• Journal of Sericultural and Entomological Science
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• v.34 no.2
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• pp.32-40
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• 1992

Many studies have been carried out on the graft finishing in order to improve the quality of silk fiber. Various vinyl monomers, for instance, styrene, methylmethacrylate, 2-hydroxyeth-ylmethacrylate and methacrylamide, have been used practically up to date. Among these monomers, methacrylamide has been applied as the most favourable monomer onto silk fibers in recent years. The polymerization mechanism about styrene- and methylmethacrylate-grafted silk fiber has been studied by many researchers. They proposed that free radicals were formed and vinyl monomers were polymerized in silk fibroin by graft polymerization mechanism, while active sites were varied by the types of monomer and initiator as well as by the reaction condition. In general. there is another Opinion that monomers are polymerized and impregnated in the internal side of the fiber by homopolymerization, which has not been proved experimentally yet More than 10 years have been passed since methacrylamide was applied on the silk fiber, and at the present time most finishings are being achieved by methacrylamide. However, no attention has been paid to the polymerization mechanism of the methacrylamide-treated silk fiber yeL In this paper, the treatments of methacrylamide on silk fibers were studied in aqueous solution using potassium persulfate as an initiator. The polymerization mechanism of the methacrylamide-treated silk fibers was investigated and analyzed on the basis of the results of infrared spectroscopy, amino acid analysis and scanning electron microscopy. From the results of these instrumental analyses, it can be suggested that polymerization mechanism about the methacrylamide-treated silk fibers is not performed by graft polymerization which has been accepted generally in styrene and methylmethacrylate-grafted silk fibers. The different mechanism is supposed to be due to the difference in monomer types, initiator types and treatment conditions.

• Transactions on Control, Automation and Systems Engineering
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• v.4 no.1
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• pp.62-74
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• 2002

The tracking of a reference temperature trajectory in a polymerization batch reactor is a common problem and has critical importance because the quality control of a batch reactor is usually achieved by implementing the trajectory precisely. In this study, only energy balances around a reactor are considered as a design model for control synthesis, and material balances describing concentration variations of involved components are treated as unknown disturbances, of which the effects appear as time-varying parameters in the design model. For the synthesis of a tracking controller, a method combining the input-output linearization of a time-variant system with the parameter estimation is proposed. The parameter estimation method provides parameter estimates such that the estimated outputs asymptotically follow the measured outputs in a specified way. Since other unknown external disturbances or uncertainties can be lumped into existing parameters or considered as another separate parameters, the method is useful in practices exposed to diverse uncertainties and disturbances, and the designed controller becomes robust. And the design procedure and setting of tuning parameters are simple and clear due to the resulted linear design equations. The performances and the effectiveness of the proposed method are demonstrated via simulation studies.

• Proceedings of the KSME Conference
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• 2007.05a
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• pp.409-414
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• 2007

Wettability of solid surfaces with liquids is governed by the chemical properties and the microstructure of the surfaces. We report on the preparation of liquid-repellent surfaces using surface-attached monolayers of perfluorinated polymer molecules on porous silica substrates. A covalent attachment of the polymer molecules to the substrate is achieved by generation of the polymer chains through starting a surface-initiated radical-chain polymerization of a fluorinated monomer. To this, self-assembled monolayers of azo initiators are attached to silica substrates, which are used to kick off the polymerization reaction in situ. The growth of the fluorinated polymer films and the characterization of the obtained surfaces by surface plasmon spectroscopy, XPS, and contact angle measurements is described. It is shown that perfluorinated polymer films can be grown with controlled thicknesses on flat and even on porous silica surfaces, essentially without changing the surface roughness. The combination of the low surface energy coating and the surface porosity allows generation of materials which are both water and oil repellent.

