• Title/Summary/Keyword: polymer synthesis and characterization

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Synthesis and Characterization of Biodegradable MethoxyPoly(ethylene glycol)-Poly$(\varepsilon-caprolactone-co-L-lactide)$ Block Copolymers (메톡시폴리(에틸렌 글리콜)-폴리(카프로락톤-co-L-락타이드) 공중합체의 합성 및 특성 분석)

  • Hyun Hoon;Cho Young Ho;Jeong Sung Chan;Lee Bong;Kim Moon Suk;Khang Gilson;Lee Hai Bang
    • Polymer(Korea)
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    • v.30 no.1
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    • pp.28-34
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    • 2006
  • A series of methoxypoly(ethylene glycol) $(MPEG)-poly(\varepsilon-co-L-lactide)$ (PCLA) diblock copolymers were synthesized by ring-opening polymerization of a mixture of $\varepsilon-caprolactone$ and L-lactide with different ratios in the presence of $Sn(Oct)_2$. The characterization of MPEG-PCLA diblock copolymers were examined by $^1H-NMR$, GPC, DSC, and XRD. Kinetic study on ring-opening polymerization of monomer mixtures was carried out in various conditions such as a variation with polymerization time, amount of catalyst, and temperature. The highest conversion obtained in 1.2 ratic of initiator venn catalyst at $110\;^{\circ}C$. The biodegradable characterization of MPEG-PCLA diblock copolymers in aqueous solution was carried out by using GPC for $1\~14$ weeks. The biodegradability of MPEG-PCLA diblock copolymers increased as the L-lactide content of diblock copolymers increased. In conclusion, we confirmed the dependence of polymerization rate according to various conditions. In addition, we can control the biodegradability of MPEC-PCLA diblock copolymers by changing the ratio of PCL and PLA block segment.

Synthesis and Characterization of H3PO4 Doped Poly(benzimidazole-co-benzoxazole) Membranes for High Temperature Polymer Electrolyte Fuel Cells

  • Lee, Hye-Jin;Lee, Dong-Hoon;Henkensmeier, Dirk;Jang, Jong-Hyun;Cho, Eun-Ae;Kim, Hyoung-Juhn;Kim, Hwa-Yong
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3279-3284
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    • 2012
  • Poly(benzimidazole-co-benzoxazole)s (PBI-co-PBO) are synthesized by polycondensation reaction with 3,3'-diaminobenzidine, terephthalic acid and 3,3'-dihydroxybenzidine or 4,6-diaminoresorcinol in polyphosphoric acid (PPA). All polymer membranes are prepared by the direct casting method (in-situ fabrication). The introduction of benzoxazole units (BO units) into a polymer backbone lowers the basic property and $H_3PO_4$ doping level of the copolymer membranes, resulting in the improvement of mechanical strength. The proton conductivity of $H_3PO_4$ doped PBI-co-PBO membranes decrease as a result of adding amounts of BO units. The maximum tensile strength reaches 4.1 MPa with a 10% molar ratio of BO units in the copolymer. As a result, the $H_3PO_4$ doped PBI-co-PBO membranes could be utilized as alternative proton exchange membranes in high temperature polymer electrolyte fuel cells.

Synthesis and characterization of thiolated hexanoyl glycol chitosan as a mucoadhesive thermogelling polymer

