• Title/Summary/Keyword: thermal polymerization

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Synthesis and Characterization of Very High Molecular Weight Nylon 4 and Nylon 4/6 Copolymers (매우 높은 분자량을 갖는 Nylon 4 및 Nylon 4/6 공중합체의 합성 및 그 특성 분석)

  • Kim, Nam Cheol;Kim, Ji-Heung;Nam, Sung Woo;Jeon, Boong Soo;Yoo, Young-Tai;Kim, Young Jun
    • Polymer(Korea)
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    • v.37 no.2
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    • pp.211-217
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    • 2013
  • Potassium tert-butoxide (t-BuOK) with $CO_2$ or benzoyl chloride (BzC) as a polymerization initiator system was used with crown ether or TMAC as catalyst to synthesize very high molecular weight nylon 4 homo- and copolymers by anionic ring opening polymerization. Effect of different amounts of catalyst, crown ether and TMAC on the polymerization was studied in terms of intrinsic viscosity, yield and thermal properties. By adding crown ether or TMAC, polymers with very higher intrinsic viscosity values were obtained in a high yield. It was possible to synthesize nylon 4 homopolymer with such a high intrinsic viscosity value of 6.36 dL/g. Crown ether was found to be more efficient in terms of intrinsic viscosity and polymer yields than TMAC. Thermal analysis confirmed that molecular weight effect on the thermal properties of both nylon 4 and nylon 4 copolymer was marginal.

Polymerization Behavior of Self-healing Agents for Damage Repair in Composite Materials (복합재 손상보수용 자가치료제의 중합 거동)

  • Oh, Jinoh;Yoon, Sungho;Jang, Seyong
    • Journal of the Korean Society of Propulsion Engineers
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    • v.18 no.5
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    • pp.35-42
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    • 2014
  • Thermal analysis properties and adhesive properties of self-healing agents were evaluated through differential scanning calorimetry, reaction heat measurement, and adhesive shear test. D1E0, D3E1, D1E1, D1E3, and D0E1, depending on the mixing ratio of DCPD and ENB, were considered as self-healing agents. The amount of Grubbs' catalyst, depending on the type of self-healing agents, was varied from 0.1 wt% to 1.5 wt%. In the case of DCPD, the polymerization reaction occurred faster and the stabilized adhesive strength increased as the amount of catalyst increased; however, a large amount of catalyst was required. ENB had excellent reactivity with a small amount of the catalyst; however, high reaction heat was observed at the early stage of polymerization. Thermal analysis properties and adhesive properties of self-healing agents can be controlled by varying a mixing ratio of DCPD and ENB. Among the self-healing agents used for this study, the D3E1 would be one of the most preferable candidates with regard to maximum adhesive strength, reaching time to maximum adhesive strength, stabilized adhesive strength, and reaction heat.

Properties of Eco-friendly Acrylic Resin/Clay Nanocomposites Prepared by Non-aqueous Dispersion (NAD) Polymerization (비수계 분산중합으로 제조된 환경친화성 아크릴수지/나노클레이 복합재료의 특성 연구)

  • Kim, Yeongho;Lee, Minho;Jeon, Hyeonyeol;Lee, Young Chul;Min, Byong Hun;Kim, Jeong Ho
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.120-126
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    • 2016
  • Eco-friendly acrylic resin/clay nanocomposites containing pristine montmorillonite (PM) or modified clays (30B and 25A) were prepared from acrylic and styrenic monomers using non-aqueous dispersion (NAD) polymerization. Effect of nanoclays on physical properties of polymerization product and resulting nanocomposites was investigated. In view of NAD particle stability, addition of nanoclay at the beginning of polymerization is proved to be good. Results of gel fraction, acid value and viscosity of the NAD product showed that nanocomposites containing clay 25A showed better physical properties than the ones with other clays. GPC results exhibit the increase in molecular weight and decrease in polydispersity index for the 25A nanocomposite. Increase in layer distance confirmed from XRD analysis showed good dispersion of 25A in the nanocomposite. Thermal and dynamic mechanical analysis showed that highest glass transition temperature and storage modulus for 25A nanocomposites. These results indicate that 25A nanoclay gives the best properties in the process of non-aqueous dispersion polymerization of acrylic resin/nanoclay nanocomposites.

Early Hydration of Tricalcium Silicate(II) (Tricalcium Silicate의 초기수화반응(II))

  • 오희갑;최상흘
    • Journal of the Korean Ceramic Society
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    • v.24 no.2
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    • pp.133-138
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    • 1987
  • The behavior of CaO and SiO2 in the reaction produced which produced in the early hydration of C3S was studied by XRD and thermal analyzer. Polymerization of hydrated siltcates was also studied by TMS method. TMS derivatives were separated by gaschromatography. Cao/SiO2 molar ratios of the produced CSH gel under the air atmosphere were higher than that in the CO2. Dimerization rate of hydrated silicates was very fast in the early hydration stage. Trimer began to appear later than dimer and its increasing rate was very low. The amount of dimer and trimer formed under the CO2 atmosphere was less than that in the air.

