학회지
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    • 제21권3호
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    • pp.231-237
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    • 2004
  • Ga-MFI was synthesized by a hydrothermal process at atmospheric pressure. The effect of mole ratios of reactants on crystallization was also investigated thoroughly. The characteristics of synthesized Ga-MFI was compared with ZSM-5. The synthesis of Ga-MFI was carried out with five different mole-compositions of $\underline{a}SiO_2-\underline{b}Ga_2O_3-\underline{c}Na_2O-\underline{d}TPA_2o-\underline{e}H_2O$. The synthesized Ga-MFI and ZSM-5 were characterized by XRD and FT-IR. The inorganic cation ($Na^+$) and water played an important role in crystallinity and the organic cation ($TPA^+$) as a template played a great influence on yields. With the increase in the amount of $Ga^{3+}$, crystallization time was increased. With a fixed $SiO_2/Ga_2O_3$ ratio of 400, the optimum reaction condition was obtained at $H_2O/SiO_2$=30${\sim}$35, $Na_2O/SiO_2$=0.5${\sim}$0.6, and $TPA_2O/Na_2O$=1${\sim}$1.25. In these cases, the crystallinity and yield were more than 95% and 90%, respectively. By comparing IR spectrum of Ga-MFI with those of ZSM-5 and silicalite, it was found that Ga-MFI showed a unique peak at 970 $cm^{-1}$, which may be used to identify Ga-MFI from ZSM-5 and silicalite.

$Ca^{2+}$$F^-$ 이온이 Struvite 결정화 반응에 미치는 영향 (Inhibition Effects of $Ca^{2+}$ and $F^-$ Ion on Struvite Crystallization)

  • 김승하;김금용;류홍덕;이상일
    • 대한환경공학회지
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    • 제32권7호
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    • pp.730-737
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    • 2010
  • 일반적으로 고농도의 암모니아성 질소, 인 및 불소가 동시에 고농도로 함유되어 있는 반도체 폐수를 처리하기 위하여 사전에 불소를 적절한 방법으로 제거하는 것이 매우 중요하다. 이를 위하여 칼슘을 이용한 제거법이 널리 채택되고 있다. 그러나 불소제거를 위하여 주입하는 칼슘은 암모니아성 질소와 인의 제거를 위한 struvite 반응에 저해를 주기 때문에 최대로 제거할 필요가 있다. 따라서 본 연구는 불소와 칼슘이 함유된 폐수를 대상으로 struvite 결정화반응을 수행할 때 미치는 영향 인자에 대하여 알아보았다. 불소 농도가 증가할수록 암모니아성 질소와 인의 제거율이 급격하게 감소하는 것으로 나타났으며, 특히 인이 암모니아성 질소보다 영향을 크게 받는 것으로 나타났다. 또한 폐수중의 칼슘 농도 증가에 따른 영향은 칼슘 농도가 500 mg/L까지 struvite의 결정구조와 일치하였으나 침전물의 순도는 떨어지는 것으로 확인되었고, struvite 반응시 칼슘에 대한 영향은 인보다 암모니아성 질소가 더 크게 받는 것으로 나타났다.

Polyvinyl Alcohol 용액법에 의해 제조된 나노크기 α-2ZrO2·P2O5 분말의 특성 연구 (Characteristics of Nano-Sized, α-2ZrO2·P2O5 Powder Prepared by Polyvinyl Alcohol Solution Method)

  • 마충일;이상진
    • 한국재료학회지
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    • 제27권4호
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    • pp.179-183
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    • 2017
  • $2ZrO_2{\cdot}P_2O_5$ powder, which is not synthesized by solid reaction method, was successfully synthesized through PVA solution method. In this process, the firing temperature and the PVA content strongly affected the crystallization behavior and final particle size. A stable ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$ was synthesized at a firing temperature of $1200^{\circ}C$ and holding time of 4 h. ${\beta}$-phase $2ZrO_2{\cdot}P_2O_5$ was observed, with un-reacted $ZrO_2$ phases, for firing temperatures lower than $1200^{\circ}C$. In terms of the PVA content effect, the powder prepared with a PVA mixing ratio of 12:1 showed stable ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$; however, the ${\beta}$-phase was found to co-exist at relatively higher PVA content. The synthesized ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$ powder showed an average particle size of 100~250 nm and an average thermal expansion coefficient of $-2.5{\times}10^{-6}/^{\circ}C$ in the range of room temp. ${\sim}800^{\circ}C$.