• 제목/요약/키워드: Allyl silica

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플라즈마 코팅된 실리카와 에폭시 수지간의 반응성 연구 (Study of Heat of Reaction Between Plasma Polymer Coated Silica Fillers and Biphenyl Epoxy Resin)

  • 김남일;강현민;윤태호
    • 한국복합재료학회:학술대회논문집
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    • 한국복합재료학회 2004년도 추계학술발표대회 논문집
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    • pp.96-99
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    • 2004
  • Silica fillers were coated by plasma polymer coatings of 1,3-diaminopropane, allylamine, pyrrole, 1,2-epoxy-5-hexene, allyl mercaptan and allyl alcohol using RF plasma (13.56 MHz). The coated fillers were then mixed with biphenyl epoxy, phenol novolac (curing agent) and/or triphenylphosphine (catalyst), and subjected to DSC analyses in order to elucidate the chemical reaction between functional moieties in the plasma polymer coatings and the epoxy resin. Only the samples with 1,3-diaminopropane and allylamine plasma polymer coated silica fillers showed heat of reaction peaks when they were mixed with biphenyl epoxy resin only, while these samples as well as the samples with 1,3-diaminopropane, allylamine and pyrrole plasma polymer coated silica fillers exhibited heat of reaction peaks when mixed with both biphenyl epoxy and phenol novolac (curing agent).

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Mo/SiO2 촉매상에서 t-Butyl hydroperoxide에 의한 염화알릴의 에폭시화반응에 관한 속도론적 연구 (Kinetic Study on the Epoxidation of Allyl Chloride by t-Butyl Hydroperoxide over Mo/SiO2 Catalyst)

  • 김성우;박대원;정종식;박대철
    • 공업화학
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    • 제3권4호
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    • pp.649-656
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    • 1992
  • t-Butyl hydroperoxide(TBHP)에 의한 염화알릴의 에폭시화에 의해서 에피클로로히드린을 합성하는데 실리카에 담지된 몰리브데늄 촉매를 사용하였다. 속도론적 연구는 회분 반응기를 사용하여 $60-80^{\circ}C$, 10기압에서 TBHP/염화알릴의 농도비를 0.01-0.1의 범위내에서 수행하였다. t-butyl alcohol(TBA)에 의해서 염화알릴의 에폭시화 반응이 억제되었고, 반응속도는 Michaelis-Menten 형태의 속도식으로 표현할 수 있었다. 반응기구는 TBHP와 TBA의 가역흡착과 $Mo/SiO_2$에 흡착된 TBHP와 염화알릴의 표면반응으로 설명할 수 있었다.

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실리카에 고정화된 이온성액체를 촉매로 이용한 알릴글리시딜에테르와 이산화탄소의 부가반응 (Cycloaddition of Carbon Dioxide to Allyl Glycidyl Ether Using Silica-supported Ionic Liquid as a Catalyst)

  • 심혜림;이미경;유정인;박대원
    • 청정기술
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    • 제14권3호
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    • pp.166-170
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    • 2008
  • 본 연구에서는 이미다졸륨계의 이온성액체를 실리카에 고정화시킨 촉매를 제조하고, 알릴글리시딜에테르(AGE)와 이산화탄소의 부가반응을 통한 이종 5원환 카보네이트의 합성반응에서 이 촉매의 반응특성을 고찰하였다. 고정화된 이온성액체는 chloropropyl 그룹이 도입된 실리카에 이미다졸이 고정화됨으로써 형성되었다. 제조된 촉매는 XRD, BET, $^{29}Si$ MAS-NM]t 그리고 SEM 등 다양한 기기분석을 통하여 특성분석을 수행하였다. $^{29}Si$ MAS-NMR을 통하여 chloropropyl 그룹이 부과된 실리카 표면에 이온성액체가 잘 형성 되어있었음을 관찰하였다. 고정화된 이온성액체 촉매는 반응온도 $80-120^{\circ}C$의 범위에서 AGE의 전환율이 55-67% 이고 생성물의 선택도가 85% 이상으로 우수한 반응성을 나타내었다. 또한 고정화된 이온성액체 촉매는 균일계 촉매인 1-n-butyl-3-methyl imidazolium bromide (BMImBr)보다 더 높은 AGE의 전환율과 생성물의 선택도를 나타내었다.