• Elastomers and Composites
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• v.47 no.1
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• pp.30-35
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• 2012

Novel bio-polybutadiene polymers with controlled molecular weight (MW), MW distribution, chemical composition and micro structure were synthesized by a living anionic polymerization of butadiene and the subsequent coupling reaction of the thus obtained living polybutadiene and a vegetable oil. Anionic polymerization of butadiene was carried out in THF solvent using n-BuLi initiator. The resulting living polybutadienyllithium polymer was then reacted with epoxidized soybean oil (ESO) to obtain a star-polymer of polybutadiene and vegitable oil. Three different bio-elastomers were prepared by coupling living polybutadienes of MWs 1000, 5000 and 1000g/mol with ESO. The molecular structure and MW of the polybutadienes and bioelastomers were characterized by $^1H$-NMR, FTIR and GPC techniques.

• Korean Membrane Journal
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• v.8 no.1
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• pp.67-73
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• 2006

Transparent materials are well known but preparation of transparent poly 2-hydroxyethyl methacrylate {poly (HEMA)} material by varying solvent is a new one and economically reliable. This material is prepared from hydroxyl based monomer HEMA by radical polymerization using benzoyl peroxide (BPO) as initiator and isobutanol, 2-butanol, 1-butanol, hexane and toluene as a solvent. The reaction temperature, time and stirring speed were set at $70^{\circ}C$, 4 hrs and 150 rpm, respectively. The polymer was characterized for functional group by IR spectroscopy. It was observed that the intensity of band at $1637 cm^{-1}$ a characteristic band of C=C stretching disappeared indicating that it was completely consumed after polymerization. It was observed that swelling percentage increases with increase as time passes but after a certain time a constant swelling percentage is achieved. SEM pictures reveals that poly (HEMA) prepared by different solvent shows pore with a distinguishable void up to several micrometers. The BET surface area, cumulative pore volume and average pore diameter is greater in poly (HEMA) prepared by hexane as a solvent compared to other solvents. Poly (HEMA) prepared by 1-butanol as a solvent shows higher glass transition temperature compared to other solvents. Poly (HEMA) prepared by different solvents shows $90{\sim}94%$ light transmission property from light transmission measurement and looks transparent.

• Macromolecular Research
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• v.15 no.7
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• pp.633-639
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• 2007

A variety of NMR techniques were applied to the micro-chemical structural characterization of polyanilines prepared via an efficient synthetic method in a self-stabilized dispersion medium in which the polymerization was conducted in a heterogeneous organic/aqueous biphasic system without any stabilizers. Here, the monomer and growing polymer chain were shown to function simultaneously as a stabilizer, imparting compatibility for the dispersion of the organic phase, and as a form of flexible template in an aqueous reaction medium. Polymerizations predicated on this concept generated polyanilines with a low defect content: solution state $^{13}C-NMR$ and solid $^{13}CDD/CP/MAS$ spectroscopy indicated that the synthesized HCPANi and its soluble derivative, HCPANi-t-BOC, evidenced distinctly different NMR spectra with fewer side peaks, as compared to conventionally prepared PANis, and the complete structural assignments of the observed NMR peaks could be determined via the combination of both 1D and 2D techniques. Ortho-linked defects in HCPANi were estimated to be as low as 7%, as shown by a comparison of the integration of the carbonyl carbon resonance peaks.

• Macromolecular Research
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• v.9 no.3
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• pp.150-156
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• 2001

Polystyrenes(PS) were grafted onto polypropylene(PP) in the PP solution by ultrasonic irradiation-initiated polymerization of styrene. The resulting products consisted of mixtures of homopolymers and PP-PS copolymer because of the homopolymerization of styrene itself and copolymerization with PP. The dependency of the designated polymerization on sonication times was investigated to monitor the evolution lion of the copolymerization. Formation of the PP-PS copolymer was confirmed by FTIR analysis of the reaction products after a proper separation procedure of free PS and PP-PS copolymer. It was found that the tendency for the formation of PP-PS copolymer was closely related with the phase behavior of the PP/styrene mixture which was also influenced by sonication time. In order to verify the effectiveness of the PP-PS copolymer as a compatibilizer for PP/PS blend, melt mixing of PP/PS/PP-PS was performed in a batch mixer. During the mixing, the average torque was higher for the blend containing PP-PS copolymer influencing compatibilization. In accordance with the results from FRIR analysis and torque measurement, the PS domain size remarkably decreased in the PP/PS/PP-PS blend.

