• Title/Summary/Keyword: cationic catalyst

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Studies on Thermal Stability and Cure Behavior of Epoxy Resins using Electron-beam Curing Technique (전자선 경화를 이용한 에폭시 수지의 열안정성과 경화동력학에 관한 연구)

  • 박수진;허건영;이재락
    • Composites Research
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    • v.15 no.2
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    • pp.40-47
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    • 2002
  • The di-functional epoxy resins, i.e., diglycidylether of bisphenol A(DGEBA) and diglycidylethere of bisphenol F(DGEBF) were initiated by cationic catalyst, i.e., benzylquinoxalinium hexafluoroantimonate(BQH) using electron-beam(EB) technique. And the effect of structure of DGEBA and DGEBF on thermal stabilities and cure behaviors was investigated. According to the experimental results, the decomposed activation energy based on Horowitz-Metzger method was higher in the case of DGEBA, but intergral procedural decomposition temperature(IPDT) of DGEBA was lower than DGEBF. This could be interpreted in terms of high crosslink density resulted from hydroxyl bond of DGEBF backbone. It was confirmed in increasing the hydroxyl band at $7000\;cm^{-1}$ and $5235\;cm^{-1}$ using near-infrared spectroscopy(NIRS).

Photo Catalytic Activity of CNT-TiO2 Nano Composite in Degrading Anionic and Cationic Dyes

  • Kim, Sang-Jin;Im, Ji-Sun;Kang, Phil-Hyun;Kim, Tae-Jin;Lee, Young-Seak
    • Carbon letters
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    • v.9 no.4
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    • pp.294-297
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    • 2008
  • A CNT-$TiO_2$ nano composite was prepared from titanium chloride ($TiCl_4$) via sol-gel process using multi walled carbon nano tube (MWCNT) followed by calcination at $450^{\circ}C$. Spectral analysis revealed that the formed $TiO_2$ resided on the carbon in anatase form. The effect of adsorption was investigated using aqueous solution of methylene blue and procion blue dye. The photochemical reaction of CNT-$TiO_2$ composite in aqueous suspensions was studied under UV illumination in batch process. The reaction was investigated by monitoring the discoloration of the dyes employing UV-Visible spectro-photometeric technique as a function of irradiation time. The catalyst composites were found to be efficient for the photodegradation of the dye.

A study on the polymerization of energetic prepolymer(GDNPF) (에너지를 함유한 선 폴리머인 Prepolymer(GDNPF) 제조 공정 연구)

  • Cheun, Young-Gu;Kim, Jin-Seuk
    • Journal of the Korea Institute of Military Science and Technology
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    • v.8 no.2 s.21
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    • pp.67-76
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    • 2005
  • We synthesized an energetic prepolymer(glycidyl dinitro propyl formal, GDNPF) for plastic-bonded explosive and measured its thermodynamic parameters. Glycidyl dinitro propyl formal(GDNPF) as an energetic monomer was epoxidized from allyl-2,2-dinitro propyl formal which is reacted with dinitro propyl alcohol and excess allyl alcohol, and then energetic polymer of GDNPF was polymerized by cationic ring opening polymerization. Thermodynamic parameters were obtained from the ceiling temperature($T_c$) values of 1 mole monomer at reaction temperature. We varied feed rate of monomer, concentration of initiator and monomer to control molecular weight and polydispersity of prepolymer (GDNPF). The activated monomer polymerization has been executed with precisely controlled feed of GDNPF monomer to reactor in the complex state catalyst generated by $BF_3{\cdot}(C_3H_5)_2$ and 1,4-butanediol in $C_2H_4Cl_2$. Number average molecular weight(Mn), polydispersity(Pd), hydroxy number and glass transition temperature($T_g$) of prepolymer(GDNPF) were $2,500{\sim}3,000,\;1.2{\sim}1,3,\;0.6{\sim}0.8eq/kg\;and\;-20{\sim}-25^{\circ}C$ respectively.

