• Title/Summary/Keyword: polymerization time

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Novel pH/Temperature Sensitive Hydrogels of Poly (ethylene glycol)-Poly (caprolactone) -Poly (${\beta}-amino\;ester$) (PAE-PCLA-PEGPCLA-PAE) Biodegradable Polyester Block Copolymer

  • Huynh Dai Phu;Lee Doo-Sung
    • Proceedings of the Polymer Society of Korea Conference
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    • 2006.10a
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    • pp.263-263
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    • 2006
  • Poly (ethylene glycol)(PEG) - Poly (${\varepsilon}-caprolactone(CL)$) - Poly (D,L lactide(LA) (PCLA-PEG-PCLA) was synthesized by ring-opening polymerization to form temperature sensitive hydrogel triblock copolymer. The triblock copolymer was acrylated by acryloyl chloride. ${\beta}-amino$ ester was used as a pH sensitive moiety, in this study ${\beta}$- amino ester obtained from 1,4-butandiol diacrylate, and 4, 4' trimethylene dipiperidine, it have pKb around 6.6. pH/temperature sensitive penta-block copolymer (PAE-PCL-PEG-PCL-PAE) was synthesized by addition polymerization from acrylated triblock copolymer, 1,4-butandiol diacrylate, and 4, 4' trimethylene dipiperidine. Their physicochemical properties of triblock and penta-block copolymers were characterized by $^1H-NMR$ spectroscopy and gel permeation spectroscopy. Sol-gel phase transition behavior of PAE-PCL-PEG-PCL-PAE block copolymers were investigated by remains stable method. Aqueous media of the penta-block copolymer (at 20 wt%) changed from a sol phase at pH 6.4 and $10^{\circ}C$ to a gel phase at pH 7.4 and $37^{\circ}C$. The sol-gel transition properties of these block copolymers are influenced by the hydrophobic/hydrophilic balance of the copolymers, block length, hydrophobicity, stereo-regularity of the hydrophobic of the block copolymer, and the ionization of the pH function groups in the copolymer depended on the changing of environmental pH, respectively. The degradation and the stabilization at pH 7.4 and $37^{\circ}C$, and the stabilization at pH 6.4 and $10^{\circ}C,\;5^{\circ}C,\;0^{\circ}C$, of the gel were determined. The results of toxicity experiment show that the penta block copolymer can be used for injection drug delivery system. The sol?gel transition of this block copolymer also study by in vitro test ($200{\mu}l$ aqueous solution at 20wt% polymer was injected to mouse). Insulin loading and releasing by in vitro test was investigated, the results showed that insulin can loading easily into polymer matrix and release time is around 14-16days. The PAE-PCL-PEG-PCL-PAE can be used as biomaterial for drug, protein, gene loading and delivery.

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Studies on Photosensitive Polymers (X). Studies on Photosensitivity and Spectral Sensitivity of Naphthoquinone-1,2-diazide-5-sulfonyl Esters (感光性 樹脂에 關한 硏究 (第10報). Naphthoquinone-1,2-diazide-5-sulfonyl Esters의 感光性과 分光感度)

  • Shim Jyong Sup;Kang Doo Whan
    • Journal of the Korean Chemical Society
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    • v.19 no.4
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    • pp.269-279
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    • 1975
  • Photosensitive properties of naphthoquinone-1,2-diazide-5-sulfonyl esters (PGND, BEND and PVAND) of polyglyceryl phthalate(PG), bisphenol A-epichlorohydrin condensate(BE) and polyvinyl alcohol(PVA) were investigated by the change of solubility before and after exposing to light. Various samples coated on glass or quartz plates were exposed to light under various conditions and steeped in aqueous alkali solution, and then the yield of residual film(W/W0) was determined. The yield of residual film, which was closely related to the sensitivity of the film, was affected by the degree of polymerization of the backbone resin, sensitizers and their concentration. In polymer homologs, the sensitivity was dependent on the degree of polymerization(the higher, the better). And also, it was most effective when 5 % of sensitizers to esters was used. The minimum exposed time was 0.6 min. for PGND-1, 1.0 min. for BEND-1, and 3.0 min. for PVAND-1. Most effective sensitizers for PGND, BEND and PVAND among those used here were benzanthrone, 5-nitroacenaphthene and picramide, respectively. The spectral sensitivities of PGND, BEND and PVAND were examined by comparing their spectrograms with UV-spectra in a solid state. Also, the sensitization and spectral sensitivity of the above polymers were studied. All the polymers containing the sensitizers showed optical sensitization. From the fact that in either case of sensitized or unsensitized sample, the ranges of absorption-maximum wave length were almost consistent with sensitivity maximum wave length, it was proved that the light absorbed by a sample served efficiently for photochemical reactions. Benzanthrone was found to be an excellent sensitizer for PGND.

