• Title/Summary/Keyword: polymerization reaction

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Characterizations of Modified Silica Nanoparticles(I)

  • Min, Seong-Kee;Park, Chan-Young;Lee, Won-Ki;Seul, Soo-Duk
    • Korean Journal of Materials Research
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    • v.22 no.6
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    • pp.275-279
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    • 2012
  • (3-mercaptopropyl)trimethoxysilane (MPTMS) was used as a silylation agent, and modified silica nanoparticles were prepared by solution polymerization. 2.0 g of silica nanoparticles, 150 ml of toluene, and 20 ml of MPTMS were put into a 300 ml flask, and these mixtures were dispersed with ultrasonic vibration for 60 min. 0.2 g of hydroquinone as an inhibitor and 1 to 2 drops of 2,6-dimethylpyridine as a catalyst were added into the mixture. The mixture was then stirred with a magnetic stirrer for 8 hrs. at room temperature. After the reaction, the mixture was centrifuged for 1 hr. at 6000rpm. After precipitation, 150 ml of ethanol was added, and ultrasonic vibration was applied for 30 min. After the ultrasonic vibration, centrifugation was carried out again for 1 hr. at 6000rpm. Organo-modification of silica nanoparticles with a ${\gamma}$-methacryloxypropyl functional group was successfully achieved by solution polymerization in the ethanol solution. The characteristics of the ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) were examined using X-ray photoelectron spectroscopy (XPS, THERMO VG SCIENTIFIC, MultiLab 2000), a laser scattering system (LSS, TOPCON Co., GLS-1000), Fourier transform infrared spectroscopy (FTIR, JASCO INTERNATIONL CO., FT/IR-4200), scanning electron microscopy (SEM, HITACHI, S-2400), an elemental analysis (EA, Elementar, Vario macro/micro) and a thermogravimetric analysis (TGA, Perkin Elmer, TGA 7, Pyris 1). From the analysis results, the content of the methacryloxypropyl group was 0.98 mmol/g and the conversion rate of acrylamide monomer was 93%. SEM analysis results showed that the organo-modification of ultra-fine particles effectively prevented their agglomeration and improved their dispensability.

Synthesis and Applications of Reactive Polymer Modifiers for Asphalt(1) (아스팔트용 반응성 고분자 개질제 합성 및 적용(1))

  • Hwang, Ki-Seob;Ahn, Won-Sool;Suh, Soong-Hyuck;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.31 no.1
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    • pp.68-73
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    • 2007
  • This study is on the synthesis of reactive polymer modifiers by emulsion polymerization to improve properties of asphalt for paving. Styrene, methyl methacrylate (MMA), isoprene and glycidyl methacrylate (GMA) which has epoxy ring to react with carboxyl group of asphaltene were used to synthesize polymer modifiers. Modifiers with various composition were tested miscibility with asphalt. Modifiers which showed good miscibility with asphalt were investigated by DSC for $T_g$. Existence of epoxy rings and their reaction with asphaltene wore investigated by FTIR. Molecular structures of synthesized modifiers were confirmed by $^1H-NMR$. The synthesized modifiers which showed good miscibility had their $Tg's$ in the range of $37.5{\sim}56.5^{\circ}C$ and had isoprene contents of 30 wt%. They showed good miscibility in the 1 and 2 wt% concentrations, but not in the 3 wt% concentration.

Improvement of Thermal Stability of Polyethylene Lithium-ion Battery Separator via Coating with Polymers Synthesized from Bis-GMA Derivatives (Bis-GMA 유도체로부터 제조된 고분자 코팅에 의한 리튬이차전지용 폴리에틸렌 격리막의 고온 안정성 향상)

  • Im, Hyun-Gu;Hong, Ji-Hye;Kim, Chang-Keun
    • Polymer(Korea)
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    • v.34 no.6
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    • pp.517-521
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    • 2010
  • Microprous polyethylene (PE) membranes are widely used as lithium-ion battery separators. A separator having higher meltdown temperature than PE separator is still required for useful safety feature at a high temperature. To enhance meltdown temperature of PE separator, it was coated with polymers synthesized from bis-GMA derivatives by radical polymerization. Polymer was not formed when bis-GMA monomer having a high viscosity was used, while polymers were formed when bis-GMA derivatives having a low viscosity were used. When the separator was coated with polymer synthesized from reaction mixture containing proper amount of bis-GMA derivative, its meltdown temperature were increased up to $160^{\circ}C$ without reduction in the air permeability.