Syntheses of Alternating Head-to-Head Copolymers of Vinyl Ketones and Vinyl Ethers, and Their Properties. Ring-Opening Polymerization of 2,3,6-Trisubstituted-3,4-dihydro-2H-pyrans

  • Lee, Ju-Yeon;Cho, I-Whan
    • Bulletin of the Korean Chemical Society
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    • v.8 no.2
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    • pp.102-105
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    • 1987
  • 2-Methoxy-6-methyl-3,4-dihydro-2H-pyran ($1_a$), 2-ethoxy-3,6-dimethyl-3,4-dihydro-2H-pyran ($1_b$), and 2-ethoxy-3-methyl-6-ethyl-3,4-dihydro-2H-pyran ($1_c$) were prepared by (4 + 2) cycloaddition reaction from the corresponding vinyl ketones and alkyl vinyl ethers. Compounds $1_{a-c}$ were ring-open polymerized by cationic catalyst to obtain alternating head-to-head (H-H) copolymers. For comparison, copolymer of head-to-tail (H-T) was also prepared by free radical copolymerization of the mixture of the corresponding monomers. The H-H copolymer exhibited some differences in its $^1H$ NMR and IR spectra. However, significant differences were showed between the H-H and H-T copolymers in the $^{13}C$ NMR spectra. Also noteworthy was that$T_g$ value of H-H copolymer was higher than that of the corresponding H-T structure. Decomposition temperature of the H-H copolymer was lower than that of the H-T copolymer. All the H-H and H-T copolymers were soluble in common solvents.

Mesoporous Silica Catalysts Modified with Sulfonic Acid and Their Catalytic Activity on Ring Opening Polymerization of Octamethylcyclotetrasiloxane (술폰산으로 표면개질된 메조기공 실리카 촉매의 제조 및 Octamethylcyclotetrasiloxane 개환중합에서의 촉매 활성)

  • Lee, Yeonsong;Hwang, Ha Soo;Lee, Jiyoung;Lo, Nu Hoang Tien;Nguyen, Tien Giang;Lee, Donghyun;Park, In
    • Applied Chemistry for Engineering
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    • v.31 no.4
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    • pp.383-389
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    • 2020
  • Mesoporous silica solid catalysts modified with sulfonic acid were prepared for cationic ring-opening polymerization of octamethylcyclotetrasiloxane (D4). Two sets of MCM-41 (1.7 and 2.8 nm) and SBA-15 (8.1 and 15.9 nm) with different pore sizes were used as catalyst supports. The surface of silica materials was modified with (3-mercaptopropyl)trimethoxysilane by silylation reaction and oxidized to sulfonic acid. The structures of the prepared catalysts were examined by X-ray diffraction and nitrogen adsorption-desorption. The pore size, specific surface area, and pore volume of the modified solid catalysts decreased slightly. In addition, the modification of the sulfonic acid on the silica surface was confirmed by using infrared spectroscopy and nuclear magnetic resonance spectroscopy. To observe the effect of the particle size on the catalytic activity, it was observed with a scanning electron microscope. The catalysts were used to synthesize PDMS through a ring-opening polymerization of D4, and the conversion and polymerization rate of the polymerization reaction depended on the pore size, specific surface area, particle size, and particle agglomeration of the catalysts. In order for the polymerization rate, the catalyst prepared with SBA-15 of 8.1 nm pore size had the fastest reaction rate and showed the best catalytic activity.