  • Cho, Ik Sung;Oh, Hye Min;Cho, Myeong Ok;Jang, Bo Seul;Cho, Jung-Kyo;Park, Kyoung Hwan;Kang, Sun-Woong;Huh, Kang Moo
    • Biomaterials Research
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    • v.22 no.4
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    • pp.249-258
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    • 2018
  • Background: Mucoadhesive polymers, which may increase the contact time between the polymer and the tissue, have been widely investigated for pharmaceutical formulations. In this study, we developed a new polysaccharide-based mucoadhesive polymer with thermogelling properties. Methods: Hexanoyl glycol chitosan (HGC), a new thermogelling polymer, was synthesized by the chemical modification of glycol chitosan using hexanoic anhydride. The HGC was further modified to include thiol groups to improve the mucoadhesive property of thermogelling HGC. The degree of thiolation of the thiolated HGCs (SH-HGCs) was controlled in the range of 5-10% by adjusting the feed molar ratio. The structure of the chemically modified polymers was characterized by $^1H$ NMR and ATR-FTIR. The sol-gel transition, mucoadhesiveness, and biocompatibility of the polymers were determined by a tube inverting method, rheological measurements, and in vitro cytotoxicity tests, respectively. Results: The aqueous solution (4 wt%) of HGC with approximately 33% substitution showed a sol-gel transition temperature of approximately $41^{\circ}C$. SH-HGCs demonstrated lower sol-gel transition temperatures ($34{\pm}1$ and $31{\pm}1^{\circ}C$) compared to that of HGC due to the introduction of thiol groups. Rheological studies of aqueous mixture solutions of SH-HGCs and mucin showed that SH-HGCs had stronger mucoadhesiveness than HGC due to the interaction between the thiol groups of SH-HGCs and mucin. Additionally, we confirmed that the thermogelling properties might improve the mucoadhesive force of polymers. Several in vitro cytotoxicity tests showed that SH-HGCs showed little toxicity at concentrations of 0.1-1.0 wt%, indicating good biocompatibility of the polymers. Conclusions: The resultant thiolated hexanoyl glycol chitosans may play a crucial role in mucoadhesive applications in biomedical areas.

Synthesis and Characterization of Electro-Active Poly(2-acrylamido-2-methylpropanesulfonic acid) Polymer Gel Actuator (전기활성 Poly(2-acrylamido-2-methylpropanesulfonic acid) 고분자 겔 구동기의 합성 및 특성분석)

  • 송영진;심우선;김홍경;김학길;최혁렬;김훈모;전재욱;이영관;남재도
    • Polymer(Korea)
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    • v.25 no.5
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    • pp.736-743
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    • 2001
  • An electro- active polymer (EAP) (poly(2-acrylamido-2- methyl propane sulfonic acid), PAMPS) gel crosslinked with N,N-methylenebisacrylamide (MBAA) has been prepared by free radical polymerization in aqueous solution with potassium persulfate as initiator PAMPS gel was swollen in surfactant solution to substitute surfactant for using as actuator. PAMPS gel showed a large movement in the surfactant solution by electric field. PAMPS gel showed the reversible binding and fast response rate. Bending mechanism of gel is related to the cooperative process of hydrophobic interaction, swelling-deswelling of gel and the electrostatic attraction between anode (+) and the anions of PAMPS gel. The response rate of PAMPS gel was increased as the applied potential and the degree of cross-linkage were increased. The response rate was increased as the bending cycle was repeated, but it was decreased with increasing the gel thickness.

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Synthesis of Polyacrylates Containing Si, Ge and Sn for High Refractive Index (실리콘, 게르마늄, 주석이 결합된 고굴절률 아크릴 고분자의 합성)

  • Maheswara, Muchchintala;Do, Jung-Yun
    • Polymer(Korea)
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    • v.34 no.6
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    • pp.588-593
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    • 2010
  • New seven acrylic monomers with covalently bonded silicon, germanium, and tin were prepared for high refractive index materials. The monomers were copolymerized with a cross-linkable comonomer (Trimer) to prepare UV-films for optical characterization. The refractive index of the copolymers increased in proportion to the monomer content and extrapolated to determine that of homopolymer. $Ph_3Si$, $Ph_3Ge$, and $Ph_3Sn$ groups contributed to increase the refractive index of acrylic polymer, in which $Ph_3Sn$ was more effective than $Ph_3Ge$. The index increment confidently occurred with $Bu_3Sn$ attachment in comparison with aliphatic acrylic polymers. $Ph_3SnS$-attached acrylate polymer showed a refractive index of 1.671 at 589 nm. The index change was similarly observed at various different wavelengths (656, 830, 1310, and 1550 nm).