Carboxy-Terminal Region of a Thermostable CITase from Thermoanaerobacter thermocopriae Has the Ability to Produce Long Isomaltooligosaccharides

  • Jeong, Woo Soo;Kim, Yu-Ri;Hong, Seong-Jin;Choi, Su-Jeong;Choi, Ji-Ho;Park, Shin-Young;Woo, Eui-Jeon;Kim, Young Min;Park, Bo-Ram
    • Journal of Microbiology and Biotechnology
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    • v.29 no.12
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    • pp.1938-1946
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    • 2019
  • Isomaltooligosaccharides (IMOs) have good prebiotic effects, and long IMOs (LIMOs) with a degree of polymerization (DP) of 7 or above show improved effects. However, they are not yet commercially available, and require costly enzymes and processes for production. The N-terminal region of the thermostable Thermoanaerobacter thermocopriae cycloisomaltooligosaccharide glucanotransferase (TtCITase) shows cyclic isomaltooligosaccharide (CI)-producing activity owing to a catalytic domain of glycoside hydrolase (GH) family 66 and carbohydrate-binding module (CBM) 35. In the present study, we elucidated the activity of the C-terminal region of TtCITase (TtCITase-C; Met740-Phe1,559), including a CBM35-like region and the GH family 15 domain. The domain was successfully cloned, expressed, and purified as a single protein with a molecular mass of 115 kDa. TtCITase-C exhibited optimal activity at 40℃ and pH 5.5, and retained 100% activity at pH 5.5 after 18-h incubation. TtCITase-C synthesized α-1,6 glucosyl products with over seven degrees of polymerization (DP) by an α-1,6 glucosyl transfer reaction from maltopentaose, isomaltopentaose, or commercialized maltodextrins as substrates. These results indicate that TtCITase-C could be used for the production of α-1,6 glucosyl oligosaccharides with over DP7 (LIMOs) in a more cost-effective manner, without requiring cyclodextran.

Synthesis and Analysis of Modified Polyesters Containing Phosphorus and Chlorine for Flame-Retardant Coatings (난연도료용 인과 염소 함유 변성폴리에스터의 합성 및 분석)

  • Park, Hong-Soo;Ahn, Sung-Hwan;Jo, Hye-Jin;Shim, Il-Woo;Hahm, Hyun-Sik;Kim, Seung-Jin;Kim, Seong-Kil
    • Journal of the Korean Applied Science and Technology
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    • v.23 no.1
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    • pp.26-36
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    • 2006
  • The aim of this study is to synthesis basic resins for the preparation of PU flame-retardant coatings that contain phosphorus and chlorine. After synthesizing intermediates of tetramethylene bis(orthophophate) (TMBO) and neohexanediol trichlorobenzoate (TBA-adduct), the condensation polymerization was performed with the intermediates, 1,4-butanediol, and adipic acid to obtain four-component copolymers. In the condensation polymerization, the content of phosphorus was fixed to be 2%, and the content of trichlorobenzoic acid (TBA) that provides chlorine component was varied to be 10, 20, and 30wt%, and we designated the prepared modified polyesters containing chlorine and phosphorus as TTBA-10C, TTBA-20C and TTBA-30C. Average molecular weight and polydispersity index of the prepared TTBAs decreased with increasing TBA content because of the increase in the number of hydroxyl groups that retards reaction. We found that the thermal stability of the prepared TTBAs increased with chlorine content at high temperatures.

