• Title/Summary/Keyword: Maleic acid

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Detection of Long Alkyl Esters of Succinic and Maleic Acid Using TLC-MALDI-MS

  • Kim, Hin-Hee;Han, Sang-Pil;Kim, Jeong-Kwon;Kim, Yeong-Joon
    • Bulletin of the Korean Chemical Society
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    • 제32권3호
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    • pp.915-920
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    • 2011
  • Four esters of succinic and maleic acid were synthesized, separated by thin-layer chromatography (TLC), and identified using matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). A comparison of matrix materials showed that 2,6-dihydroxybenzoic acid (2,6-DHB) yielded a greater ionization efficiency than 2,5-DHB prior to TLC separation. The location of each ester sample on the TLC plate was estimated by comparing the developed plate with a duplicate plate that had been visualized by immersion in a $KMnO_4$ solution. Generally, mass spectra obtained from the $KMnO_4$-visualized plate were relatively poor. Reproducible mass spectra with high peak abundance were difficult to obtain using the 2,6-DHB matrix from crude synthetic esters extracted from the TLC plates. Significant improvements in both reproducibility and sensitivity were realized by using pencil lead as the MALDI matrix. The current methodology will be beneficial to organic chemists since it can provide a guideline for simple and rapid characterization of small organic compounds.

Selective Esterification of N-Benzyl-L-aspartic Acid. (I). Some Modified Methods for the Preparation of N-Benzylaspartic Anhydride Hydrobromide

  • Lee Chal-Ho;Chai, Kyu-Yun;Lee, Man-Koo;Chung, Bong-Young
    • Bulletin of the Korean Chemical Society
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    • 제8권6호
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    • pp.457-459
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    • 1987
  • Racemic N-benzylaspartic acid (4) was prepared from maleic anhydride and used to modify and develop some efficient methods for the preparation of N-benzylaspartic anhydride hydrobromide (5). Thus, successive treatment of the compound 4 with 30% HBr in acetic acid and acetic anhydride afforded the title compound 5 in 75% yield. From this compound 5, ${\alpha}$-benzyl and ${\alpha}$-methyl N-benzylaspartates were also prepared.

含할로겐 異元素環化合物에 關한 硏究 (第2報) 풀퍼릴誘導體-마레인酸無水物 附加物의 할로겐化反應 (Halogen Containing Heterocyclic Compounds (Part Ⅱ) Halogenation of Furfuryl Derivatives-Maleic Anhydride Adduct)

  • 김유선;김정희
    • 대한화학회지
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    • 제9권2호
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    • pp.88-95
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    • 1965
  • 퓨란, 醋酸풀퍼릴, 풀퍼릴알코올과 마레인酸無水物을 에틸 에테르 存在下에서 附加反應시켜 exo附加物을 만들고 이 化合物들에 對한 臭素化反應을 물 存在下에서 行한 바 各各 모노부롬化락톤 및 디브롬酸을 生成하였으며 락톤의 生成收率은 轉位된 carbonium ion에 對한 carboxylic acid의 反應기여(participation)에 依하여 決定되면 化合物 自體의 立體條件(steric requirement)이 그 기여에 영향을 준다는 것을 究明하였다. 퓨란附加物을 有機溶媒(四鹽化炭素, 메틸렌크로라이드)存在下에서 臭素化反應하면 二臭化物이 生成하고 光線 存在下에서 鹽素化反應하면 四鹽化反應物이 生成됨을 究明하였다. 各 化合物의 合成方式 및 反應過程에 關하여 論及하였다.

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실리카 화합물을 함유한 PVA/PSSA-MA 전해질 막의 제조 및 특성과 연료전지로의 응용 (Preparation and Characterization of PVA/PSSA-MA Electrolyte Membranes Containing Silica Compounds for Fuel Cell Application)

