• Title/Summary/Keyword: Condensation Reaction

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Synthesis of Aliphatic Ester-Carbonate Copolymer (지방족 에스터-카보네이트 공중합체의 합성)

  • Kim, Dong-Kook;Kim, Ki-Seab;Chang, Young-Wook
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.970-976
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    • 1996
  • An ester-carbonate copolymer was synthesized, in which carbonate was inserted into a biodegradable aliphatic polyester, poly(butylene succinate) (PBS), to modify its mechanical properties. The synthesis was carried out by condensation reactions in two steps. In the first step, oligo(butylene succinate) was prepared by the reaction of succinic acid with 1,4-butanediol (BD). In the second step, it was reacted with oligohexamethylenecarbonate diol (OHMCG) to prepare the ester-carbonate copolymer. Titanium(IV) isopropoxide (TIP) was used as a catalyst for the reaction. The structure of the copolymer was confirmed by FT-IR and $^1H$-NMR and the thermal behavior and mechanical properties were investigated by differential scanning calorimetry (DSC) and universal testing machine (UTM), respectively. It was found that optimum amount of the catalyst for the formation of high molecular weight copolymer was 1wt% for succinic acid. When the BD:OHMCG is in the range 149:1~249:1, the copolymer with high viscosity was obtained. As the OHMCG content was increased, melting temperature ($T_m$) of the copolymer was decreased. When BD:OHMCG is 149:1, the copolymer showed a increase in ultimate strain by two times and the slight decrease in modulus compared to those of PBS.

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Synthesis of Oleic Acid Esters containing Thiocarbamate Group as Anti-wear Additives (티오카바메이트 그룹을 함유하는 올레인산 에스테르계 내마모제의 합성)

  • Hwang, Do-Huak;Kim, Young-Wun;Chung, Keunwo;Yang, Tae-Kyun
    • Applied Chemistry for Engineering
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    • v.19 no.1
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    • pp.51-58
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    • 2008
  • A series of oleic acid esters containing mercaptobenzothiazole and dialkylenedithiocarbamate, which are potential environmentally friendly lubricating grease additives, were synthesized as 90% yield through several method such as nucleophilic substitution of dialkyl amine and carbon disulfide, reduction reaction, and condensation reaction. The structures of the additives were confirmed by $^1H$-NMR, FT-IR and EA analysis. The additives (1 wt%) were soluble in 100 N BO except C4-DTC-OE and soluble in soybean oil. The tribological properties as lubricating additives in 100 N BO were evaluated using 4-ball tester and the results showed as follows: Bz-thia-OE < C4-DTC-OE < Pyrro-DTC-OE < C8-DTC-OE. Whereas, the 4-ball anti-wear properties were not shown in soybean oil.

Reactivity of SO2 Catalytic Reduction over Sn-Zr Based Catalyst under High Pressure Condition (고압조건에서 Sn-Zr계 촉매상에서 SO2 촉매환원 반응특성)

  • Park, Jung Yun;Park, No-Kuk;Lee, Tae Jin;Baek, Jeom-In;Ryu, Chong Kul
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.316-321
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    • 2010
  • The $SO_2$ catalytic reduction was carried out under the condition of high pressure in this study. Sn-Zr based oxide and CO were used as the catalyst and reducing agent for the reduction of $SO_2$ to element sulfur, respectively. In order to compare the reactivity with the pressure on the catalytic process, the reactivity tests were performed under the conditions of atmospheric pressure and 20 atm. $SO_2$ conversion, the element sulfur yield and COS selectivity were also compared with changing the reaction temperature, $CO/SO_2$ mole ratio and the space velocity(GHSV). $SO_2$ conversion increased with increasing temperature and $CO/SO_2$ mole ratio under the condition of atmospheric pressure and element sulfur yield decreased due to the production of COS by the series reaction of CO and the produced sulfur. However, high $SO_2$ conversion and high element sulfur were obtained under the condition of 20 atm. It was concluded that COS decreased due to the condensation of the produced element sulfur under the condition of high pressure. Therefore, the high sulfur yield for $SO_2$ catalytic reduction could be profitably obtained under the condition of high pressure.

Soluble Polyimide Binder for Silicon Electrodes in Lithium Secondary Batteries (리튬이차전지 실리콘 전극용 용해성 폴리이미드 바인더)

  • Song, Danoh;Lee, Seung Hyun;Kim, Kyuman;Ryou, Myung-Hyun;Park, Won Ho;Lee, Yong Min
    • Applied Chemistry for Engineering
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    • v.26 no.6
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    • pp.674-680
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    • 2015
  • A solvent-soluble polyimide (PI) polymeric binder was synthesized by a two-step reaction for silicon (Si) anodes for lithium-ion batteries. Polyamic acid was first prepared through ring opening between two monomers, bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride (BCDA) and 4,4-oxydianiline (ODA), followed by condensation reaction. Using the synthesized PI polymeric binder (molecular weight = ~10,945), the coating slurry was then prepared and Si anode was fabricated. For the control system, Si anode based on polyvinylidene fluoride (PVDF, molecular weight = ~350,000) having the same constituent ratio was prepared. During precycling, PI polymeric binder revealed much improved discharge capacity ($2,167mAh\;g^{-1}$) compared to that of using PVDF polymeric binder ($1,740mAh\;g^{-1}$), while the Coulombic efficiency of two systems were similar. PI polymeric binder improved the cycle retention ability during cycles compared to that of using PVDF, which is attributed to an improved adhesion property inside Si anode diminishing the dimensional stress during Si volume changes. The adhesion property of each polymeric binder in Si anode was confirmed by surface and interfacial cutting analysis system (SAICAS) (Si anode based on PI polymeric binder = $0.217kN\;m^{-1}$ and Si anode based on PVDF polymeric binder = $0.185kN\;m^{-1}$).