Dispersion polymerization of styrene and Methylmethacrylate using macromonomers as a reactive stabilizer

  • Jung, Hye-Jun;Lee, Kang-Seok;Choe, Soon-Ja
    • Proceedings of the Polymer Society of Korea Conference
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    • 2006.10a
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    • pp.86-88
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    • 2006
  • The novel linear- (V-LUM) and cross-type macromonomers (C-VUM) of vinyl-terminated bifunctional polyurethane were synthesized and applied to the dispersion polymerization of styrene and MMA in ethanol. The existence of the vinyl terminal groups and the grafted macromonomer with styrene and PMMA was verified using 1H NMR and 13C NMR. Monodisperse polystyrene (PS) microspheres were successfully obtained above 15 wt % of macromonomer relative to styrene. The macromonomer can efficiently stabilize higher surface area of the particles compared to a conventional stabilizer, PVP. The grafting ratio of the PS calculated from 1H NMR linearly increased up to 0.048 with 20 wt % of the macromonomer and the high molecular weights (501,300 g/mol) of PS with increased glass transition and enhanced thermal stability were obtained. Furthermore, the stable and monodisperse PMMA microspheres having a weight-average diameter of $5.09{\mu}m$ and a good uniformity of 1.01 were obtained with 20 wt% L-VUM. The molecular weight increased, but the size of the PMMA particles decreased with the macromonomer concentration due to the increased stabilizing effect. The molecular weight of the PMMA was approximately two fold higher than that by a conventional PVP. The L-VUM acts as a reactive stabilizer, which gives polyurethane-grafted PS or PMMA with a high molecular weight. In addition, the XPS result showed that the C-PS (PS using the C-VUM) was anchored with a larger amount of PEG than that of the L-PS (PS using the L-VUM) on the particle surface. Thus, the reaction and stabilizing mechanism of the macromonomers for the formation of PS particles is proposed.

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Atom Transfer Radical Polymerization of [Poly(ethylene glycol)methyl ether] Methacrylate Using an Amide-Based Initiator (아미드기를 가지는 개시제를 이용한 [Poly(ethylene glycol)Methyl Ether] Methacrylate의 원자 이동 라디칼 중합)

  • Lee, Hyo-Kyung;Lee, Sun-Gu;Paik, Hyun-Jong
    • Polymer(Korea)
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    • v.31 no.6
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    • pp.550-554
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    • 2007
  • Atom transfer radical polymerization (ATRP) has been widely used in bioconjugation as it is an efficient and facile method to prepare polymers with pre-designed structures. Quite often, bioconjugation with proteins employs primary amines in proteins as a functional group to attach an initiator. When 2-bromoisobutryl bromide, the most widely used precursor for ATRP initiator, is used, ${\alpha}-halo$ amide initiating groups are formed in the proteins, which are known to exhibit slow initiation behavior in the ATRP process. Here we studied the ATRP of [poly(ethylene glycol)methyl ether] methacrylate (PEGMA) using amide-based initiator. PEGMA differs for both the nature and size of the polymer side branches and shows good solubility in water and a property that made it an ideal candidate for biomaterials. While normal ATRP produced ill-defined p(PEGMA) with amide based initiators, the halogen exchange method and the external additional of deactivator effectively improved the control of ATRP of PEGMA.

Preparation of Ampholyte Grafted Hollow-fiber Membrane and Its Adsorption Characteristic on Metallic Ions (양성전해질 고정막의 제조 및 그것의 금속이온 흡착 특성)

