• 제목/요약/키워드: chemical crosslinking

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Physicochemical Characterization of Extrudate Solid Formulation of Angelica gigas Nakai Prepared by Hot Melt Extrusion Process

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Koo, Ja Seong;Park, Cheol Ho;Kang, Wie Soo
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2018.04a
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    • pp.72-72
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    • 2018
  • The root of Angelica gigas Nakai (AGN) is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, a major challenge associated with the usage of the active compounds from AGN is their poor water solubility. Therefore, this work aimed to enhance the solubility of active compounds by a chemical (viz. surfactant) and physical (hot melt extrusion) crosslinking method (CPC). Infrared Fourier transform spectroscopy (FT-IR) revealed multiple peaks in extrudate solids representing new functional groups including carboxylic acid, alkynes and benzene derivatives. Differential scanning calorimetry (DSC) analysis of the extrudate showed lower glass transition temperature (Tg) and lower enthalpy (${\Delta}H$) (Tg: $43^{\circ}C$; ${\Delta}H$: <6 (J/g)) compared to the non-extrudate (Tg $68.5^{\circ}C$; ${\Delta}H$: 123.2) formulations. X-ray powder diffraction (XRD) analysis revealed amorphization of crystal materials in extrudate solid. In addition, nanonization, enhanced solubility and higher extraction of phenolic compounds were achieved in the extrudate solid. Among the different extrudates, acetic acid- and Span 80-mediated formulations showed superior extractions. We conclude that the CPC method successfully enhanced the production of amorphous nano dispersions from extrudate solid formulations.

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Enhancement of Solubility and Nanonization of Phenolic Compound in Extrudate from Angelica gigas Nakai by Hot Melt Extrusion using Surfactant (유화제 첨가 용융압출을 이용한 참당귀 성형체의 페놀성분 나노화 및 용해도 향상)

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Go, Eun Ji;Lim, Jung Dae;Park, Cheol Ho;Kang, Wie Soo
    • Korean Journal of Medicinal Crop Science
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    • v.26 no.4
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    • pp.317-327
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    • 2018
  • Background: The root of Angelica gigas Nakai is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, the poor water solubility of the active components in A. gigas Nakai is a major obstacle to its bioavailability. Methods and Results: This work aimed at enhancing the solubility of the active compounds of A. gigas Nakai by a chemical (using a surfactant) and physical (hot melt extrusion, HME) crosslinking method. Fourier transform infrared spectroscopy revealed multiple peaks in the case of the extrudate solids, attributable to new functional groups including carboxylic acid, alkynes, and benzene derivatives. Differential scanning calorimetry analysis showed that the extrudate soilid had a lower glass transition temperature ($T_g$) and enthalpy (${\Delta}H$) ($T_g:43^{\circ}C$, ${\Delta}H$ : < 6 J/g) as compared to the non-extrudate ($T_g:68.5^{\circ}C$, ${\Delta}H:123.2$) formulations. X-ray powder diffraction analysis revealed the amorphization of crystalline materials in the extrudate solid. In addition, enhanced solubility (53%), nanonization (403 nm), and a higher amount of extracted phenolic compounds were achieved in the extrudate solid than in the non-extrudate (solubility : 36%, nanonization : 1,499 nm) formulation. Among the different extrudates, acetic acid and span 80 mediated formulations showed superior extractions efficiency. Conclusions: HME successfully enhanced the production of amorphous nano dispersions of phenolic compound including decursin from extrudate solid formulations.

Preparation of Glycidylmethacrylate-Divinylbenzene Copolymers Containing Phosphoric Acid Groups and Their Adsorption Characteristics of Uranium(II) - Adsorption Equilibrium and Kinetics of Uranium on RGP Resins - (인산기를 함유한 Glycidylmethacrylate-Divinylbenzene 공중합체의 제조와 우라늄 흡착특성(제2보) - RGP수지에 대한 우라늄의 흡착평형과 흡착속도 -)

  • Huh, Kwang Sun;Park, Sang Wook
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.689-697
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    • 1998
  • In this work, we studied the equilibrium, rate and rate determining step of uranium adsorption on RGP resins of MR type prepared by varying the degree of crosslinking and the amount of diluent. The equilibrium of uranium adsorption on RGP resins were well explained by Frendrich isotherm as well as Langmuir isotherm model. The amount of adsorption and adsorption rate increase with the adsorption temperature. The heat of the adsorption was 11 kcal/mol. The adsorption rates of uranium on RGP resins were decreased in the order of RGP-10(50)>RGP-1(50)>RGP-2(50)>RGP-5(50)>RGP-0(50) and RGP-2(75)>RGP-2(100)>RGP-2(50)>RGP-2(30)>RGP-2(0). The diffusion resistance of uranium into RGP resin increased as follows; molecular diffusion < pore diffusion < surface diffusion. On the other hand, the surface diffusion was more dominative than the pore diffusion in intraparticle region. Thus, this result indicates that the adsorption mechanism of uranium on RGP resins is intraparticle diffusion controlled.