Development of Environmental-friendly N-Acyl Taurates Manufacturing Process and Evaluation of their Physical Properties (N-Acyl Taurates의 환경친화적인 제조공정 개발 및 이의 물성 연구)

  • Park, Ji Na;Song, Ah Ram;Jeong, Yong Wu;Bae, Jae Heum;Ji, Heung Jin;Lim, Ho
    • Clean Technology
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    • v.11 no.4
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    • pp.195-204
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    • 2005
  • A new condensation process for manufacturing N-acyl taurates which generates less pollutant and produces more than 60 % yield in comparison with the conventional process has been developed in this work. Its optimum process conditions are at $210{\sim}230^{\circ}C$ of reaction temperature and 6 ~ 9 hour of reaction time when Parasol 123 of petroleum refired oil is employed as process solvent and mixed catalysts of sulfonic acid and phosphoric acid are utilized as process catalyst. And the qualities of N-acyl taurates produced by this new process are similar to or better than those of imported product judging from their acid value, amine value and color. Thus, it can be said that the newly developed process for manufacturing N-acyl taurates in this work is better than the conventional process. The physical properties of N-acyl taurates produced in this work such as surface tension, foaming power, foaming stability, hard water stability, and emulsifying power etc. were compared with those of commercially available anionic surfactants. And the experimental results show that N-acyl taurates shows good physical properties and that they can be alternative to conventional anionic surfactants.

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The Synthesis and Evaluation of Antihypertensive 4-(${\beta}$-Guanidinoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol (혈압강하제인 4-${\beta}$-Guanidinoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol의 합성 및 평가)

  • Jack C. Kim;Lee Euk-suk;Charles C. Chang;Norman J. Doorenbos
    • Journal of the Korean Chemical Society
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    • v.19 no.3
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    • pp.174-178
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    • 1975
  • The intermediate, 17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(Ⅸ) required for the synthesis of 4-(${\beta}$-guanidinoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(V) was obtained through a reaction of 17${\alpha}$-methyl-3,5-seco-4-norandrostan-17${\beta}$-ol-5-on-3-oic acid(VI) with ammonium hydroxide followed by two reductions(platinum dioxide with hydrogen and lithium aluminium hydride). Condensation of Ⅸ with chloroacetonitrile under anhydrous condition, followed by reduction of the nitrile with lithium aluminium hydride gave 4-(${\beta}$-aminoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(XI). The reaction of XI with 2-methyl-2-thiopseudourea or 3,5-dimethylpyrazole-1-carboxamidine, or cyanamide provided the title compound, V. Relaxation of the nictitating membrane, in the absence of mydriasis, is considered to be evidence of adrenergic neurone blockade. Thus the test compound(V) resembles that of the classical adrenergic neurone blocking agents.

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Synthesis of Diketo Copper(II) Complex and Its Binding toward Calf Thymus DNA (CTDNA) (이케토 구리(II) 착물의 합성 및 송아지 Thymus DNA(CTDNA)와의 상호작용)

  • Tak, Aijaz Ahmad;Arjmand, Farukh
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.177-182
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    • 2011
  • A diketo-type ligand was synthesized by the Knoevenagel condensation reaction of thiophene-2-aldehyde with acetylacetone, subsequently its transition metal complexes with Cu(II), Ni(II), and Co(II) chlorides were also prepared. All the complexes were characterized by various physico-chemical methods. The molar conductivity data reveals ionic nature for the complexes. The electronic spectrum and the EPR values suggest square planar geometry for the Cu(II) ion. Interaction of the Cu(II) complex with CTDNA (calf thymus DNA) was studied by absorption spectral method and cyclic voltammetry. The $k_{obs}$ values versus [DNA] gave a linear plot suggesting psuedo-first order reaction kinetics. The cyclic voltammogram of the Cu(II) complex reveals a quasi-reversible wave attributed to Cu(II)/Cu(I) redox couple for one electron transfer with $E_{1/2}$ values -0.240 V and -0.194 V. respectively. On addition of CTDNA, there is a shift in the $E_{1/2}$ values 168 mV and 18 mV respectively and decrease in Ep values. The shift in $E_{1/2}$ values in the presence of CTDNA suggests strong binding of Cu(II) complex to the CTDNA.