  • 변홍식;김대훈;이병성;이보성;윤석원;임지원
    • 멤브레인
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    • 제18권4호
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    • pp.336-344
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    • 2008
  • 본 연구에서는 Poly(vinyl alcohol) (PVA)을 주쇄부(base polymer)로 하여 화학적 가교를 실시하기 위하여 Poly(styrene sulfonic acid-co-maleic acid) (PSSA-MA)를 첨가하고, 실리카와 술폰산기를 함유한 3-(trihydroxysilyl)-1-propanesulfonic acid (THS-PSA)의 함량변화와 열 가교온도 변화를 통하여 직접 메탄을 연료전지(DMFC)에 적용하기 위한 고분자 전해질 막 소재에 관한 연구를 실시하였다. 제조된 막을 Nafion 115와 함께 비교하기 위하여 동일한 조건에서 함수율, 열 중량 분석(TGA), 이온교환용량, 이온전도도 및 메탄올 투과도를 실시하였다. 실험을 통하여 THS-PSA의 함량과 열 가교 온도변화에 따라서 메탄올 투과도가 $10^{-6}$에서 $10^{-8}\;cm^2/s$로 감소된 결과를 얻었으며, 이온전도도는 $10^{-3}$에서 $10^{-2}\;S{\cdot}cm^{-1}$으로 향상되어 Nafion 115보다 우수한 결과를 나타내었다.

이온교환용량이 막 결합형 축전식 탈염공정에서 염 제거율에 미치는 영향 (Effect of Ion Exchange Capacity on Salt Removal Rate in Membrane Capacitive Deionization Process)

  • 윤원섭;정성일;임지원
    • 멤브레인
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    • 제28권5호
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    • pp.332-339
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    • 2018
  • 막 결합형 축전식 탈염공정에서 이온교환막의 이온교환용량이 염 제거 효율에 미치는 영향을 알아보기 위해 poly(vinyl alcohol)(PVA) 수용성 고분자에 sulfosuccinic acid (SSA) 가교제를 첨가하고 poly(4-styrene sulfonic acid-co-maleic acid)(PSSA_MA)를 PVA 질량대비 10, 50, 90 wt%로 달리 첨가하여 제조하였다. PSSA_MA의 함량이 증가함에 따라 함수율과 이온교환용량이 증가하는 경향을 나타내었으며 막 결합형 축전식 탈염공정에서 염 제거 효율도 상승되었다. PSSA_MA 90 wt%, 100 mg/L NaCl의 공급액과 유속 15 mL/min에서 흡착 1.4 V/5분의 조건에서 가장 높은 65.5%의 염 제거 효율을 나타내었다.

PVDF 중공사막의 표면친수화 후 PVA/PAM 용액의 코팅을 통한 복합막제조와 이의 물-에탄올계의 투과증발 분리 (Preparation of Composite Membranes Via PVA/PAM Solution Coating onto Hydrophilized PVDF Hollow Fiber Membrane and Their Pervaporation Separation of Water-ethanol Mixture)

  • 김지선;박채영;박헌휘;서창희;임지원
    • 멤브레인
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    • 제23권4호
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    • pp.312-318
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    • 2013
  • Poly vinylidene fluoride (PVDF) 중공사막을 polyethylenimine (PEI)와 p-xylylene dichloride (XDC)를 이용해 친수화 시킨 후 poly(vinyl alcohol) (PVA)과 가교제인 poly(acrylic acid-co-maleic acid) (PAM) 혼합용액을 코팅하여 막을 제조하였다. 중공사막 표면의 코팅여부는 scanning electron microscope (SEM)을 통해 관찰하였으며, 막의 특성평가를 위해 물/에탄올 혼합액에 대한 투과증발 실험을 수행하였다. 공급액 조성은 90 wt% 에탄올 수용액을 사용하였으며, 가교제 농도, 공급액과 반응온도 변화에 따른 투과도 및 선택도를 측정하였다. 투과도는 반응온도 $100^{\circ}C$, PAM 농도 3 wt%, 공급액온도 $70^{\circ}C$에서 $1,480g/m^2hr$, 그리고 선택도는 반응온도 $100^{\circ}C$, PAM 농도 15 wt%, 공급액온도 $25^{\circ}C$에서 ${\alpha}_{W/E}=82$의 결과를 얻을 수 있었다.

