• Title/Summary/Keyword: polymerization reaction

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Synthesis and Their Properties of PP Graft Copolymers by E-beam Radiation and Vapor Phase Reaction (전자선 조사 기상 반응에 의한 PP 기재 공중합체의 합성과 특성)

  • 황택성;박진원;이재천
    • Polymer(Korea)
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    • v.26 no.3
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    • pp.287-292
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    • 2002
  • Graft copolymerization of styrene and glycidyl methacrylate (GMA) to the peroxidized polypropylene (PP) fabric with E-beam in $O_2$ atmosphere was carried out in vapor phase with benzoyl peroxide (BPO) as an initiator. The degree of grafting of copolymers was increased with the increase of the reaction temperature and the highest degree of grafting was obtained at $70^{\circ}C$ with styrene, and at $80^{\circ}C$ with GMA. The highest degree of grafting of styrene grafted PP according to reaction time was higher than that of GMA grafted PP. In vapor phase graft polymerization, the degree of grafting of copolymers according to water composition in monomer mixture was effected by the boiling temperature of monomers.

Synthesis of Silicone/Acrylic Resins for Super-Weatherable Coatings (초내후성 도료용 실리콘/아크릴수지의 합성)

  • Kim, Seong-Kil;Choi, Yong-Ho;Park, Hong-Soo
    • Journal of the Korean Applied Science and Technology
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    • v.16 no.2
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    • pp.171-177
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    • 1999
  • The objectives of this study is to investigate the optimum reaction conditions and to identify the product formula in the synthesis of a silicone/acrylic resin that curing in moisture at room temperature. By the addition polymerization of monomers, n-butyl acrylate, methyl methacrylate, n-butyl methacrylate, and 3-methacryloxypropyltrimethoxysilane. a quarter polymer was obtained. Among various initiators investigated in this study, 2.2'-azobisisobutyronitrille was found to be the most suitable initiator. The optimum reaction conditions found in this study are 70 wt% of initial solvent amount, 120 minutes of dropping time, 3 times of initiator addition, $82{\sim}105^{\circ}C$ of reaction temperature, and 8 hrs of reaction time. Also, number average molecular weight of $11700{\sim}33100$ and molecular weight distribution of $1.81{\sim}3.44$ were obtained.

Preparation and Characterization of High Molecular Weight Poly(butylene succinate)

  • Han, Yang-Kyoo;Kim, Sung-Rim;Kim, Jinyeol
    • Macromolecular Research
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    • v.10 no.2
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    • pp.108-114
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    • 2002
  • Poly(butylene succinate) (PBS) prepolymers were prepared by the condensation polymerization of 1,4-butanediol (1,4-BD) and succinic atid (SCA) in the presence of titanium (VI) isoproxide(TPI) catalyst. The PBS prepolymers reacted with 1,4-BD or SCA to obtain hydroxyl or carboxylic acid group terminated PBS. High molecular weight linear or branched PBS was synthesized by a coupling reaction between hydroxyl and carboxylic acid group terminated PBS, or by a branching reaction between carboxylic acid group terminated PBS and glycerol as a branching agent. The weight average molecular weight of the prepared linear or branched PBS was in the range of 100,000-220,000. Both melting point and thermal stability of the high molecular weight linear and branched PBSs were somewhat higher than those of general PBS. From a tensile behavior by Instron test, modulus, tensile strength and elongation at break improved with increase in the molecular weight of the prepared PBS through the coupling or the branching reaction. In particular, the high molecular weight linear PBS had about 2.5 times higher value in modulus than the branched one.

Synthesis and Characterization of Low Molecular Weight Poly(methyl acrylate)-b-Polystyrene by a Combination of ATRP and Click Coupling Method

  • Hasneen, Aleya;Kim, Su-Jeong;Paik, Hyun-Jong
    • Macromolecular Research
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    • v.15 no.6
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    • pp.541-546
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    • 2007
  • The combination of atom transfer radical polymerization (ATRP) and click chemistry was employed for the efficient preparation of well-defined block copolymers. Bromo terminated poly(methyl acrylate) (pMA-Br) was prepared by an ATRP initiator, ethyl-2-bromoisobutyrate (EBiB). Subsequently, the bromine chain end of pMA-Br was converted to an azide group by simple nucleophilic substitution reaction. ${\alpha}-Alkyn-{\omega}-bromo-functionalized$ polystyrene was also synthesized by ATRP using the alkyn-functionalized initiator, propargyl-2-bromoisobutyrate (PgBiB). In both cases, the conversion was limited to a low level to ensure a high degree of chain end functionality. Then the coupling reaction between the azide end group in $pMA-N_3$ and alkyn-functionalized PgBiB-pSt was performed by Cu(I)catalysis. This coupling reaction was monitored by gel permeation chromatography (GPC). The synthesized block copolymer was characterized by FT-IR, $^1H-NMR$ spectroscopy and $^1H-^1H$ COSY correlation spectroscopy.

