• Title/Summary/Keyword: THF

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Reaction of Thexylalkoxyboranes with Selected Orgnic Compounds Containing Representative Functional Groups Comparison of Reducing Characteristics of the Alkoxy Derivatives

  • 차진순;장석원;권오운;전중현
    • Bulletin of the Korean Chemical Society
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    • v.19 no.2
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    • pp.243-249
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    • 1998
  • The reaction of alcohol with a solution of thexylborane (ThxBH2) in tetrahydrofuran (THF) provides a new class of mild and selective reducing agents, thexylalkoxyboranes (ThxBHOR: R=Et, i-Pr, i-Bu, s-Bu, t-Bu, Ph). In order to elucidate the effect of the alkoxy group in reduction reactions, the reducing power of ThxBHOR toward selected organic compounds containing representative functional groups under practical conditions (THF, 25°, the quantitative amount of reagent to compound) has been investigated. Generally, the reactivity of ThxBHOR is largely dependent upon the alkoxy substituent. ThxBHOR can be synthesized from a variety of alcohols, thus allowing control of the steric and electronic environment of these reagents.

Synthesis and Properties of Organosilicon Polymers Containing 3,4-Benzo-1-silacyclopentene Derivatives

  • 박영태;박상욱;김호창;이광
    • Bulletin of the Korean Chemical Society
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    • v.19 no.3
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    • pp.328-332
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    • 1998
  • Anionic ring-opening polymerization of 3,4-[(dimethylsilyl)isopropyl]benzo-1,1-dimethyl-1-silacyclopentene in the presence of n-butyllithium and HMPA in THF at - 78 ℃ afforded poly[3,4-(dimethylsilylisopropyl)benzo-1,1-dimethyl-1-silapentene]. The characteristic Si-H stretching frequency in the IR is observed at 2100 cm-1. The polycarbosilane has been modified by chloroplatinic acid catalyzed addition of styrene to the polycarbosilane SiH units. Molecular weights and thermal properties of the polymers were compared. The sol-gel polymerization of 3,4-[(dimethoxysilyl)isopropyl]benzo-1,1-dimethoxy-1-silacyclopentene in the presence of aqueous HCl or NaOH in THF resulted in a cross-linked polysiloxane. The xerogel has a low surface area of 13-14 m2/g and is stable up to about 400 ℃ with only 5% weight loss under a nitrogen atmosphere.

Study on thermodynamic and kinetic properties of $CO_2/H_2$ hydrate with THF, TBAB addition (THF, TBAB 첨가에 의한 $CO_2/H_2$ 하이드레이트의 특성 연구)

  • Ha, Rin;Lee, Hyun Ju;Park, Young Bin;Shin, Jae Ho;Kim, Yang Do
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.11a
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    • pp.153.2-153.2
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    • 2010
  • 화력발전 분야에서 $CO_2$ 분리는 크게 연소전 탈탄소화(pre-combustion capture)와 연소후 포획(post-combustion capture)으로 나누어진다, 연소후 포획은 연료를 연소한 후 발생하는 $CO_2$$N_2$가스에서 $CO_2$를 분리하는 기술로 흡수나, 흡착, 막분리 등을 주로 이용한다, 연소전 탈탄소화는 연소 전에 $CO_2$가 발생되지 않도록 하는 기술로써, 부분 산화나 개질 및 수성가스 변위반응 등이 포함되며 생성된 $H_2$$CO_2$를 분리하여 수소를 생산하는 기술($CO_2/H_2$분리가 핵심)이다. 우리나라는 대부분 연소후 포획 위주로 많은 연구가 진행되어 왔다, 하지만 최근 고유가 시장이 형성되면서 석탄화력 발전 및 복합가스발전(IGCC)에 필요한 연소전 탈탄소화($H_2/CO_2$ 가스로부터 $CO_2$ 회수) 연구에 산업적 관심이 급상승되고 있다. 특히, 연소전 탈탄소화 과정에서는 높은 자체압력(약 2.5 - 5.0MPa)과 비교적 높은 농도의 $CO_2$(약 40%의)가 발생되기 때문에, 연소전 탈탄소화는 가스하이드레이트 형성/분해 원리가 가장 잘 적용될 수 있는 기술이라 할 수 있다. 본 연구에서는 가스 하이드레이트 형성원리를 이용하여 정온 정압 조건에서 $CO_2/H_2$ 하이드레이트를 제조하였으며 특히, 하이드레이트 형성 촉진제인 THF(Tetrahydrofuran)와 TBAB(Tetra-n-butyl ammonium bromide)를 첨가하여 각각 0.5, 1, 3mol% 농도에 따른 상평형 및 속도론 실험을 수행 하였다. 또한 라만 분석을 통하여 $CO_2$ 회수 분리에 대한 연구도 병행하였다. 이러한 연구는 연소전 탈탄소화 기술에서의 $CO_2$ 회수 분리에 대한 핵심 연구임과 동시에 탄소배출권 규제에 실질적인 기여를 할 수 있을 것으로 사료된다.

