研究目的
Investigating a novel photochemical thiol–ene reaction method using alkyl halides and an Ir(ppy)3 photocatalyst for mechanistic understanding and application in polymer synthesis.
研究成果
The photoredox thiol–ene reaction using Ir(ppy)3 and alkyl halide initiators is efficient, oxygen-tolerant, and rapid, with EBIB as the optimal initiator. It enables quick step-growth polymerization and crosslinked network formation under mild visible light conditions, offering advantages over traditional methods.
研究不足
The study is limited to specific monomers and conditions; oxygen tolerance varies with initiator; reaction rates plateau at higher catalyst and initiator concentrations; scalability and industrial applicability are not addressed.
1：Experimental Design and Method Selection:
The study involves photochemical thiol–ene reactions initiated by an Ir(ppy)3 photocatalyst and alkyl halides under visible light irradiation. The mechanism is explored by varying initiator types, concentrations, catalyst concentrations, light wavelengths, and other conditions.
2：Sample Selection and Data Sources:
Small-molecule reactions use allyl alcohol and mercaptoethanol; polymerization uses 2,20-(ethylenedioxy)diethanethiol and tri(ethylene glycol) divinyl ether; network synthesis uses tri(ethylene glycol) divinyl ether and pentaerythritol tetrakis(3-mercaptopropionate). Reagents are purchased from commercial sources.
3：List of Experimental Equipment and Materials:
Equipment includes NMR spectrometers (Bruker 300 or 500 MHz), UV-Vis spectrometer (Perkin Elmer Lambda 35), fluorescence spectrometer (Perkin Elmer LS 55), FTIR spectrometer (Perkin Elmer Spectrum 100), SEC system (Agilent 1260 GPC), rheometer (TA Instruments Discovery HR-1), and custom-built LED photoreactors. Materials include various alkyl halides, Ir(ppy)3, DMF, TEMPO, and monomers.
4：Experimental Procedures and Operational Workflow:
Reactions are conducted in flasks or molds under LED light irradiation at room temperature. Samples are taken at intervals for analysis via NMR, SEC, IR, and rheology. Control experiments vary parameters like initiator type, light source, and presence of TEMPO.
5：Data Analysis Methods:
NMR spectroscopy monitors conversion by tracking alkene signal loss. SEC analyzes molecular weights using PMMA standards. Rheology measures storage and loss moduli. UV-Vis and fluorescence spectroscopy characterize light sources and catalyst properties.
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NMR Spectrometer
300 or 500 MHz
Bruker
Performing nuclear magnetic resonance spectroscopy for reaction monitoring and analysis.
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UV-Vis Spectrometer
Lambda 35
Perkin Elmer
Conducting UV-Vis spectroscopy for characterization.
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Fluorescence Spectrometer
LS 55
Perkin Elmer
Performing fluorescence spectroscopy.
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FTIR Spectrometer
Spectrum 100
Perkin Elmer
Conducting infrared spectroscopy for analysis.
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SEC System
1260 GPC
Agilent
Performing size exclusion chromatography for molecular weight analysis.
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Photodiode Meter
PM100A
Thorlabs
Measuring power intensity of light sources.
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Rheometer
Discovery HR-1
TA Instruments
Measuring rheological properties like storage and loss moduli.
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LED Strip
Blue LED
Lighting Ever
Providing blue light irradiation for photochemical reactions.
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Spectrograph
SP2300
Princeton Instruments
Characterizing emission spectra of light sources.
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CCD
SpectraPro 512 × 512 BUV electron-multiplying CCD
Princeton Instruments
Detecting light in spectrograph measurements.
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