Effects of Equivalent Weight of Epoxy Resins and Content of Catalyst on the Curing Reaction in Cationic Catalyst/Epoxy Cure System (양이온 촉매/에폭시 경화계에서 에폭시 수지의 당량 및 촉매 함량이 경화반응에 미치는 영향)

  • Kim, Youn Cheol;Park, Soo-Jin;Lee, Jae-Rock
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.960-966
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    • 1997
  • The effects of epoxy resins and content of catalyst on the cure characteristics were studied by FT-IR, DSC and dynamic viscometer for the thermal properties and rheological properties of the catalytic (N-Benzylpyrazinium hexafluoroantimonate, BPH) epoxy thermosetting system. Compared with DSC results of DEGBF containing 0.5wt% BPH, the DSC thermograms of DGEBA containing 0.5wt% BPH indicated that the reaction was faster than that of DGEBF/BPH and the conversion rate of DGEBA/BPH was high in the initial stage of the reaction. As the concentration of BPH increases, the reaction and conversion rates show similar value in both the cases. The influence of hydroxyl group of epoxy resin on gel point defined from the crossover point of storage modulus (G') and loss modulus (G") could be explained by the formation of 3-dimensional network in the initial stage owing to the curing reaction between epoxides and hydroxyl groups of epoxy resin. This was consistent with the gel point obtained from DSC, FT-IR and moduli crossover. The activation energy (Et) obtained from the crossover point (G'/G"=1) are $31-39kJ.mol^{-1}$ for various BPH compositions in case of two epoxy systems.

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The Separation of Vanadium and Tungsten from Spent Selective Catalytic Reduction Catalyst Leach Solution by Alamine 336 (탈질 폐촉매 침출액으로부터 Alamine 336에 의한 바나듐과 텅스텐의 분리)

  • Seongsu Kang;Gyeonghye Moon;In-Hyeok Choi;Dakyeong Baek;Kyoungkeun Yoo
    • Resources Recycling
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    • v.33 no.3
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    • pp.30-37
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    • 2024
  • In this study, we investigated the separability of vanadium and tungsten from spent SCR (Selective Catalytic Reduction) catalyst leach solution by reduction of vanadium and solvent extraction using Alamine 336 and conducted experiments to optimize process conditions. It is difficult to separate vanadium and tungsten due to their similar chemical behavior, but tungsten can be selectively extracted from acidic solution when vanadium extraction is prevented by reducing anionic pentavalent vanadium to cationic tetravalent vanadium. The results showed that NaHSO3 was most suitable as a reducing agent, and the extraction efficiency of vanadium decreased and the separation efficiency increased as the amount of reducing agent added, reaction time, and temperature increased. When reducing NaHSO3 1.5 eq, 60 min, and 60℃, which are optimal conditions of reduction, vanadium and tungsten were effectively separated with vanadium extraction efficiency of 5.8%, tungsten extraction efficiency of 99%, and separation factor of vanadium and tungsten of 7,564.

Platinum-Catalyzed and Ion-Selective Polystyrene Fibrous Membrane by Electrospinning and In-Situ Metallization Techniques

  • Hong, Seung-Hee;Lee, Sun-Ae;Nam, Jae-Do;Lee, Young-Kwan;Kim, Tae-Sung;Won, Sung-Ho
    • Macromolecular Research
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    • v.16 no.3
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    • pp.204-211
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    • 2008
  • A platinum-catalyzed polyelectrolyte porous membrane was prepared by solid-state compression of electrospun polystyrene (PS) fibers and in-situ metallization of counter-balanced ionic metal sources on the polymer surface. Using this ion-exchange metal-polymer composite system, fiber entangled pores were formed in the interstitial space of the fibers, which were surrounded by sulfonic acid sites ($SO_3^-$) to give a cation-selective polyelectrolyte porous bed with an ion exchange capacity ($I_{EC}$) of 3.0 meq/g and an ionic conductivity of 0.09 S/cm. The Pt loading was estimated to be 16.32 wt% from the $SO_3^-$ ions on the surface of the sulfonated PS fibers, which interact with the cationic platinum complex, $Pt(NH_3)_4^{2+}$, at a ratio of 3:1 based on steric hindrance and the arrangement of interacting ions. This is in good agreement with the Pt loading of 15.82 wt% measured by inductively coupled plasma-optical emission spectroscopy (ICP-OES). The Pt-loaded sulfonated PS media showed an ionic conductivity of 0.32 S/cm. The in-situ metallized platinum provided a nano-sized and strongly-bound catalyst in robust porous media, which highlights its potential use in various electrochemical and catalytic systems.