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Synthesis of Polystyrene-b-Poly(ethylene oxide)-b-Polylactide Copolymers via Sequential Anionic and Ring-Opening Polymerizations (순차적 음이온 및 개환중합반응을 통한 폴리스티렌-폴리에틸렌옥사이드-폴리락티드 블록공증합체의 합성)

  • Song, Jie;Cho, Byoung-Ki
    • Polymer(Korea)
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    • v.33 no.5
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    • pp.458-462
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    • 2009
  • We have synthesized ABC linear triblock copolymers, i.e., polystyrene-b-poly(ethylene oxide)-b-polylactide, via sequential anionic and ring-opening polymerizations. In the first anionic polymerization step, styrene was polymerized in cyclohexane using sec-butyllithium as the initiator. Poly (styryl) lithium was hydroxylated by the addition of ethylene oxide, and the subsequent protonation with methanolic HCl. In the second anionic polymerization step, potassium naphthalenide was used to deprotonate the hydroxyl group of the PS to generate the macroinitiator of PS-$O^-K^+$. Polymerization of ethylene oxide was performed in THF and terminated with methanolic HCl. In the ring-opening polymerization step, the PS-b-PEO-$AlEt_2$ macroinitiator was prepared from an $AlEt_3$/pyridine system in THF, and the polymerization of lactide was performed at $90^{\circ}C$. The resulting block copolymers showed well-defined molecular weights and narrow molecular weight distributions as revealed by $^1H$- NMR spectroscopy and gel permeation chromatography (GPC).

Photochromic Spiropyran-Functionalized Organic-Inorganic Hybrid Mesoporous Silica for Optochemical Gas Sensing (광화학적 가스 센싱을 위한 광변색 스피로피란 개질된 유기-무기 하이브리드 메조포러스 실리카)

  • Park, Sung Soo;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.17 no.4
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    • pp.141-148
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    • 2016
  • In this work, mesoporous silica (SBA-15) was synthesized via self-assembly process using triblock copolymer ($PEO_{20}PPO_{70}PEO_{20}$, P123) as template and tetraethyl orthosilicate (TEOS) as silica source under acidic condition. SBA-15 have high surface area ($704m^2g^{-1}$) and uniform pore size (8.4 nm) with well-ordered hexagonal mesostructure. Spiropyran-functionalized SBA-15 (Spiropyran-SBA-15) was synthesized via post-synthesis process using 3-(triethoxysilyl)propyl isocyanate (TESPI) and 1-(2-Hydroxyethyl)-3,3-dimethy-lindolino-6'-nitrobenzopyrylo-spiran (HDINS). Spiropyran-SBA-15 was produced with hexagonal array of mesopores without damage of mesostructre. Surface area and pore size of Spiropyran-SBA-15 were $651m^2g^{-1}$ and 8.0 nm, respectively. Optochemical properties of Spiropyran-SBA-15 was studied with chemical vapors such as EtOH, THF, $CHCl_3$, Acetone and HCl. Main peaks of photofluorescence of Spiropyran-SBA-15 exhibited blue shift in the range of 603.4~592.1 nm after exposure under EtOH, THF, $CHCl_3$, and Acetone vapors. Normalized peak intensities decreased in the range of 0.8~0.3. The main peak of photofluorescence of Spiropyran-SBA-15 showed significant blue shift of 592.1 nm after exposure under HCl vapor, while normalized peak intensity decreased to 0.1.

