研究目的
To calculate the degree of conversion in the photopolymerization using new quinoline derivatives and verify the thermal and ?uorescence properties of ?nal polymers.
研究成果
Quinoline dyes are efficient photoinitiators for UDMA polymerization, achieving high conversions (up to 74.24%) at low concentrations (0.1%). Thermal properties were similar across polymers, with no significant differences in stability or degradation steps. Polymers exhibited solid rigid morphology and fluorescent properties under UV light, with bathochromic shifts in solid state. These findings suggest potential applications in luminescent polymers, light filters, and PLEDs.
研究不足
The study focused on specific quinoline dyes and UDMA monomer; other monomers or dyes were not tested. The photopolymerization was conducted under fixed conditions (e.g., 470 s exposure), which may not optimize all parameters. Potential side reactions or terminations in systems with excess radicals (e.g., Q-4) could affect efficiency.
1：Experimental Design and Method Selection:
The study involved synthesizing quinoline dyes and using them as photoinitiators in the photopolymerization of urethane dimethacrylate (UDMA) monomer. The polymerization was initiated by blue light LED. Thermal, morphological, and spectroscopic analyses were conducted to characterize the polymers.
2：Sample Selection and Data Sources:
Four quinoline dyes (Q-1, Q-2, Q-3, Q-4) were synthesized and used in monomeric mixtures with UDMA. Polymers (PQ-1, PQ-2, PQ-3, PQ-4) were prepared and analyzed.
3：List of Experimental Equipment and Materials:
Equipment included STA 499 F3 (Netzsch) for TG-DTA, Mettler-Toledo DSC1 STARe for DSC, Vertex 70 (Bruker) for MIR, EVO LS15 (Zeiss) for SEM, Perkin Elmer Lambda 1050 for UV–vis, D-2000 (DMC Ltd.) blue light LED for photopolymerization, and Bruker DRX 400 for NMR. Materials included UDMA (Aldrich), quinoline dyes, ethyl-p-dimethylaminobenzoate, acetone, acetonitrile, NbCl5, Pd/C, hydrazine, ethanol.
4：Experimental Procedures and Operational Workflow:
Quinoline dyes were synthesized and mixed with UDMA and coinitiator. Mixtures were photopolymerized using blue light LED for 470 s. Polymers were washed with acetone and characterized using TG-DTA, DSC, MIR, SEM, and UV–vis analyses.
5：Data Analysis Methods:
Degree of conversion was calculated using MIR spectroscopy and eq. (1). Thermal properties were analyzed from TG-DTA and DSC curves. Morphology was examined via SEM images. Optical properties were determined from UV–vis spectra.
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Vertex 70
Vertex 70
Bruker
Used for mid-infrared spectroscopy (MIR) with a diamond crystal ATR system to calculate the degree of conversion and rate of polymerization.
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EVO LS15
EVO LS15
Zeiss
Used for scanning electron microscopy (SEM) to analyze morphological characteristics of polymers.
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Lambda 1050
Lambda 1050
Perkin Elmer
Used for solid ultraviolet–visible (UV–vis) analysis to obtain absorption and transmittance spectra, and determine optical band gap.
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DRX 400
DRX 400
Bruker
Used for NMR analysis to determine the structure and purity of quinoline dyes.
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STA 499 F3
STA 499 F3
Netzsch
Used for thermogravimetry-differential thermal analysis (TG-DTA) to obtain thermal properties such as thermal stability, mass loss steps, and thermal events.
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DSC1 STARe
DSC1 STARe
Mettler-Toledo
Used for differential scanning calorimetry (DSC) to study thermal events like glass transition and solvent evaporation.
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D-2000
D-2000
DMC Ltd.
Used as a blue light LED equipment for photopolymerization of monomer mixtures.
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UDMA
Aldrich
Used as the dimethacrylate monomer in photopolymerization to form luminescent polymers.
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ethyl-p-dimethylaminobenzoate
Used as a coinitiator in the photopolymerization system to assist in radical formation.
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acetone
Used as a solvent to assist with homogenization of monomer mixtures and to wash polymers to remove unreacted monomers and photoinitiators.
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acetonitrile
Used as a solvent in the synthesis of quinoline dyes.
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NbCl5
Used as a catalyst in the synthesis of quinoline dyes.
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Pd/C
Used as a catalyst in the reduction of nitroquinoline compounds to aminoquinolines.
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hydrazine
Used as a reducing agent in the synthesis of quinoline dyes.
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ethanol
Used as a solvent in the reduction step of quinoline dye synthesis.
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blue light LED
DMC Ltd.
Used to initiate photopolymerization by providing light in the 430–490 nm range.
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Teflon mold
Used to support the photopolymerization process by holding the monomer mixtures.
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α-alumina open crucible
Used in TG-DTA analysis to hold polymer samples.
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closed aluminum crucible with perforated lid
Used in DSC analysis to hold polymer samples.
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diamond crystal ATR system
Bruker
Used with the Vertex 70 spectrophotometer for MIR spectroscopy to measure degree of conversion.
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