Suzuki-Miyaura Cross-coupling Reaction Catalyzed by Nickel Nanoparticles Supported on Poly(N-vinyl-2-pyrrolidone)/TiO2-ZrO2 Composite

  • Kalbasi, Roozbeh Javad;Mosaddegh, Neda
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2584-2592
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    • 2011
  • Nickel nanoparticle-poly(N-vinyl-2-pyrrolidone)/$TiO_2-ZrO_2$ composite (Ni-PVP/$TiO_2-ZrO_2$) was prepared by in situ polymerization method. The physical and chemical properties of Ni-PVP/$TiO_2-ZrO_2$ were investigated by XRD, FT-IR, BET, TGA, SEM and TEM techniques. The catalytic performance of this novel heterogeneous catalyst was determined for the Suzuki-Miyaura cross-coupling reaction between aryl halides and phenylboronic acid in the presence of methanol-water mixture as solvent. The effects of reaction temperature, the amount of catalyst, amount of support, solvent, and amount of metal for the synthesis of Ni-PVP/$TiO_2-ZrO_2$, were investigated as well as recyclability of the heterogeneous composite. The catalyst used for this synthetically useful transformation showed considerable level of reusability besides very good activity.

Synthesis, Characterization and Application of Poly(4-Methyl Vinylpyridinium Hydroxide)/SBA-15 Composite as a Highly Active Heterogeneous Basic Catalyst for the Knoevenagel Reaction

  • Kalbasi, Roozbeh Javad;Kolahdoozan, Majid;Massah, Ahmadreza;Shahabian, Keinaz
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2618-2626
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    • 2010
  • In this paper poly (4-methyl vinylpyridinium hydroxide)/SBA-15 composite was prepared as a highly efficient heterogeneous basic catalyst by in situ polymerization method for the first time. It was characterized by XRD, FT-IR, BET, TGA, SEM and back titration using NaOH. This catalyst exhibited the excellent catalytic activities for the Knoevenagel condensation of various aldehydes with ethyl cyanoacetate. Over this catalyst, ${\alpha},{\beta}$-unsaturated carbonyl compounds were obtained in the reasonable yield at $95^{\circ}C$ in 10 - 30 min in $H_2O$ as a solvent with a 100% selectivity to the condensation products. Catalyst could be easily recycled after the reaction and it could be reused without the significant loss of activity/selectivity performance. No by-product formation, high yields, short reaction times, mild reaction conditions and operational simplicity with reusability of the catalyst were the salient features of the present synthetic protocol. Presence of $H_2O$ as a solvent was also recognized as a "green method".

Studies on Telomerization (I) Telomerization of Vinyl Acetate with Chlorinated Hydrocarbons (Telomerization 에 關한 硏究 (I) Vinyl Acetate 와 Chlorinated Hydrocarbons 과의 Telomerization 에 關하여)

  • Shim, Jyong-Sup;Hong, Suck-Joo
    • Journal of the Korean Chemical Society
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    • v.6 no.1
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    • pp.88-93
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    • 1962
  • The telomerization of vinyl acetate with carbon tetrachloride, chloroform and monochlorobenzene were investigated with respect to the synthesis of those telomers, properties and molecular weights of the formed telomers, and reaction mechanisms. Vinyl acetate reacted with carbon tetrachloride and chloroform to form telomers at 70-90$^{\circ}C$ and 60-70$^{\circ}C$, respectively and it formed polymer with monochlorobenzene. As a chain transfer agent, carbon tetrachloride was more effective than chloroform. In the telomerization of vinyl acetate and carbon tetrachloride: 1) The average molecular weight of the telomer decreased as the mole ratio of carbon tetrachloride to vinyl acetate increased. The optimum conditions for the highest yield of the telomer were as follows: Mole ratio of carbon tetrachloride to vinyl acetate : 2.5 Reaction time : 20 hours. 2) As the reaction proceeded, the refractive index and average molecular weight of the telomer increased rapidly in the first 10 hours but the increase was slow through the next 10 hours, so that, the average recurring number(n) of taxogen in the final product reached an almost definite value, i.e., 3. The telomer formed in the telomerization of vinyl acetate with carbon tetrachloride and chloroform turned to brown color in the air due to decomposition or polymerization. The suggested telomerization mechanism was supported by the hexachloroethane detected in the course of reaction.