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The Production of Microcapsules containing Fragrant material (방향물질을 함유한 마이크로캡슐 제조)

  • 김혜림;송화순
    • Journal of the Korean Society of Clothing and Textiles
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    • v.26 no.5
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    • pp.684-690
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    • 2002
  • The microcapsules containing fragrant material as functional compound were produced by in-situ polymerization. The prepolymer was made from urea-formaldehyde(UF) and melamine-formaldehyde(MF) as wall materials of microcapsules. The effects of wall material, dispersing agent and ratio of wall material to core material on the mean diameter variation were investigated. Thermal efficiency and release behavior of microcapsules were measured. The resultant UF and MF microcapsules are capable of preserving fragrant oil for long self-life.

Preparation of Slate-Plastic Composite

  • Pyun, Hyung-Chick;Cho, Bong-Rae;Kwon, Suk-Keun
    • Nuclear Engineering and Technology
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    • v.7 no.1
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    • pp.9-14
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    • 1975
  • Slate-plastic composite was prepared by impregnating methyl methacrylate monomer into the slate and subsequent curing the monomer either by gamma radiation or by thermal-catalytic method. Experiments were carried out to determine the polymerization rate and to investigate the properties of the composite. Significant improvements in flexural strength, water absorbability and acid resistance were observed in the products. Differences in properties between the composites obtained via two different methods were discussed as well as the cause of such results.

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STRAIN AND TEMPERATURE CHANGES DURING THE POLYMERIZATION OF AUTOPOLYMERIZING ACRYLIC RESINS

  • Ahn Hyung-Jun;Kim Chang-Whe;Kim Yung-Soo
    • The Journal of Korean Academy of Prosthodontics
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    • v.39 no.6
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    • pp.709-734
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    • 2001
  • The aims of this experiment were to investigate the strain and temperature changes simultaneously within autopolymerzing acrylic resin specimens. A computerized data acquisition system with an electrical resistance strain gauge and a thermocouple was used over time periods up to 180 minutes. The overall strain kinetics, the effects of stress relaxation and additional heat supply during the polymerization were evaluated. Stone mold replicas with an inner butt-joint rectangular cavity ($40.0{\times}25.0mm$, 5.0mm in depth) were duplicated from a brass master mold. A strain gauge (AE-11-S50N-120-EC, CAS Inc., Korea) and a thermocouple were installed within the cavity, which had been connected to a personal computer and a precision signal conditioning amplifier (DA1600 Dynamic Strain Amplifier, CAS Inc., Korea) so that real-time recordings of both polymerization-induced strain and temperature changes were performed. After each of fresh resin mixture was poured into the mold replica, data recording was done up to 180 minutes with three-second interval. Each of two poly(methyl methacrylate) products (Duralay, Vertex) and a vinyl ethyl methacrylate product (Snap) was examined repeatedly ten times. Additionally, removal procedures were done after 15, 30 and 60 minutes from the start of mixing to evaluate the effect of stress relaxation after deflasking. Six specimens for each of nine conditions were examined. After removal from the mold, the specimen continued bench-curing up to 180 minutes. Using a waterbath (Hanau Junior Curing Unit, Model No.76-0, Teledyne Hanau, New York, U.S.A.) with its temperature control maintained at $50^{\circ}C$, heat-soaking procedures with two different durations (15 and 45 minutes) were done to evaluate the effect of additional heat supply on the strain and temperature changes within the specimen during the polymerization. Five specimens for each of six conditions were examined. Within the parameters of this study the following results were drawn: 1. The mean shrinkage strains reached $-3095{\mu}{\epsilon},\;-1796{\mu}{\epsilon}$ and $-2959{\mu}{\epsilon}$ for Duralay, Snap and Vertex, respectively. The mean maximum temperature rise reached $56.7^{\circ}C,\;41.3^{\circ}C$ and $56.1^{\circ}C$ for Duralay, Snap, and Vertex, respectively. A vinyl ethyl methacrylate product (Snap) showed significantly less polymerization shrinkage strain (p<0.01) and significantly lower maximum temperature rise (p<0.01) than the other two poly(methyl methacrylate) products (Duralay, Vertex). 2. Mean maximum shrinkage rate for each resin was calculated to $-31.8{\mu}{\epsilon}/sec,\;-15.9{\mu}{\epsilon}/sec$ and $-31.8{\mu}{\epsilon}/sec$ for Duralay, Snap and Vertex, respectively. Snap showed significantly lower maximum shrinkage rate than Duralay and Vertex (p<0.01). 3. From the second experiment, some expansion was observed immediately after removal of specimen from the mold, and the amount of expansion increased as the removal time was delayed. For each removal time, Snap showed significantly less strain changes than the other two poly(methyl methacrylate) products (p<0.05). 4. During the external heat supply for the resins, higher maximum temperature rises were found. Meanwhile, the maximum shrinkage rates were not different from those of room temperature polymerizations. 5. From the third experiment, the external heat supply for the resins during polymerization could temporarily decrease or even reverse shrinkage strains of each material. But, shrinkage re-occurred in the linear nature after completion of heat supply. 6. Linear thermal expansion coefficients obtained from the end of heat supply continuing for an additional 5 minutes, showed that Snap exhibited significantly lower values than the other two poly(methyl methacrylate) products (p<0.01). Moreover, little difference was found between the mean linear thermal expansion coefficients obtained from two different heating durations (p>0.05).