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Titanized or Zirconized Porous Silica Modified with a Cellulose Derivative as New Chiral Stationary Phases

  • Seo, You-Jin;Kang, Gyoung-Won;Park, Seong-Tae;Moon, Myeong-Hee;Park, Jung-Hag;Cheong, Won-Jo
    • Bulletin of the Korean Chemical Society
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    • 제28권6호
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    • pp.999-1004
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    • 2007
  • Spherical porous silica supports modified with titanium or zirconium alkoxides were prepared, and allyl groups were chemically attached to the titanized or zirconized silica supports, and the product was cross-polymerized with a double bond containing cellulose derivative to yield new CSPs (chiral stationary phases). Magic angle spinning 13C solid state NMR and elemental analysis were used to characterize the CSPs. The performances of the chiral stationary phases were examined in comparison with a conventional chiral stationary phase. Spherical porous silica particles modified with 3,5-dimethylphenylcarbamate of cellulose were prepared and used as the conventional chiral stationary phase. Chromatographic data were collected for a few pairs of enantionmers in heptane/2-propanol mixed solvents of various compositions with the three chiral columns and the results were comparatively studied. The separation performance of the chrial phase made of the titanized silica was better than the others, and the separation performance of the chiral phase of the zirconized silica was comparable to that of the conventional chiral phase. The superiority of titanized silica over bare or zirconized silica in chiral separation seemed to be owing to the better yield of crosslinking (monitored by increase of carbon load) for titanized silica than for the others.

실리카겔에 고정화된 산성 이온성 액체 촉매를 이용한 올레산의 에스터화 반응연구 (The Esterification of Oleic Acid Using Acidic Ionic Liquid Catalysts Immobilized on Silica Gel)

  • 최재형;박용범;이석희;천재기;우희철
    • Korean Chemical Engineering Research
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    • 제48권5호
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    • pp.583-588
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    • 2010
  • 유리지방산 함량이 높은 원료의 효율적인 바이오디젤 생산을 위해 다양한 고체산 촉매를 사용하여 회분식 반응기에서 유리지방산의 에스터화 반응에 대한 연구를 수행하였다. 고체산 촉매는 상용 촉매인 황산기를 지닌 이온교환수지(Amberlyst-15, Dowex 50Wx8)와 실리카겔에 술폰기 및 염화술폰기 지닌 산성 이온성 액체가 고정화된 촉매($SiO_2-[ASBI][HSO_4]$, $SiO_2-[ASCBI][HSO_4]$), 단순히 실리카겔에 술폰기 및 염화술폰기의 산성적 기능기를 도입한 촉매들을 사용하여 반응특성을 비교하였다. 또한 에스터화 반응 실험변수로써 반응시간, 온도, 반응물간의 몰 비율(메탄올:올레산), 촉매량에 대한 영향을 조사하였다. 사용된 고체산 촉매들 중 실리카겔에 고정화된 알릴이미다졸리움을 포함한 산성 이온성 액체 촉매가 가장 우수한 반응성을 나타내었다. 특히 실리카겔에 3-allyl-1-(4-sulfobutyl)imidazolium hydrogen sulfate가 고정화된 $SiO_2-[ASBI][HSO_4]$ 촉매가 같은 반응조건에서 기존의 알려진 Amberlyst-15보다 더 나은 성능을 보였으며, 353 K 반응온도와 5 wt%의 촉매량, 메탄올/올레산의 몰 비율 20의 조건에서 2시간 동안 약 96%의 높은 전환율을 나타내었다. $SiO_2-[ASBI][HSO_4]$의 높은 촉매 활성은 실리카에 고정화된 강한 브뢴스테드산의 작용기에 기인한 것으로 생각된다. 바이오디젤로부터 촉매의 분리 및 회수는 간단한 경사법 혹은 여과법에 의해 쉽게 분리할 수 있고, 이를 회수하여 재사용이 가능하다.

나무가지꼴 실란 거대분자의 제법 (Ⅱ) (Preparation of Silane Dendrimer (Ⅱ))

  • 김정균;박은미;강은주
    • 대한화학회지
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    • 제39권10호
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    • pp.799-805
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    • 1995
  • 96개의 allyl기를 가진 나무가지꼴 실란 거대분자를 alkenylation 과 hydrosilylation의 반복된 과정을 경유하여 매우 높은 수율로 합성하였다. 이 두 과정을 통해서 나무가지꼴 거대분자는 크로마토그래피법을 이용한 정제법(silica hel, chloroform)에서 순수한 물질을 얻어졌음이 $/_1/H,\;/_13/CNMR$과 원소분석 등에 의해 확인되었다.