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Gelation of Rapeseed Protein Induced with Microbial Transglutaminase (미생물성 Transglutaminase에 의한 유채단백질의 겔화)

  • Hyun, Eun-Hee;Kang, Yeung-Joo
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1262-1267
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    • 1999
  • Optimum reaction conditions for gel formation of rapeseed, Brassica napus, protein catalyzed by microbial TGase(transglutaminase) were evaluated by measuring breaking strength and deformation of gel. The polymerization of the protein gel was ascertained by SDS-PAGE and content of GL crosslinking$[{\varepsilon}-({\gamma}-glutamyl)lysine]$. In the reaction between rapeseed protein and TGase at $45^{\circ}C$ for 60 min, the breaking strength and deformation of the gel was the maximum at the ratio of 1 : 40 of enzyme to substrate. 10%(w/v) of rapeseed protein concentrate was optimum for gel production. The maximum breaking strength and deformation was shown at $45^{\circ}C$ The breaking strength increased linearly up to 90 min of the reaction time and remained unchanged. The breaking strength and deformation by TGase treatment was pH dependent and pH 7 was optimum for 10% rapeseed protein solution. SDS-PAGE analysis indicated that new band of highmolecular polymers were formed by the enzyme reaction, with disappearing the original bands of rapeseed protein. According to HPLC analysis. the content of GL crosslinking was increased from 0 to $7.14\;{\mu}mol/g$ gel for 90 min of the reaction time.

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Studies on the Graft Polymerization of Polyethyleneglycol Monomethacrylate onto Chitosan and Drug(Vitamin B12) Permeation Behavior (키토산과 폴리에틸렌글리콜 모노메타크릴레이트의 그라프트중합과 약물(Vitamin B12)방출에 관한 연구)

  • Chung, Joo-Eun;Chung, Byung-Ok;Chang, Byung-Kwon;Choi, Kyu-Suk
    • Applied Chemistry for Engineering
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    • v.5 no.3
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    • pp.524-536
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    • 1994
  • Chitosan is known to be a good biocompatible natural polymer. Polyethyleneglycol monomethacrylates(PEGM) were grafted onto chitosan and their reaction conditions and properties of the graft polymers obtained were estimated. Using ceric ammonium nitrate(CAN) as the initiator, the optimum condition for graft polymerization was determined amount of the initiator and monomer concentrations and reaction time. Grafting yields such as total conversion, the percentage of grafting and the efficiency of grafting were calculated and examined the optimum reaction condition for high grafting yields. The percentage of grafting and total conversion were maximum at condition that the concentration of initiator was $4{\sim}5{\times}10^{-3}M$, the concentration of monomer was 0.5~0.6M, the reaction time was 2~3 hours and the reaction temperature was about $40^{\circ}C$. Thermal characteristics, solubility for chitosan solvents and inherent viscosity of synthesized graft copolymers were investigated. In high initiator concentration, characteristics of chitosan were greatly diminshed. In case of inherent viscosities, chitosan-g-PE-90 was 2.81 dl/g, chitosan-g-PE-200, 3.01dl/g and chitosan-g-PE-350, 4.93dl/g. And a tendency of viscosity increase depending on the length of ethylene oxide residue was confirmed. Degree of swelling, tensile strength, elongation of membrane prepared from graft copolymers were determined. Properties of graft copolymers were affected by percentage of grafting and length of ethylene oxides residue in polyethylene glycol monomethacrylates. Tensile strength, elongation and degree of swelling of graft copolymers were remarkably improved than chitosan. As percentage of grafting increased, the amount of drug permeation was also increased.

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The Characteristics of Mesophase Pitch Prepared by Heterogeneous Fluorination Process from Pyrolysis Fuel Oil (열분해잔사유로부터 불균일계 불소화공정에 의해 제조된 메조페이스 피치의 특성)

  • Kim, Do Young;Kim, Ji-Hyun;Lee, Hyung-Ik;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.27 no.5
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    • pp.537-542
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    • 2016
  • In this study, we have prepared mesophase pitch from pyrolysis fuel oil (PFO) by heterogeneous reforming process. This process was conducted by direct fluorination at various temperature and followed by the heat treatment at $390^{\circ}C$. The reformed pitch was then investigated by softening point analysis, elemental analysis, fourier-transform infrared spectroscopy, high resolution X-ray diffraction and polarization microscope analysis. Carbon contents of reformed pitch increased according to increasing the reaction temperature of fluorination, while oxygen, nitrogen and sulfur contents were completely eliminated. As the fluorination temperature increased, the creation, growth, coalescence and alignment process of mesophase spheres were observed. Also the interlayer spacing of carbon hexagonal planar structure decreased, while its crystalline size increased. In addition, aromatic ring compound contents increased by the condensation polymerization of aliphatic compound. These results can be attributed to the radical reactivity of the fluorine increased as the reaction temperature increased. It was considered that the fluorination reaction could help PFO to generate aromatic compounds, via promoting polymerization by radical reaction.