폴리(비닐 알코올)과 폴리(아크릴산-말레산) 공중합체의 블렌드 필름 (I) : 열적-기계적 성질 및 가스 투과도 (Blend Films of Poly(acrylic acid-co-maleic acid) with Poly(vinyl alcohol) (I) : Thermo-mechanical Properties and Gas Permeability)

  • 함신균;정민혜;장진해
    • 폴리머
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    • 제30권4호
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    • pp.298-304
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    • 2006
  • 폴리(비닐 알코올)(PVA)과 폴리(아크릴산-말레산) 공중합체(PAM) 혼합물은 증류수를 사용하여 용액 블렌딩으로 제조하였다. 제조된 블렌드 필름은 다양한 PAM 농도에 따라 변하는 열적-기계적 성질, 모폴로지 및 가스 투과도를 측정하였다. 블렌드 필름의 전이온도 ($T_g$$T_m$)는 PAM의 농도에 관계없이 일정한 값을 가졌다. 그러나, 용융 엔탈피 $({\Delta}H_m)$와 초기 분해온도 $({T_D}^i)$는 PAM 함량이 증가됨에 따라 서서히 감소하였다. 인장 강도와 초기 인장 탄성률은 PAM 함량이 12 wt% 일 때 최대값을 나타냈으며, PAM 함량이 15 wt% 가 되면 오히려 감소하였다. PVA/PAM 필름의 가스 투파도는 PVA 블렌드 용액을 폴리 (에틸렌 테레프탈레이트)(PET)와 이축 연신한 폴리프로필렌(BOPP) 필름 위에 코팅하여 측정하였다. 산소 투과도 $(O_2\;TR)$는 PAM의 함량이 $0{\sim}12wt%$ 까지 증가됨에 따라 코팅된 PET 와 BOPP 필름 모두 일정하게 감소하였지만, 수증기 투과도 (MVTR)는 첨가된 PAM 농도에 무관하게 일정하였다.

경화된 상아질의 접합 양상에 관한 주사전자현미경적 연구 (A SCANNING ELECTRON MICROSCOPIC STUDY OF BONDING ASPECTS TO THE SCLEROTIC DENTIN)

  • 이린;이형일;이광원;손호현
    • Restorative Dentistry and Endodontics
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    • 제22권1호
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    • pp.228-243
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    • 1997
  • The changes of microstructures, morphology of sclerotic dentin and bonding aspects generated by an adhesive resin was investigated. Incisors and premolars showing natural cervical abrasions were collected and conditioned with 10 % phosphoric acid or 10 % maleic acid. The sclerotic dentin specimens were then rinsed and blot-dried and applied with dentin adhesive (All Bond 2) to the conditioned dentin surface. To examine the morphologic change of the sclerotic dentin specimen after etching and bonding procedure, the treated specimens were examined by SEM. To analyze the chemical composition of sclerotic dentin and crystals occluding dentinal tubules, the sclerotic dentin specimen was powdered and examined with X-ray Diffractometer. To investigate the Ca/P weight percent ratio within the dentinal tubules, the sclerotic dentin specimen was fractured perpendicularly to the long axis of the tooth from the center of cervical abrasion lesion and then examined with EDX(Energy Dispersive X-ray) microanalyzer. The results were as follows : 1. The increased width of peritubular dentin and the depositions of the irregular amorphous materials within the dentinal tubules were showed in the sclerotic dentin specimens. 2. After the treatment of sclerotic dentin specimen with 10 % phosphoric acid or 10 % maleic acid, the lateral side of tubules rather than cross-sectional tubule openings was showed exclusively at the incisal and gingival incline of the specimens. 3. After the treatment of sclerotic dentin specimen with 10 % phosphoric acid or 10 % maleic acid, the hybrid layer was not formed evidently and the resin tag was not formed or shortly penetrated into the tubules with the thinner diameter. 4. According to the results of XRD analysis of the sclerotic dentin specimen, Hydroxyapatite and Octacalcium phosphate were predominent, however, Whitlockite crystals were rare. 5. The mean Ca/P weight percent ratio analysed from 5 fractured sclerotic dentin specimens was $2.322{\pm}0.170$ at the intertubular dentin, $1.826{\pm}0.051$ within the dentinal tubule.