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Synthesis and Characterization of Vinylbenzyl Chloride-co-Styrene-co-Hydroxyethyl Acrylate (VBC-co-St-co-HEA) Anion-Exchange Membrane for All-Vanadium Redox Flow Battery (전바나듐계 레독스-흐름 전지용 Vinylbenzyl Chloride-co-Styrene-co-Hydroxyethyl Acrylate (VBC-co-St-co-HEA) 음이온교환막의 합성 및 특성)

  • Baek, Young-Min;Kwak, Noh-Seok;Hwang, Taek-Sung
    • Polymer(Korea)
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    • v.35 no.6
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    • pp.586-592
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    • 2011
  • In this study, we synthesized vinylbenzyl chloride-co-styrene-co hydroxyethyl acrylate (VBC-co-St-co-HEA) copolymer that can be applied to redox the flow battery process. The anion exchange membrane was prepared by the amination and crosslinking of VBC-co-St-co-HEA copolymer. The chemical structure and thermal properties of VBC-co-St-co-HEA copolymer and aminated VBC-co-St-co-HEA(AVSH) membrane were characterized by FTIR, $^1H$ NMR, TGA, and GPC analysis. The membrane properties such as ion exchange capacity(IEC), electrical resistance, ion conductivity and efficiency of all-vanadium redox flow battery were measured. The IEC value, electrical resistance, and ion conductivity were 1.17 meq/g, $1.9{\Omega}{\cdot}cm^2$, 0.009 S/cm, respectively. The charge-discharge efficiency, voltage efficiency and energy efficiency from all-vanadium redox flow battery test were 99.5, 72.6 and 72.1%, respectively.

Study of the Crystal Structure of a Lyocell Precursor for Carbon Fibers (탄소섬유용 리오셀 전구체의 결정구조에 관한 연구)

  • Park, Gil-Young;Kim, Woo-Sung;Lee, Su-Oh;Hwang, Tae-Kyung;Kim, Yun-Chul;Seo, Sang-Kyu;Chung, Yong-Sik
    • Journal of the Korean Society of Propulsion Engineers
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    • v.23 no.5
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    • pp.36-42
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    • 2019
  • In this study, the pre-treatment of lyocell fabrics was performed using phosphoric acid (PA) as a phosphorus flame retardant and melamine resin (MR) as a cross-linking agent to fabricate carbon fabrics using lyocell fibers. The physical and chemical changes were investigated by thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD) and weight analysis. We confirmed that the weight yield of the carbon fabrics compared to the untreated fabrics increased by 14.7%, and width and length yield of the fabrics increased by 15% and 15.5%, respectively. This may be due to the effect of promoting the dehydration reaction of cellulose, forming char on the fiber surface, which induces a crosslinking reaction in the cellulose molecule and stabilizes the structure upon pyrolysis.

Effects of heat and gamma radiation on the degradation behaviour of fluoroelastomer in a simulated severe accident environment

  • Inyoung Song ;Taehyun Lee ;Kyungha Ryu ;Yong Jin Kim ;Myung Sung Kim ;Jong Won Park;Ji Hyun Kim
    • Nuclear Engineering and Technology
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    • v.54 no.12
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    • pp.4514-4521
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    • 2022
  • In this study, the effects of heat and radiation on the degradation behaviour of fluoroelastomer under simulated normal operation and a severe accident environment were investigated using sequential testing of gamma irradiation and thermal degradation. Tensile properties and Shore A hardness were measured, and thermogravimetric analysis was used to evaluate the degradation behaviour of fluoroelastomer. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy were used to characterize the structural changes of the fluoroelastomer. Heat and radiation generated in nuclear power plant break and deform the chemical bonds, and fluoroelastomer exposed to these environments have decreased C-H and functional groups that contain oxygen and double bonds such as C-O, C=O and C=C were generated. These functional groups were formed by auto oxidation by reacting free radicals generated from the cleaved bond with oxygen in the atmosphere. In this auto oxidation reaction, crosslinks were generated where bonded to each other, and the mobility of molecules was decreased, and as a result, the fluoroelastomer was hardened. This hardening behaviour occurred more significantly in the severe accident environment than in the normal operation condition, and it was found that thermal stability decreased with the generation of unstable structures by crosslinking.