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An Improved Manufacturing Method of p-Dicyclopentadiene (DCPD) using Tungsten Type Catalyst in Air Condition (대기 조건에서 경화가 가능한 텅스텐계 p-DCPD의 개선된 성형 방법)

  • Kwon, Dong-Jun;Shin, Pyeong-Su;Kim, Jong-Hyun;Park, Joung-Man
    • Composites Research
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    • v.29 no.4
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    • pp.216-222
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    • 2016
  • Ring-opening metathesis polymerization of p-dicyclopentadiene (DCPD) can be performed using the tungsten type catalyst. This reaction usually progresses in nitrogen condition, because the catalysts are extremely sensitive in air condition. To solve this problem, DCPD resin with tungsten (W) was cured using hot press after stirring of DCPD A and B liquid in air condition. Mechanical properties of DCPD were improved by reducing microvoid occurrence successfully by using hot press method. It might be because hot press could provide sufficient press on DCPD specimen. Addition of catalyst was not effective for the curing of resin in a short time. During polymerization, pressure and temperature had a great influence on the mechanical properties of DCPD.

The Relationship between Structural Denaturation of Antioxidative Enzymes and Their Enzyme Activity due to Repeated Exposure to UV-A (UV-A 반복노출로 인한 항산화효소의 구조변성과 효소활성의 상관관계)

  • Park, Mijung;Yoo, Hyo Jung;Kim, Jong Chan;Kim, So Ra
    • Journal of Korean Ophthalmic Optics Society
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    • v.20 no.1
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    • pp.75-81
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    • 2015
  • Purpose: The present study was conducted to investigate whether the changes in structure and activity of antioxidative enzymes, superoxide dismutase(SOD) and catalase(CAT) present in the eyes appeared when they were repeatedly exposed to UV-A, and reveal the correlation of these changes. Methods: Each enzyme solution was prepared from the standardized SOD and CAT, and repeatedly exposed to UV-A of 365 min under the condition of 30 minutes, 1 hour and 2 hours a day over 1, 2, 3, 4 and 5 days. Structural denaturation of SOD and CAT induced by repeat UV-A irradiation was confirmed by the electrophoretic analysis, and their enzyme activity was determined by the colorimetric assay using the proper assay kit. Results: SOD exposed repeatedly to UV-A showed the polymerization pattern through the electrophoretic analysis when it was repeatedly exposed under the condition of at least 1 hour a day however, the change of its activity was found to be less than 12%. On the other hand, CAT repeatedly exposed to UV-A showed reduced size of the electrophoretic band which indicated a structure denaturation and its activity was significantly decreased. In the case of that the repeat exposure time was longer, CAT activity was completely lost even though some enzyme band was shown in the electrphoretic analysis. Conclusions: From these results, it was revealed that the degree and pattern in structural denaturation of antioxidative enzymes differently appeared according to the type of enzyme, and the degree of structural denaturation was not always consistent with the reduction in enzyme activity.

The Mechanism to Oxidative Polymerization of N-Methyl-p-Aminophenol and Thermal Characteristics of the Polymer Formed (N-Methyl-p-Aminophenol의 酸化重合機構 및 生成重合體의 熱特性)

  • Choi Kyu Suck
    • Journal of the Korean Chemical Society
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    • v.16 no.5
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    • pp.314-319
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    • 1972
  • N-Methyl-p-aminophenol was polymerized by oxidative couplng in the aqueous iron chelate solution in the presence of oxygen, and black precipitate of oligo-(N-methyl-p-aminophenol) was formed quantitatively. In this oxidative polymerization reaction, methyl group attached to N in the monomer was partly eliminated, and it was clarified by the infrared spectra from the fact that the absorption of ${\delta}\;asym\;CH_3\;1460\;cm^{-1}$ and ${\delta}\;sym\;CH_3\;1380\;cm^{-1}$ in acetone insoluble fraction was much weaker than that in acetone soluble fraction. From Thermo-gravimetric analysis, oligo-(N-methyl-p-aminophenol) showed about 40% weight loss at $600^{\circ}C$ and it was less heat-resistant than oligo (p-aminophenol) that methyl group was not contained. In pyrolysis of oligo-(N-methyl-p-aminophenol) in He atmosphere, monomer N-methyl-p-aminophenol and water were formed, and in the pyrolytic gases, $H_2,\;CO,\;CO_2$ were detected by gas chromatography. From the above facts, to the structural change on oligo-(N-methyl-p-aminophenol) when it was heat-treated, it was considered that original linear structure was partly degraded, and the most of the oligomer was to go in with melt polycondensation to form polymer, and heat-resistant cyclic structure was formed at a time.