Synthesis and Characterization of New Positive Photosensitive Polyimide Having Photocleavable 4,5-Dimethoxy-2-nitrobenzyl (DMNB) Groups (감광성 DMNB 기를 함유한 새로운 포지형 감광성 폴리이미드의 합성 및 물성)

  • 최옥자;류윤미;정민국;이명훈
    • Polymer(Korea)
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    • v.26 no.6
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    • pp.701-709
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    • 2002
  • To synthesize a new positive photosensitive polyimide precursor, parts of carboxylic acid groups in poly (amic acid) were esterified with 4,5-dimethoxy-2-nitrobenzyl bromide in the presence of K$_2$CO$_3$/HMPA followed by the chemical imidization of residual carboxylic acid units. The chemical structure of resulting polymer was characterized by $^1$H-NMR, UV/vis and FT-IR spectroscopic methods, and its thermal properties were examined by DSC and TGA. Upon UV irradiation, 4,5-dimethoxy-2-nitrobenzyl moiety underwent the photodegradation. As a result, the polymer became soluble in alkaline developer due to the formation of carboxylic acid moiety, which was used to make a micron-sized positive pattern. Sensitivity curves were obtained from the gel fraction experiments with respect to the various 4,5-dimethoxy-2-nitrobenzyl ester contents. From those curves, the sensitivity was ranged iron 4000 to 6000 mJ/㎠, and the contrast was measured to be from 3.1 to 4.9.

Synthesis and Characterization of π-Conjugated Polymer Based on Phthalimide Derivative and its Application for Polymer Solar Cells (프탈이미드 유도체를 기본으로 하는 공액고분자의 합성과 특성, 그리고 태양전지의 적용)

  • Do, Thu Trang;Ha, Ye Eun;Kim, Joo Hyun
    • Polymer(Korea)
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    • v.37 no.6
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    • pp.694-701
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    • 2013
  • A new copolymer named T-TI24T (poly((5,5-(2-butyl-5,6-bisdecyloxy-4,7-di-thiophen-2-yl-isoindole-1,3-dione))- alt-(2,5-thiophene))) based on phthalimide derivative and thiophene is synthesized by the Stille-coupling reaction. The polymer shows relatively high number average molecular weight of 86500 g/mol with good solubility in common organic solvents such as chloroform, 1,2-dichlorobenzene, and toluene and is thermally stable up to $380^{\circ}C$. Besides, it possesses a relatively low highest occupied molecular orbital (HOMO) energy level of -5.33 eV, promising the high open circuit voltage ($V_{oc}$) for photovoltaic applications. Active layer solution of polymer T-TI24T-as a donor and (6)-1-(3-(methoxycarbonyl)- {5}-1-phenyl[5,6]-fullerene (PCBM)-as an acceptor in different weight ratios is applied to fabricate the polymer solar cell devices. The ratio of polymer/PCBM affects the solar cell efficiency and the best performance exhibits in the device with polymer/PCBM = 1:3 (w/w), which shows a power conversion efficiency (PCE) of 0.199% and a $V_{oc}$ of 0.99 V, respectively. Even though the device shows the very low PCE, the $V_{oc}$ is higher than that of well known bulk heterojunction type solar cell based on P3HT:PC61BM (c.a. 0.5 V).

Synthesis and characterization of silicone-containing polyamideimide and its gas separation