Synthesis of Resole-type Phenolic Beads via Suspension Polymerization Technique (현탁중합을 이용한 레졸형 구형 페놀입자의 합성)

  • Hahn, Dongseok;Kim, Daejung;Kim, Hongkyeong
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.279-284
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    • 2013
  • The phenolic beads in macrosize range were obtained by suspension polymerization at $98^{\circ}C$ from phenol and formaldehyde in the presence of basic catalyst with a phenol to formaldehyde (P/F) range of 1:1~1:4, and they were carbonized to spherical carbon beads under nitrogen at $700^{\circ}C$. Thermal analysis on spherical phenolic beads obtained by suspension polymerization showed that the postcuring process is essential. In order to optimize the suspension polymerization, the effects of the P/F molar ratio, the pH of catalyst, and the molecular weight of stabilizer on the size distribution and yield of spherical phenol beads were examined separatively. The particle size was increased whereas the yield was decreased with P/F molar ratio. The increasing basicity of catalyst made the particle size to increase, while the molecular weight of stabilizer had more effect on the yield rather than on the particle size distribution. The thermal stability of the spherical phenolic beads obtained through postcure was also examined by TGA. The phenol beads of high P/F ratio still showed the weight loss at $220^{\circ}C$ even after postcure due to the high possibility of dibenzyl ether, while those of low P/F ratio showed the steady decrease in weight during $220^{\circ}C$ to $400^{\circ}C$, which showed that the optimal P/F ratio was 1:2.

Thermodynamic Study of Poly(dimethylsiloxane)-Solvents Systems Using Inverse Gas Chromatography (Inverse Gas Chromatography를 이용한 Poly(dimethylsiloxane)-Solvent계의 열역학적 연구)

  • Cho, Joung-Mo;Kang, Choon-Hyoung
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.718-725
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    • 1999
  • In order to investigate the interaction characteristics of poly(dimethylsiloxane) (PDMS) with various solvents such as water, ethanol, and iso-propanol, Inverse Gas Chromatography(IGC) at finite concentration, which is a very fast, accurate, and thus promising technique in thermodynamic study of polymer systems, is employed. By measuring the specific retention volumes of the probes, the interaction parameters are calculated by means of the Flory-Huggins equation. From the results, the interaction parameters of the probes are, as expected due to the hydrophobicity of the polymer, found to be of large positive values (2$2.0{\times}10^{-3}mol/g$. For the linear PDMS, interpretation of the space distribution of molecules is performed by the Kirkwood-Buff-Zimm(KBZ) integrals, which give intuitive information about physical properties. From the KBZ integrals, water does not show the tendency of preferential solvation with the PDMS but formed self-cluster. The larger solvent molecules show a stronger tendency to distribute more randomly in the mixture.

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Evaluation of Durability for Glass fabric/Phenolic Composites under Salt Water Environment (염수환경에 노출된 유리섬유직물/페놀 복합재의 내구성 평가)

  • Yoon, Sung-Ho
    • Composites Research
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    • v.18 no.4
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    • pp.27-34
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    • 2005
  • Salt water spray and immersion tests were experimentally conducted for over 6 months to investigate the durability of glass fabric/phenolic composites under salt water environment. Mechanical properties such as tensile properties, flexural properties, and shear properties were evaluated and thermal analysis properties such as storage shear modulus, loss shear moduls, and tan 6 were obtained through a DMA. A change in chemical structures was analyzed through a FTIR. According to the results, mechanical properties and thermal analysis properties were sensitive to salt water environment and these properties began to degrade in increasing in exposure times. However, tensile and flexural moduli started to decrease and then slightly increase as increasing in exposure times due to plasticization and crosslinking in matrix as well as physical swelling in composites. Beyond a certain exposure times, these properties began to decrease as further increasing in exposure times. Also the shape and location of peaks in FTIR curves were insensitive to exposure times, but the intensity of peaks would be. finally we found that the durability of glass fabric/phenolic composites were affected on salt water immersion environment rather than salt water spray environment.

Preparation and Characterization of Biomass-based Polymer Blend Films(2) (Biomass-based 고분자 블렌드 필름의 제조 및 특성 연구(2))

  • Lee, Soo;Park, Myung-Ho
    • Journal of the Korean Applied Science and Technology
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    • v.30 no.2
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    • pp.305-311
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    • 2013
  • PLA(polylactic acid), one of biodegradable polymers was blended with various amounts of wood pulp powder through solution blending technic to verify the effect of reinforcing pulp amount on the mechanical properties of blend films. Also these blend films were further modified with TDI(toluene diisocyanate) as crosslinking agent to introduce urethane functions by reaction of pulp hydroxyl groups and isocyanate. As a result, the tensile strength of blend film with 0.25 wt% pulp was increased from $565.25kg_f/cm^2$ for PLA film itself to $624.20kg_f/cm^2$. However, elongation of this film was decreased by 50% of that of PLA film itself. Only PLA/pulp blend film further modified with 500% of TDI/0.25 wt% pulp showed the slightly increased tensile strength but decreased elongation. Melting point and glass transition temperature of PLA/pulp blend films were confirmed by using Differential Scanning Calorimeter(DSC). Thermal stability of these blend films measured by TGA showed only a slight increase at temperature lower than $300^{\circ}C$.