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Anticoagulation and Anticancer Constituents from Eugenia caryophyllata Thunb

  • Han, Kyung-Min;Kim, Dong-Hyun;Ahn, Eun-Mi;Lee, Youn-Hyung;Chung, In-Sik;Kim, Dae-Keun;Kwon, Byoung-Mog;Kim, Sung-Hoon;Baek, Nam-In
    • 한국약용작물학회지
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    • 제15권2호
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    • pp.82-88
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    • 2007
  • From the EtOAc fraction of Eugenia caryophyllata, four compounds were isolated through activity-guided silica gel column chromatography, From the result of spectroscopic data including NMR, MS and IR, the chemical structures of the compounds were determined as 1-allyl-4-hydroxy-3-methoxybezene acetate (eugenol acetate, 1), 1-allyl-4-hydroxy-3-methoxybezene (eugenol, 2), $3{\beta}-hydroxyolean-12-en-28-oic$ acid (oleanolic acid, 3) and $2{\alpha}$, $3{\beta}-dihydroxyolean-12-en-28-oic$ acid (maslinic acid, 4). Compounds 3 and 4 were isolated for the first time from this plant. Also, compounds 1, 2 and 3 exhibited relatively high platelet aggregation inhibitory activity with the $IC_{50}$ values of 0.24, 0.09 and 0.07 mM, respectively. Compound 2 significantly prolonged activated partial thromboplastin time (aPTT) with the value of $124{\pm}11.2$ seconds as compared to the control with the value of $37.5{\pm}2.2$ seconds at the concentration of 50 ${\mu}g/ml$. Compounds 1 and 3 revealed inhibitory activity on farnesyl protein transferase (FPTase) with the $IC_{50}$ values of 0.49 and 0.24 mM and compounds 1 and 2 highly inhibited the growth of rat-H-ras cells with the $Gl_{50}$ values of 6.63 and 5.70 ${\mu}M$, respectively.

Preparation of Cucurbituril Anchored Silica Gel by Cross Polymerization and Its Chromatographic Applications

  • Cheong, Won-Jo;Go, Joung-Ho;Baik, Yoon-Suk;Kim, Sung-Soon;Nagarajan, Erumaipatty R;Selvapalam, Narayanan;Ko, Young-Ho;Kim, Ki-Moon
    • Bulletin of the Korean Chemical Society
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    • 제29권10호
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    • pp.1941-1945
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    • 2008
  • A new chromatographic stationary phase has been prepared by cross polymerization between allylsilica and perallyloxycucurbit[6]uril and characterized by elemental analysis and FT-IR spectroscopy. The double endcapping has been proven to improve the separation efficiency of the cucurbituril-based stationary phase material. The first end-capping was carried out when allylsilica was made. The second end-capping was done as the final step of the whole process, and the use of a mixture of hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) as an end-capping reagent was found better than the use of only HMDS or TMCS. Our stationary phase has shown generally good results in separation of nonpolar and polar analytes. This phase showed even better separation performance than the commercial C18 phase for the case where hostguest chemistry was properly incorporated in solute retention.

입본특이적(立本特異的) 방법(方法)과 $^{13}C-NMR$ 기법(技法)에 의한 잣기름의 트리아실 글리세롤의 구성지방산(構成脂肪酸)의 분포(分布)에 관한 연구(硏究) (Studies on the Fatty Acid Distribution in the Position of Triacylglycerols from the Seed of Pinus Koraiensis by Stereo-specific Analysis and $^{13}C-NMR$ Techniques)

  • 우효경;김성진;조용계
    • 한국응용과학기술학회지
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    • 제15권4호
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    • pp.35-44
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    • 1998
  • All the triacylglycerols including the molecular species having ${\Delta}^5$-unsaturated fatty acids from the seeds of Pinus Koraiensis, were split into a mixture of diacylglycerols by a Grignard reagent prepared with allyl bromide without arousing acyl chains of a glycerol moiety to migration, and were also easily partially hydrolyzed to diacylglycerols by pancreatic lipase. (S)-(+)-(1-naphthyl)ethyl urethane(NEU) derivatives of the diacylglycerol mixture derived from the triacylglycerols were fractionated into sn-1, 3-, sn-1, 2- and sn-2, 3-DG-NEU by silica-HPLC and the fatty acid composition of these fractions was analysed. $C_{18:1{\omega}9}$ is distributed evenly in the three positions of TG with $C_{18:2{\omega}6}$ mainly located in sn-2 position, while ${\Delta}^5$-unsaturated fatty acids such as ${\Delta}^{5.9}-C_{18:2}$, ${\Delta}^{5.9.12}-C_{18:3}$ and ${\Delta}^{5.11.14}-C_{20:3}$ are exclusively present in the sn-3 position. These results could be confirmed by $^{13}C$-NMR spectroscopy : the signals at $^{\delta}$173.231 ppm and $^{\delta}$172.811 ppm of the carbonyl carbon of acyl moieties indicate the presence of saturated acids and/or $C_{18:1{\omega}9}$ (oleic acid) in the ${\alpha}({\alpha}')$- or ${\beta}$- positions, and $C_{18:2{\omega}6}$ including $C_{18:1{\omega}9}$ in the ${\beta}$-position, respectively. In addition, the resonance at $^{\delta}$173.044 ppm suggested a location of ${\Delta}^5$-unsaturated fatty acid moiety in the ${\alpha}({\alpha}')$-position.