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THE POLYMERIZATION RATE AND THE DEGREE OF CONVERSION OF COMPOSITE RESINS BY DIFFERENT LIGHT SOURCES (광원의 종류에 따른 복합레진의 중합거동 및 중합률에 관한 연구)

  • Ryoo, Joo-Hee;Lee, In-Bog;Yoo, Hyun-Mee;Kim, Mi-Ja;Seok, Chang-In;Kwon, Hyuk-Choon
    • Restorative Dentistry and Endodontics
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    • v.29 no.4
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    • pp.386-398
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    • 2004
  • Objectives: The purpose of this study was to observe the reaction kinetics and the degree of polymerization of composite resins when cured by different light sources and to evaluate the effectiveness of the blue Light Emitting Diode Light Curing Units (LED LCUs) compared with conventional halogen LCUs. Materials and Methods: First, thermal analysis was performed by a differential scanning calorimeter (DSC). The LED LCU (Elipar Freelight, $320{\;}mW/\textrm{cm}^2$) and the conventional halogen LCU (XL3000, $400{\;}mV/\textrm{cm}^2$) were used in this study for curing three composite resins (SureFil, Z-250 and AEliteFLO). Second. the degree of conversion was obtained in the composite resins cured according to the above curing mode with a FTIR. Third, the measurements of depth of cure were carried out in accordance with ISO 4049 standards. Statistical analysis was performed by two-way ANOVA test at 95% levels of confidence and Duncan's procedure for multiple comparisons. Results: The heat of cure was not statistically different among the LCUs (p > 0.05). The composites cured by the LED (Exp) LCUs were statistically more slowly polymerized than by the halogen LCU and the LED (Std) LCU (p < 0.05). The composite resin groups cured by the LED (Exp) LCUs had significantly greater degree of conversion value than by the halogen LCU and the LED (Std) LCU (p =0.0002). The composite resin groups cured by the LED (Std) LCUs showed significantly greater depth of cure value than by the halogen LCU and the LED (Exp) LCU (p < 0.05).

The Change in Interfacial and Mechanical Properties for Glass Fiber/p-DCPD Composites with Degree of Ruthenium Catalyst Activation (루테늄촉매 활성정도에 따른 유리섬유/폴리다이사이클로펜타다이엔 복합재료의 기계 및 계면물성 변화)

  • Shin, Pyeong-Su;Kim, Jong-Hyun;Baek, Yeong-Min;Park, Ha-Seung;Kwon, Dong-Jun;Park, Joung-Man
    • Journal of Adhesion and Interface
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    • v.19 no.1
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    • pp.13-18
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    • 2018
  • At ruthenium (Ru) catalyst was exposed from the atmosphere, the degree of catalyst activation decreased. The change of catalyst activity with the number of days of exposure to air for the Ru catalyst was confirmed using the surface tension method quantitatively. Mechanical properties and surfactant change after polymerization by DCPD using Ru catalyst for each air exposure day was evaluated. The Ru catalyst mixed with a dilution agent was exposed in the air and color was monitored for each day. Surface tension was measured using Wilhelmy and PTFE and associated with different catalyst activities. Heat was measured in real time during polymerizing DCPD with Ru catalyst. After polymerization, tensile strength was measured for p-DCPD and the change of material property was measured. Interfacial properties were also evaluated via microdroplet pull-out tests between glass fiber and p-DCPD. The surface tension was stable until the 4 days (33 dyne/cm) whereas the surface energy increased at the 10 days (34 dyne/cm), which could be correlated with oxidation of the catalyst. Tensile property and interfacial shear strength (IFSS) was also stable until the 4 days (tensile strength: 38 MPa and IFSS: 26 MPa) whereas the mechanical property decrease at 10 days (tensile strength: 15 MPa and IFSS: 3 MPa) dramatically.

