研究目的
To synthesize high-performance cyclic olefin polymers (COPs) with ester groups for improved properties such as adjustable glass transition temperature, hydrophilicity, and mechanical performance.
研究成果
The synthesis of ester-functionalized COPs via ROMP and hydrogenation successfully produced polymers with tunable Tg, hydrophilicity, and mechanical properties. These COPs exhibit high transparency, thermal stability, and film-forming ability, broadening their potential applications in optical and material sciences. Future work could explore other functional groups and catalysts for further property enhancements.
研究不足
The study is limited to specific ester-functionalized comonomers and the Grubbs first generation catalyst; other catalysts or functional groups were not explored. Hydrogenation efficiency and scalability may need optimization. Applications in real-world optical or medical devices were not tested.
1:Experimental Design and Method Selection:
The study involved ring-opening metathesis copolymerization (ROMP) of HBM with ester-functionalized comonomers (NMA, NME, NMD) using Grubbs first generation catalyst (G1), followed by hydrogenation. This method was chosen for its tolerance to functional groups and ability to produce well-defined polymers.
2:Sample Selection and Data Sources:
Monomers HBM, NMA, NME, and NMD were synthesized or obtained from suppliers. Copolymers were prepared with varying feed ratios to study composition effects.
3:List of Experimental Equipment and Materials:
Equipment included Schlenk techniques, glovebox, NMR spectrometer, FT-IR spectrometer, DSC, GPC, TGA, tensile testing machine, contact angle goniometer, UV-Vis spectrophotometer, XPS. Materials included solvents (dichloromethane, toluene, methanol), catalysts (G1), hydrogenation agents (4-methylbenzenesulfonhydrazide), and monomers.
4:Experimental Procedures and Operational Workflow:
Polymerization was conducted in dichloromethane at room temperature with G1 catalyst, followed by hydrogenation using toluenesulfonyl hydrazide. Polymers were precipitated, washed, and dried. Films were cast from tetrachloroethane solutions. Characterization involved NMR, FT-IR, DSC, GPC, TGA, tensile tests, contact angle measurements, UV-Vis, and XPS.
5:Data Analysis Methods:
Data were analyzed using NMR for composition, GPC for molecular weights, DSC for Tg, TGA for thermal stability, tensile tests for mechanical properties, and statistical methods for reactivity ratios (Fineman-Ross method).
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NMR Spectrometer
Bruker400 MHz
Bruker
Characterization of monomer and polymer samples by nuclear magnetic resonance.
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FT-IR Spectrometer
Jasco FT/IR-410
Jasco
Acquisition of infrared spectra for polymer characterization.
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TGA Analyzer
Perkin–Elmer Pyris 1
PerkinElmer
Thermogravimetric analysis for thermal stability.
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UV-Vis Spectrophotometer
Shimadzu UV-3600
Shimadzu
Recording transparency of copolymer films.
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XPS Spectrometer
Thermal ESCALAB 250
Thermo Fisher Scientific
Analysis of surface oxygen atomic state.
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DSC Calorimeter
DSC1 Stare System
Mettler Toledo
Measurement of glass transition temperatures and thermal properties.
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GPC System
Waters 1525
Waters
Determination of molecular weights and distributions.
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Universal Testing Machine
Instron 1211
Instron
Tensile testing for mechanical properties.
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Contact Angle Goniometer
DSA
KRUSS
Measurement of static water contact angles.
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Glovebox
MBraun
MBraun
Handling air- and moisture-sensitive compounds under argon atmosphere.
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Solvent Purification System
SPS
MBraun
Purification of solvents.
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