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Nd : YAG 레이저를 조사한 상아질 표면변화에 관한 주사전자현미경적 연구 (THE SEM STUDY ABOUT THE MORPHOLOGICAL CHANGES OF THE DENTINAL SURFACE IRRADIATED WITH Nd : YAG LASER)

  • 임성삼;윤수한;박동성
    • Restorative Dentistry and Endodontics
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    • 제22권1호
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    • pp.479-489
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    • 1997
  • The purpose of this study was to evaluate the effect of the Nd : YAG laser on the tooth hypersensitivity by the observation of the morphological changes of the dentinal surface irradiated with Nd : YAG laser by use of SEM. In 40 mandibular and maxillary molars without any carious lesion or restoration, severe attrition and abrasion, Enamel was removed with fine grit diamond bur and exposed dentinal surfaces were polished with Soflex discs. In control group (10 teeth), exposed dentinal surfaces were acid-etched with 10 % Maleic acid for 15 seconds. In the experimental group 1 (10 teeth), acid-etched dentinal surfaces with 10% Maleic acid were prepared by Nd : YAG laser (6 watts power, 1 psi water, 18 psi air) for 2 minutes. In the experimental group 2 (10 teeth), exposed dentinal surfaces were irradiated with Nd: YAG laser (10 watts power, 3 psi water, 10 psi air) until the painted black stains on the dentinal surfaces were completely removed. In the experimental group 3 (10 teeth). dentinal surfaces were prepared with Nd : YAG laser (6 watts power, 1 psi water, 18 psi air) until the painted black stanins on them were completely removed and then the irradiated dentinal surfaces were acid-etched with 10 % Maleic acid for 15 seconds. The specimens were routinely processed and observed with scanning electron microscope. The results were as follows : 1. In the irradiated dentinal surfaces, the characteristics of the melting and recrystalization on the dentinal surfaces were observed. Compared with the results in the control group, we could observe that in the irradiated dentinal surfaces, the aperture of the dentinal tubules were reduced and there were more debris obstructing the dentinal tubules. 2. In the irradiated dentinal surfaces, crater structures were commonly present and in the crater bottoms, there were a lot of bead like melted dentin structures, which had the ruptured opening in the center of them. 3. The melted dentins and cracks in the smear layer were less frequently observed in the irradiated dentinal surfaces using copious cooling water than in the irradiated dentinal surfaces using scare cooling water.

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Preparation of Ion Exchange Membranes for Fuel Cell Based on Crosslinked Poly(vinyl alcohol) with Poly(acrylic acid-co-maleic acid)

  • Kim, Dae-Sik;Park, Ho-Bum;Lee, Chang-Hyun;Lee, Young-Moo;Moon, Go-Young;Nam, Sang-Yong;Hwang, Ho-Sang;Yun, Tae-II;Rhim, Ji-Won
    • Macromolecular Research
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    • 제13권4호
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    • pp.314-320
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    • 2005
  • Crosslinked poly(vinyl alcohol) (PVA) membranes were prepared at various crosslinking temperatures using poly(acrylic acid-co-maleic acid) (PAM) containing different PAM contents. The thermal properties of these PVA/PAM membranes prepared at various reaction temperatures were characterized using differential scanning calorimetry (DSC). The proton conductivity and methanol permeability of PVA/PAM membranes were then investigated as PAM content was varied from 3 to 13 wt%. It was found that the proton and methanol transport were dependent on PAM content in their function both as crosslinking agent and as donor of hydrophilic -COOH groups. Both these properties decreased monotonously with increasing PAM concentration. The proton conductivities of these PVA/PAM membranes were in the range from $10^{-3}\;to\;10^{-2}S/cm$ and the methanol permeabilities from $10^{-7}\;to\;10^{-6}cm^{2}/sec$. In addition, the effect of operating temperature up to $80^{\circ}C$ on ion conductivity was examined for three selected membranes: 7, 9 and 11 wt% PAM membranes. Ion conductivity increased with increasing operating temperature and showed and S/cm at $80^{\circ}C$, respectively. The effects of crosslinking and ionomer group concentration were also examined in terms of water content, ion exchange capacity (IEC), and fixed ion concentration. In addition, the number of water molecules per ionomer site was calculated using both water contents and IEC values. With overall consideration for all the properties measured in this study, $7{\sim}9\;wt%$ PAM membrane prepared at $140^{\circ}C$ exhibited the best performance. These characteristics of PVA/PAM membranes are desirable in applications related to the direct methanol fuel cell (DMFC).