THE EFFECT OF DIFFERENT CURING MODES ON COMPOSITE RESIN/DENTIN BOND STRENGTH IN CLASS ICAVITIES (1급 와동에서 상아질과 복합레진의 결합강도에 대한 중합방법의 효과)

  • Baek, Shin-Young;Cho, Young-Gon;Song, Byeong-Choon
    • Restorative Dentistry and Endodontics
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    • v.33 no.5
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    • pp.428-434
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    • 2008
  • The purpose of this study was to compare the microtensile bond strength in Class I cavities associated with different light curing modes of same light energy density. Occlusal enamel was removed to expose a flat dentin surface and twenty box-shaped Class I cavities were prepared in dentin. Single Bond (3M Dental product) was applied and Z 250 was inserted using bulk technique. The composite was light-cured using one of four techniques, pulse delay (PD group), soft-start (SS group), pulse cure (PC group) and standard continuous cure (CC group). The light-curing unit capable of adjusting time and intensity (VIP, Bisco Dental product) was selected and the light energy density for all curing modes was fixed at $16J/cm^2$. After storage for 24 hours, specimens were sectioned into beams with a rectangular cross-sectional area of approximately $1mm^2$ Microtensile bond strength $({\mu}TBS)$ test was per- formed using a univel·sal testing machine (EZ Test, Shimadzu Co.). The results were analyzed using oneway ANOVA and Tukey's test at significance level 0.05. The ${\mu}TBS$ of PD group and SS group was higher than that of PC group and CC group. Within the limitations of this in vitro study, modification of curing modes such as pulse delay and soft start polymerization can improve resin/dentin bond strength in Class I cavities by controlling polymerization velocity of composite resin.

Hydrolysis characteristics and applications of silk sericin I. Control of molecular weight of sericin (실크 세리신의 가수분해 특성과 응용 I. 세리신의 분자량 제어)

  • 김정호;배도규
    • Journal of Sericultural and Entomological Science
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    • v.45 no.1
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    • pp.46-57
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    • 2003
  • This study was carried out to investigate the characteristics of the soluble sericins after degumming and after hydrolysis of insoluble sericin with various enzymes. Especially, the hydrolysis characteristics were examined in terms of molecular weight of the soluble sericin. Amino acid composition and molecular weight characteristics of the soluble sericins were also studied. When the insoluble sericin was hydrolyzed with kojizyme and flavourzyme, the solubility was highest at pH 7 and 50$^{\circ}C$. On the other hand, in the cases of protamex and alcalase, the highest solubility was obtained at 60$^{\circ}C$. In these cases, solubility increased with pH. In enzymatic hydrolysis, the solubility was increased with concentration of enzymes until 4 hours. After then, a slight difference was found along with treatment times. In enzymatic hydrolysis, the absorbance of the soluble sericin was increased with concentration of enzymes and treatment times. Average degree of polymerization was decreased with treatment time and concentration. The amino acid compositions were similar in low(low molecular weight by degumming) and high (high molecular weight by degumming). Those of PK (soluble sericin hydrolyzed with kojizyme), PP (soluble sericin hydrolyzed with protamex), and PA(soluble sericin hydrolyzed with alcalase) were similar to each other. Serine and tyrosine compositions were higher in low and high than those of PK, PP, and PA. However proline was absent in low and high. Molecular weights of the various sericins became higher as KP>high>PP>low>PA and those of KP and PA were 9,800 and 905 respectively.

Enzyme-Free Glucose Sensing with Polyaniline-Decorated Flexible CNT Fiber Electrode (Polyaniline을 이용한 CNT fiber 유연 전극 기반의 비효소적 글루코스 검출)

  • Song, Min-Jung
    • Korean Chemical Engineering Research
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    • v.60 no.1
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    • pp.1-6
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    • 2022
  • As the demand for wearable devices increases, many studies have been studied on the development of flexible electrode materials recently. In particular, the development of high-performance flexible electrode materials is very important for wearable sensors for healthcare because it is necessary to continuously monitor and accurately detect body information such as body temperature, heart rate, blood glucose, and oxygen concentration in real time. In this study, we fabricated the nonenzymatic glucose sensor based on polyaniline/carbon nanotube fiber (PANI/CNT fiber) electrode. PANI layer was synthesized on the flexible CNT fiber electrode through electrochemical polymerization process in order to improve the performance of a flexible CNT fiber based electrode material. Surface morphology of the PANI/CNT fiber electrode was observed by scanning electron microscopy. And its electrochemical characteristics were investigated by chronoamperometry, cyclic voltammetry, electrochemical impedance spectroscopy. Compared to bare CNT fiber electrode, this PANI/CNT fiber electrode exhibited small electron transfer resistance, low peak separation potential and large surface area, resulting in enhanced sensing properties for glucose such as wide linear range (0.024~0.39 and 1.56~50 mM), high sensitivity (52.91 and 2.24 ㎂/mM·cm2), low detection limit (2 μM) and good selectivity. Therefore, it is expected that it will be possible to develop high performance CNT fiber based flexible electrode materials using various nanomaterials.