• Macromolecular Research
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• v.15 no.2
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• pp.173-177
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• 2007

Living anionic and cationic polymerizations have been combined to prepare various types of comb-like copolymers composed of polystyrene (PS) and polyisoprene (PI) blocks, with a precisely controlled architecture. According to the relative placement of these elementary building blocks, combs with randomly distributed PS and PI or with poly(styrene-b-isoprene) diblock branches (I & II, respectively) can be prepared. The reaction procedure initially includes the synthesis of a poly(chloroethylvinyl ether) using living cationic polymerization, which is used as the reactive backbone to successively graft $PS^-Li^+$ and $PI^-Li^+$ or $PI-b-PS^-Li^+$ to obtain structures (I) or (II). The synthesis of Janus-type PS-comb-b-PI-combs (III) initially involves the synthesis of a diblock backbone using living cationic polymerization, which bears two distinct reactive functions having either a protected or activated form. Living $PS^-Li^+$ and $PI^-Li^+$ are then grafted, in two separate steps, onto each of the reactive functions of the backbone, respectively.

• Macromolecular Research
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• v.14 no.3
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• pp.373-382
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• 2006

A series of crosslinkable, waterborne polyurethanes (I-WBPUs) were prepared by in-situ polymerization using isophorone diisocyanate (IPDI)/poly(tetramethylene oxide) glycol (PTMG, $M_n$=2,000)/dimethylol propionic acid (DMPA)/ethylene diamine (EDA)/triethylamine (TEA)/aminoplast[hexakis(methoxymethyl)melamine (HMMM)] as a crosslinking agent. Typical crosslinkable, waterborne polyurethanes (B-WBPUs) blended from WBPU dispersion and aqueous HMMM solution was also prepared to compare with the I-WBPUs. The crosslinking reaction between WBPU and HMMM was verified using FTIR and XPS analysis. The effect of the HMMM contents on the dynamic mechanical thermal, thermal, mechanical, and adhesion properties of the I-WBPU and B-WBPU films were investigated. The storage modulus(E'), glass transition temperatures of the soft segment ($T_{gs}$) and the amorphous regions of higher order ($T_{gh}$), melting temperature ($T_m$), integral procedural decomposition temperature (IPDT), residual weight, $T_{10%}$ and $T_{50%}$ (the temperature where 10 and 50% weight loss occurred), tensile strength, initial modulus, hardness, and adhesive strength of both I-WBPU and B-WBPU systems increased with increasing HMMM content. However, these properties of the I-WBPU system were higher than those of the B-WBPU system at the same HMMM content. These results confirmed the in-situ polymerization used in this study to be a more effective method to improve the properties of the WBPU materials compared to the simple blending process.

• Journal of the Korean Society of Safety
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• v.19 no.1
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• pp.81-87
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• 2004

Composite particles using inorganic and organic chemicals were synthesized and the results of those reaction were compared to variation of temperature and agitation speed in presence of $CaCO_3$ which was adsorbed SDBS. Also the synthesises were optimized according to conversion rate of composite particles. In inorganic/organic core-shell composite particle polymerization, $CaCO_3$ adsorbed by 0.5wt% surfactant SDBS was prepared initially and then core $CaCO_3$ was encapsulated by sequential emulsion polymerization using MMA at the addition of APS 3.16${\times}$$10^{-3}$mol/L to minimize the coagulated PMMA particle itself during MMA shell polymerization. Encapsulated PMMA on $CaCO_3$ as inorganic/organic core-shell particles was verified by FT-IR and DSC analysis. It was found that the $CaCO_3$ was very well encapsulated by PMMA as shell. The surfaces were distinctly found as spindle shape and broad particle distribution after capsulation.