Preparation of PMSQ/TiO2 Composite Fine Powder by Sol-Gel Process (Sol-Gel Process를 이용한 PMSQ/TiO2 복합 미립자의 합성)

  • Lee, Dong Hyun;Koo, Sangman
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.634-638
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    • 1998
  • Monodisperse, spherical $PMSQ/TiO_2$ composite fine powders were prepared by modified sol-gel process where 300 nm $TiO_2$ fine powders were used as seed particles for hetero-condensation with hydrolyzed MTMS (Methyltrimethoxysilane). The reaction was carried out under $N_2$ atmosphere at ambient temperature using $NH_3$ as a catalyst. Methanol was used as a solvent. Powder was obtained by the filtration of the solution with a glass filter and washing with acetone. The stirring rate, reaction temperature, $[H_2O]/[MTMS]$ and $[MTMS]/[TiO_2]$ ratio were varied to investigate shapes and sizes of particles. Monodisperse particles of $1-2{\mu}m$ diameter were obtained with [MTMS]=0.2 M, $[NH_3]=0.6M$, $[H_2O]/[MTMS]=100$, $[MTMS]/[TiO_2]=10-50$ at ambient temperature with mild stirring condition. These composite particles had a contact angle of almost 180 degree contact angle with water, which proves their excellent hydrophobicity. The study of UV absorption spectra showed that they have UV protecting effect.

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Preparation and Characterization of Pitch based Coke with Anisotropic Microstructure Derived from Pyrolysis Fuel Oil (열분해유 유래 피치로부터 이방성 미세구조 코크스 제조 및 특성 평가)

  • Cho, Jong Hoon;Kim, Ji Hong;Lee, Young-Seak;Im, Ji Sun;Kang, Seok Chang
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.640-646
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    • 2021
  • In this study, pitch was synthesized using pyrolysis fuel oil (PFO). Coke with mesophase microstructure was then prepared from the synthesized pitch and its properties were evaluated. Pitch was synthesized by poly-condensation reaction, which is an endothermic reaction at a temperature above 400 ℃ because the PFO was mainly composed of molecules with two to three aromatic rings. The Coke reactor was composed of the pretreatment reactor, preheater for applying heat energy, and coke drum for inducing microstructure of coke. Coke was prepared from synthesized pitch by controlling the temperature of the preheater to 400~490 ℃, and properties were evaluated by polarization microscope, XRD and Raman spectroscopy. The coke prepared at a preheater temperature of 460 ℃ identified flow anisotropic microstructure, and the electrical conductivity was 72.0 S/cm due to high crystallinity. And the flow anisotropic coke showed approximately 2.2 times higher electrical conductivity than that of Super-P, a conductive carbon material.

Reaction Mechanism and Curing Characteristics of Chicken Feather-Based Adhesives and Adhesive Properties of Medium-Density Fiberboard Bonded with the Adhesive Resins (닭털로 제조한 접착제의 반응기작 및 경화 특성과 이를 이용하여 제조한 중밀도섬유판의 접착 특성)

  • Yang, In;Park, Dae-Hak;Choi, Won-Sil;Oh, Sei Chang;Ahn, Dong-uk;Han, Gyu-Seong
    • Korean Chemical Engineering Research
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    • v.55 no.3
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    • pp.385-394
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    • 2017
  • In this study, reaction mechanism and curing characteristics of adhesives formulated with NaOH- and $H_2SO_4$-hydrolyzed chicken feather (CF) and formaldehyde-based crosslinkers were investigated by FT-IR and DSC. In addition, adhesive properties and formaldehyde emission of medium-density fiberboards (MDF) applied with the adhesives were measured. CF-based adhesives having a solid content of 40% and over were very viscous at $25^{\circ}C$, but the viscosity reduced to $300{\sim}660m{\cdot}Pa{\cdot}s$ at $50^{\circ}C$. Consequently, the adhesives could be used as a sprayable resin. Through the FT-IR spectra of liquid and cured CF-based adhesives, addition reaction of methylol group and condensation reaction between the functional groups with the use of formaldehyde-based crosslinkers were identified. From the analysis of DSC, it was elucidated for CF-based adhesives to require a higher pressing temperature or longer pressing time comparing to commercial urea-formaldehyde (C-UF) resin. MDF bonded with CF-based adhesives, which was formulated with 5% NaOH-hydrolyzed CF (CF-AK-5%) and PF of formaldehyde to phenol mole ratio of 2.5 (PF-2.5), and pressed for 8 min had higher MOR and IB than those with other CF-based adhesives. MOR and IB of MDF bonded with the CF-based adhesives regardless of formulation type and pressing time were higher than those with C-UF resin. When the values compared with the minimum requirements of KS standard, IB exceeded the KS standard in all formulations and pressing time, but MOR of only MDF bonded with CF-AK-5% and PF-2.5 and pressed for 8 min satisfied the KS standard. What was worse, 24-TS of MDF bonded with all CF-based adhesives did not satisfied the KS standard. However, MOR and 24-TS can be improved by increasing the target density of MDF or the amount of wax emulsion, which is added to improve the water resistance of MDF. Importantly, the use of CF-based adhesives decreased greatly the formaldehyde emission. Based on the results, we reached the conclusion that CF-based adhesives formulated under proper conditions had a potential as a sprayable resin for the production of wood panels.