  • 이용범;심진기;이영무
    • Proceedings of the Membrane Society of Korea Conference
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    • 1997.10a
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    • pp.83-84
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    • 1997
  • 1. INTRODUCTION : Polyimides containing siloxane moiety(poly(imide siloxane), or polysiloxaneimide) have been synthesized because of their some merits over polyimide itseft. Polyimides have excellent thermal and mechanical properties but their poor solubility and processibility in their fullly imidized form give disadvantages in applications. Incorporation of siloxane units make it possible to increase solubility and processibility, and also impart impact resistance, low moisture uptake, low dielectric constant, thermo-oxidative resistance, good adhesion properties to substrate and etc.. Incorporation methods of siloxane groups into the polyimide was mainly copolymerization or terpolymerization between oligomeric dimethylsiloxane and aromatic dianhydride. A few methods of introducing siloxane units in functional groups of polyimide was reported. In our laboratory poly(amideimide siloxane) and poly(imide siloxane) were prepared and the study about their thermal kinetics was performed. In separation membrane area, polysiloxaneimides was utilized in pervaporation and gas separation. Polyimides in gas separation show high selectivity and very low permeability, and introduction of siloxane segments increase permeability with low decrease in selectivity. We aimed to introduce silicone segments into poly(amic acid) state and synthesize polymer partially imidized, and also show the gas separation characteristics of the synthesized polymer.

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Synthesis and Characterization of Phenanthrene-substituted Fullerene Derivatives as Electron Acceptors for P3HT-based Polymer Solar Cells

  • Mi, Dongbo;Park, Jong Baek;Xu, Fei;Kim, Hee Un;Kim, Ji-Hoon;Hwang, Do-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1647-1653
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    • 2014
  • 9,10-Bis(bromomethyl)phenanthrene reacted with fullerenes via a Diels-Alder reaction to give phenanthrene-substituted fullerene mono-adducts (PCMA) and bis-adducts (PCBA) as electron acceptors for organic photovoltaic cells (OPVs). The syntheses of the fullerene derivatives were confirmed by $^1H$ $^{13}C$ NMR spectroscopy and MALDI-TOF mass spectrometry. PCMA and PCBA showed better light absorption in the UV-visible region than $PC_{61}BM$. Their electrochemical properties were measured using cyclic voltammetry. Accordingly, the lowest unoccupied molecular orbital (LUMO) energy levels of PCMA and PCBA were -3.66 and -3.57 eV, respectively. Photovoltaic cells were fabricated with a ITO/PEDOT:PSS/poly(3-hexylthiophene)(P3HT):acceptor/LiF/Al configuration, where P3HT and PCBA are the electron donors and acceptors, respectively. The polymer solar cell fabricated using the P3HT:PCBA active layer showed a maximum power conversion efficiency of 0.71%.

Synthesis and Characterization of Di and Triblock Copolymers Containing a Naphthalene Unit for Polymer Electrolyte Membranes (고분자전해질 막을 위한 나프탈렌 단위를 포함하는 디 및 트리 블록공중합체의 합성 및 특성분석)

  • KIM, AERHAN
    • Transactions of the Korean hydrogen and new energy society
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    • v.27 no.6
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    • pp.660-669
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    • 2016
  • A fluorinated-sulfonated, hydrophobic-hydrophilic copolymer was planed subsequently synthesized using typical nucleophilic substitution polycondensation reaction. A novel AB and ABA (or BAB) block copolymers were synthesized using sBCPSBP (sulfonated 4,4'-bis[4-chlorophenyl)sulfonyl]-1,1'-biphenyl), DHN (1,5-dihydroxynaphthalene), DFBP (decafluorobiphenyl) and HFIP (4,4'-hexafluoroisopropylidenediphenol). All block copolymers were easily cast and made into clear films. The structure and synthesized copolymers and corresponding membranes were analyzed using GPC (gel permeation chromatography), $^1H$-NMR ($^1H$ nuclear magnetic resonance) and FT-IR (Fourier transform infrared). TGA (Thermogravimetric analysis) and DSC (differential scanning calorimetry) analysis showed that the prepared membranes were thermally stable, so that elevated temperature fuel cell operation would be possible. Hydrophobic/hydrophilic phase separation and clear ionic aggregate block morpology was confirmed in both triblock and diblock copolymer in AFM (atomic force microscopy), which may be highly related to their proton transport ability. A sulfonated BAB triblock copolymer membrane with an ion-exchange capacity (IEC) of 0.6 meq/g has a maximum ion conductivity of 40.3 mS/cm at $90^{\circ}C$ and 100% relative humidity.