  • Choi, Hyuk-Jun;Park, Sang-Jin;Kim, Min
    • Membrane Journal
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    • v.20 no.2
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    • pp.151-158
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    • 2010
  • This paper presents the synthesis of ampholyte immobilized hollow-fiber membranes and adsorption characteristic of metallic ions. This is prepared by radiation induced grafting polymerization of an epoxy group containing Glycidyl methacrylate (GMA) onto an existing polyethylene porous hollow-fiber membrane. Ampholyte ion-exchanged alkalic group, $-NH_2$ (amine function) of Taurine (TAU) is reacted with glycidyl of GMA for the synthesis of stable membrane. However, Sodium sulfite (SS) membrane is also prepared by making chemical bonds with GMA of porous hollow-fiber membrane for the comparison of adsorption characteristic of metallic ions. These are called as TAU and SS membranes, respectively. It is shown that TAU membrane shows a steady flux, 0.9 m/h regardless of the density of TAU, while the flux of SS membrane decreases rapidly as the density of $SO_3H$ group increases. SS membrane showed a negligible flux. TAU membrane with the density 0.8 mmol/g shows the amount of metallic ions adsorbed in the following order, Cu > Cd > Mg > Sb > Pb. In general, TAU membrane with high density and reaction time showed the high amount of metallic ions adsorbed and flux.

Molecular weight Control of Polyhydroxybutyrate (PHB) in Recombinant Escherichia coli (재조합 대장균에서의 Polyhydroxybutyrate (PHB)의 분자량 조절)

  • 심상준;안토니신스키
    • KSBB Journal
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    • v.13 no.1
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    • pp.96-100
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    • 1998
  • Two promoters (trc and P$\rho$) were inserted in PHA operon derived from Alcaligenes eutrophus to obtain high chain molecules of polyhydroxybutyrate (PHB) in recombinant Escherichia coli. Newly designed PHA operon was used to control the gene expressions of hydroxybutyric CoA and PHA polymerization, separately. Plasmids containing new synthetic operon was transformed into E. coli DH5$\alpha$ and analyzed for PHB production. Without induction of the PHA biosynthetic operon, PHA synthase which has low activity might supply low concentration of initiator during the polymerization reaction, resulting very high molecular weight of polymer. An increase of PHB average molecular weight was observed with decreased IPTG (isopropyl $\beta$ -Dithiogalactosidase) concentration. When no IPTG was added to the culture of E. coli DH5$\alpha$ /$\rho$ SJS1 which contained two promoters in PHA operon, high chain polymer having an average molecular weight of $2.5{\times}10^7$ was achieved. Analysis of the enzyme activities of PHA biosynthetic enzymes suggests that PHA synthase, the enzyme responsible for polymerizing 3-hydroxybutyric CoA, controls the molecular weight of PHB produced in vivo.

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Synthesis and Analysis of Modified Polyesters Containing Phosphorus and Bromine for Flame-Retardant Coatings (난연도료용 인과 브롬 함유 변성폴리에스터의 합성 및 분석)

  • Park, Hong-Soo;Yoo, Gyu-Yeol;Kim, Ji-Hyun;Yang, In-Mo;Kim, Seung-Jin;Kim, Young-Geun;Jung, Choong-Ho
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.4
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    • pp.319-331
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    • 2007
  • The aim of this study is to enhance the flame retardancy by the synergism effect of phosphorus and bromine groups. The flame-retardant polyurethane coatings containing phosphorus and bromine compounds were synthesized. After synthesizing the intermediate products of tetramethylene bis(orthophosphate) (TBOP) and trimethylolpropane/2,3-dibromopropionic acid (2,3-DBP) [2,3-DBP-adduct], the condensation polymerization was performed with four different monomers of two intermediate products, 1,4-butanediol, and adipic acid to obtain four-components copolymer. In the condensation polymerization, the content of phosphorus was fixed to be 2wt%, and the content of 2,3-DBP that provides bromine component was varied to be 10, 20, and 30wt%, and we designated the prepared modified polyesters containing phosphorus and bromine as DTBA-10C, -20C, -30C. Average molecular weight and polydispersity index of the preparation of DTBAs were decreased with increasing 2,3-DBP content because of increase of hydroxyl group that retards reaction. We found that the thermal stability of the prepared DTBAs increased with bromine content at high temperature.