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A Study on Synthesis of Functional Composite Latex and Characteristics of Thermal Decomposition (기능성 복합 라텍스의 합성과 열분해 특성에 관한 연구)

  • Kwon, Jae-Beom;Kim, Nam-Suk;Lee, Nae-Woo;Seul, Soo-Duck
    • Journal of the Korean Society of Safety
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    • v.19 no.2
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    • pp.47-53
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    • 2004
  • Emulsion polymerization ws carried out using Alkyl methacrylate(RMA) like MMA, EMA, BMA and Styrene Monomer(SM) for core-shell latex preparation. It was synthesized at $80^{\circ}C$ in the presence of anionic surfactant SLS(Sodium Lauryl Sulfate). FT-IR and DSC analysis are used to confirm the synthesized core-shell emulsion latexes. Moreover DSC and TGA were used to investigate the thermal characterisitcs of them. The differences of the decomposition rate and the activation energy from TGA and DSC analysis are not so big. It considers that the pendent group is not affect of the thermal characteristics and stability on core-shell latexes, which is synthesized with RMA and Styrene. For investigating combustion products, LC50 values were calculated by FED(Fractional Effective Dose)from the Pyrolyzer-Mass sepctrometer.

Syntheses of New Film-Forming Aromatic Poly(amide-imide)s Containing Isoindoloquinazolinedione Unit in the Backbone: Poly(biphenylphthalicdianhydride-oxydianiline-4,4-diamino-3-carbamoyl-benzanilide) (Poly(BPDA-ODA-DACB))

  • Kang, Seog-Joo;Hong, Sung-Il;Park, Chong-Rae;Oh, Tae-Jin
    • Fibers and Polymers
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    • v.2 no.2
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    • pp.92-97
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    • 2001
  • New film forming aromatic poly(amide-imide)s containing isoindoloquinazolinedione (IQ) unit in the backbone chain (polymer XIV) have been successfully synthesized by preparing prepolymers of poly(amic acid-carbonamide). followed by subsequent thermal cyclization of the prepolymers. 4,4-Diamino-3-carbamoylbenzanilide (DACB) V has been synthesized by reduction of 3-carbamoyl-4-amino-4-nitrobenzanilide IV. The prepolymers of poly(amic-acid-carbonamide) (polymers VII and VIII) which exhibit viscosities ranging from 1.4 to 1.7 dl/g have been prepared by a condensation polymerization of monomers such as BPDA, ODA, and DACB. Polymer XIV has been obtained by thermal cyclization of the polymers VII and VIII. During the thermal cyclization reaction, imide ring structure was first introduced and then transformed to the structure of IQ unit. The thermal degradation rate of the resultant polymers were influenced by the cleavage of amide bond but the final char yield was comparable to that of poly(BPDA-ODA).

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Synthesis and Characterization of Colorless Polyimide Nanocomposite Films Containing Pendant Trifluoromethyl Groups

  • Jin, Hyo-Seong;Chang, Jin-Hae;Kim, Jeong-Cheol
    • Macromolecular Research
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    • v.16 no.6
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    • pp.503-509
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    • 2008
  • A series of colorless polyimide (PI) nanocomposite films were synthesized from 2,2'-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride (6FDA) and 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl (TFDB) with various organoclay contents by solution intercalation polymerization to poly(amic acid)s, followed by thermal imidization. The variation with the organoclay content of the thermomechanical properties, morphology, and optical transparency of the hybrids was examined at organoclay loadings ranging from 0 to 1.0 wt%. The hybrid films showed high optical transparency and almost no color, with cut-off wavelengths ranging from 352 and 356 nm and very low $b^*$ values of 1.19-1.77. The hybrid PI films showed good thermal properties with a glass transition temperature of $280-287^{\circ}C$. Most films did not show any significant thermal decomposition below $490^{\circ}C$. The addition of only a small amount of organoclay was sufficient to improve the tensile properties of the PI films with maximum enhancement being observed at 0.25 wt% organoclay. Moreover, these PI hybrids also had low coefficients of thermal expansion (CTE).