Prediction of Residual Curing Capacity of Melamine-Formaldehyde Resins at an Early Stage of Synthesis by In-Line FTIR Spectroscopy
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Resin Preparation
2.3. Experimental Design
2.4. Differential Scanning Calorimetry (DSC)
2.5. Inline Infrared Spectroscopic Analysis
2.6. Multivariate Data Analysis
3. Results and Discussion
3.1. Spectral Time Course of MF Resin Synthesis and Infrared Band Assignment
3.2. Process Trajectories of MF Resin Synthesis
3.2.1. Time Course of Entire MF Resin Synthesis
3.2.2. Time Course of the Condensation Reaction in Homogenous Medium (Phase 3 of MF Resin Synthesis)
3.3. Predicting Residual Curing Capacity of MF Resin Using PLS-Regression
3.3.1. PLS-Regression in the Spectral Range from 1750 to 750 cm−1
3.3.2. PLS-Regression Using a Reduced Data Set and Concept for a Low-Cost Process Spectrometer
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Resin | Factors | Response | Use in PLS Model | |
---|---|---|---|---|
pHstart | M:F Ratio | Enthalpy H (J/g) | ||
8.5-MF2 | 8.5 | 1:2.0 | 62.56 | cal |
11.5-MF2 | 11.5 | 1:2.0 | 74.01 | cal |
8.5-MF4 | 8.5 | 1:4.0 | 37.41 | cal |
11.5-MF4 | 11.5 | 1:4.0 | 42.15 | cal |
7.9-MF3 | 7.9 | 1:3.0 | 42.65 | cal |
12.1-MF3 | 12.1 | 1:3.0 | 68.30 | cal |
10-MF1.5 | 10.0 | 1:1.5 | 82.97 | cal |
10-MF4.5 | 10.0 | 1:4.5 | 47.37 | cal |
10-MF3 a | 10.0 | 1:3.0 | 50.16 | val |
10-MF3 b | 10.0 | 1:3.0 | 49.39 | val |
10-MF3 c | 10.0 | 1:3.0 | 43.62 | val |
10-MF3 d | 10.0 | 1:3.0 | 61.08 | val |
10-MF3 avg | 10.0 | 1:3.0 | 51.06 | cal |
y Reference (Enthalpy H) | y Predicted (Spectral Information) | |
---|---|---|
Mean value | 51.06 | 48.34 |
SD | 6.31 | 0.80 |
SE | 3.16 | 0.40 |
Stage of Synthesis Used | Model Based On | Wavenumbers (cm−1) | R2cal | RMSEC |
---|---|---|---|---|
TP | Entire spectral range | 1750–750 | 0.89 | 4.98 |
TP | 6 single wavenumbers | 1620, 1540, 1390, 1160, 1050, 985 | 0.92 | 4.20 |
TP | 3 single wavenumbers | 1620, 1540, 985 | 0.82 | 6.86 |
CP | Entire spectral range | 1750–750 | 0.85 | 5.87 |
CP | 6 single wavenumbers | 1620, 1540, 1390, 1160, 1050, 985 | 0.85 | 5.77 |
CP | 3 single wavenumbers | 1620, 1540, 985 | 0.90 | 5.17 |
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Seidl, R.; Weiss, S.; Kessler, R.W.; Kessler, W.; Zikulnig-Rusch, E.M.; Kandelbauer, A. Prediction of Residual Curing Capacity of Melamine-Formaldehyde Resins at an Early Stage of Synthesis by In-Line FTIR Spectroscopy. Polymers 2021, 13, 2541. https://doi.org/10.3390/polym13152541
Seidl R, Weiss S, Kessler RW, Kessler W, Zikulnig-Rusch EM, Kandelbauer A. Prediction of Residual Curing Capacity of Melamine-Formaldehyde Resins at an Early Stage of Synthesis by In-Line FTIR Spectroscopy. Polymers. 2021; 13(15):2541. https://doi.org/10.3390/polym13152541
Chicago/Turabian StyleSeidl, Regina, Stephanie Weiss, Rudolf W. Kessler, Waltraud Kessler, Edith M. Zikulnig-Rusch, and Andreas Kandelbauer. 2021. "Prediction of Residual Curing Capacity of Melamine-Formaldehyde Resins at an Early Stage of Synthesis by In-Line FTIR Spectroscopy" Polymers 13, no. 15: 2541. https://doi.org/10.3390/polym13152541