Thermal Properties of Diglycidyl Ether of Terephthalylidene-bis-(4-amino-3-methylphenol) (Diglycidyl ether of terephthalylidene-bis-(4-amino-3-methylphenol)의 열적 성질에 대한 연구)

  • Hyun, Ha-Neul;Choi, Ji-Woo;Cho, Seung-Hyun
    • Composites Research
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    • v.35 no.2
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    • pp.53-60
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    • 2022
  • This study uses Diglycidyl ether of terephthalylidene-bis-(4-amino-3-methylphenol) (DGETAM), an amine hardener 4,4'-diaminodiphenylethane (DDE) and cationic catalyst N-benzylpyrazinium hexafluoroantimonate (BPH) to make epoxy film. For analysis, 1H_NMR and FT-IR were used to verify proper synthesis, and the liquid crystallinity of DGETAM was checked using Differntial Scanning Calorimetry and Polarized Optical Microscopy. Thermal conductivity of the sample was measured using Laser Flash Apparatus. Thermal stability as well as thermal conductivity is important when used as a packaging material. Activated energy is the energy needed to generate a response, which can be used to estimate the energy required to maintain physical properties. It was obtained using the Arrhenius equation based on the data measured by isothermal decomposition using Thermogravimetric Analysis. Measurement of the thermal conductivity of epoxy films showed higher thermal conductivity when DDE was used, and it was found that thermal conductivity had an effect on thermal stability, given that it represented an activation energy similar to a film with BPH upon 5% decomposition.

Structure-Property Relationship of PVA-SbQ Water Soluble Photosensitive Polymer and its Application to Screening Process of Color Monitor (PVA-SbQ 수용성 감광성 고분자의 구조와 감도관계 및 칼라 수상관 스크린 공정에의 응용)

  • Park, Lee Soon;Han, Yoon Soo;Kim, Bong Chul
    • Applied Chemistry for Engineering
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    • v.7 no.2
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    • pp.379-386
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    • 1996
  • Photosensitive compound, 1-methyl-4-[2-(4-diethylacetylphenyl)ethenyl] pridinium methosulfate(SbQ-A salt), was synthesized from dimethyl sulfate, terephthalaldehyde mono-(diethylacetal) and 4-picoline. SbQ-A salts were reacted with poly(vinyl alcohol)s, (PVA) in aqueous solution with phosphoric acid as catalyst to give photosensitive PVA-SbQ with different SbQ content and molecular weight. Relative photosensitivity of PVA-SbQ was determined by gray scale(GS) method. The rotative sensitivity of PVA-SbQ increased with increasing amount of bound SbQ in the case of high molecular weight(MW=77,000-79,000g/mol) as substrate and decreased with decreasing molecular weight of PVA with about constant(1.3mol%) amount of bound SbQ. The most sensitive polymer was obtained when SbQ group content in PVA-SbQ reached about 2.63mol% in the case of high molecular weight(77,000-79,000g/mol) PVA. This sample showed 90 times greater sensitivity than dichromated PVA as reference photosensitive system. PVA-SbQ photosensitive polymer synthesized was applied to the photolithographic screening process of phosphor on the panel of cathode ray tube(CRT). Phosphor slurry was made with PVA-SbQ, phosphor, a small amount of surfactant and other additives using water as medium. The slurry was coated onto panel, dried by heater, exposed to UV light and then developed by distilled water. When a small amount of cationic surfactant such as cetyltrimethylammonium chloride was used in the slurry formulation, the sharpness of phosphor pattern was equal to or better than that of dichromated PVA photosensitive polymer system used currently.

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