Solvent-Polymer Interactions for Stable Non-Aqueous Graphene Dispersions in the Presence of PVK-b-PVP Block Copolymer (PVK-b-PVP 블록 공중합체의 존재 하에서 안정한 비 수계 그래핀 분산액을 위한 용매-고분자 상호작용에 관한 연구)

  • Park, Kyung Tae;Perumal, Suguna;Lee, Hyang Moo;Kim, Young Hyun;Cheong, In Woo
    • Journal of Adhesion and Interface
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    • v.18 no.3
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    • pp.109-117
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    • 2017
  • Poly(N-vinyl carbazole) (PVK) homopolymer, poly(4-vinylpyridine) (PVP) homopolymer, and PVK-b-PVP block copolymer were synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization and the polymers were used to prepare non-aqueous graphene dispersions with four different solvents, ethanol, N-methyl-2-pyrrolidone (NMP), dichloromethane (DCM), and tetrahydrofuran (THF). $^1H-$ and $^{13}C-NMR$ spectroscopy, size exclusion chromatography (SEC), and differential scanning calorimetry (DSC) were carried out to confirm the chemical structure of the polymers. Stability of graphene dispersions was measured by on-line turbidity measurement. Time-dependent Turbiscan Stability Index (TSI) values were interpreted in terms of surface tension (${\sigma}$) and solubility parameter (${\delta}$) among solvents, polymers, and graphene. It was confirmed that the solubilities of polymer and surface tension between solvent and graphene affected the dispersion stability of graphene. PVK-b-PVP block copolymer could effectively maintain the low TSI values of graphene dispersions in ethanol and THF, which have been known as poor solvents for graphene dispersions. It can also be noted that DCM shows good dispersion stability comparable to NMP, which has been known as the best solvent for graphene dispersion.

Production of PBT(polybutylene terephthalate) Oligomer from Recycled PET(polyethylene terephthalate) (재활용 PET(polyethylene terephthalate)를 이용한 PBT(polybutylene terephthalate) 올리고머 제조)

  • Cho, Minjeong;Yang, Jeongin;Noh, Seunghyun;Joe, Hongjae;Han, Myungwan
    • Korean Chemical Engineering Research
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    • v.54 no.4
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    • pp.437-442
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    • 2016
  • A new route for PBT (Poly butylene terephthalate) production from recycled PET (Poly ethylene terephthalate) has been explored. The route consists of glycolysis of PET (Poly ethylene terephthalate) wastes using 1,4-butandiol into BHBT oligomers and polycondensation of the oligomers into PBT oligomer. This process uses post-consumer or post-industrial recycled PET and converts it into high-end PBT type engineering thermoplastic via a chemical recycling process. Zink acetate was used as a catalyst for both glycolysis and polycondensation. Two types of reactor for the glycolysis, batch and semi-batch reactor, were investigated and their performances were compared. Semi-batch reactor removes ethylene glycol (EG) and THF (tetrahydrofuran) during the reaction. Amounts of EG and THF generated during the glycolysis reaction were measured and used as criteria for the reactor performance. Performance of semi-batch reactor was shown to be better than that of batch reactor. Optimum reaction condition for the semi-batch reactor was BD/PET ratio of 4, and reaction temperature of $220^{\circ}C$, giving high EG yield (max 91%) and low production of THF. In addition, it was confirmed that the molecular weight of PBT oligomer increases in accordance with the progress of the polycondensation reaction.

Quantitative Extraction Analysis of Brominated Flame Retardant Substances Using Supercritical-Fluid Method for Environmental Assessment (초임계추출법을 이용한 브롬계 난연제 화합물 환경성 평가 추출효율 분석 연구)

  • Oh, Min-Kyung;Yoon, Sang-Hwa;Lee, Young-Kwan;Han, Jae-Sung;Won, Sung-Ho;Nam, Jae-Do
    • Polymer(Korea)
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    • v.32 no.1
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    • pp.13-18
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    • 2008
  • For the evaluation of brominated flame retardants included in polymeric electronic devices, we investigated the extraction methods and solvent systems for four different types of polymers of PC (polycarbonate), PP (polyropylene), PET (poly(ethylene terephthalate)) and PBT (poly(butylene terephthalate)) using different solvent systems of hexane/acetone, THF, toluene, and THF/toluene. In order to compare the extraction efficiency of different methods and solvent systems, the deca-BDE (decabromo diphenyl ether) flame retardant was included in PC, PP, PET and PBT systems and subsequently extracted by soxhlet, ultrasonic, accelerated solvent, microwave and supercritical fluid extraction methods. The amount of the extracted flame retardant was monitored to evaluate the extraction efficiency. The ultrasonic extraction method was found not to be acceptable as an extraction method for the polymer systems mainly due to a low salvation efficiency of the organic solvents. Soxhlet, accelerated solvent and microwave extraction methods exhibited over 80% of extraction efficiency for toluene. The supercritical fluid extraction method, which has been used as an extraction method for flame retardants in polymers, showed the extraction efficiencies of ca. 100% for PC and PP in the optimal extraction conditions of $60^{\circ}C$ and 120 bar.