研究目的
To investigate the hydrolysis kinetics of silane coupling agents using FT-NIR spectroscopy combined with a PLS model to quantitatively monitor H2O concentration changes in real-time.
研究成果
The FT-NIR PLS model effectively studied hydrolysis kinetics, confirming second-order reactions dependent on catalyst concentration and temperature. Electrophilic substitution mechanisms were identified, with kinetic parameters (Ea, A) varying by silane type. This method is reliable for optimizing surface treatment conditions.
研究不足
The method assumes hydrolysis dominates in the initial stage, ignoring condensation reactions; it may not be suitable for very rapid reactions beyond the scanning speed, and the model's accuracy depends on the quality of standard samples and spectral preprocessing.
1：Experimental Design and Method Selection:
The study used FT-NIR spectroscopy with a PLS model for real-time monitoring of hydrolysis reactions. The PLS model was chosen for its data processing capabilities to relate spectral data to H2O concentration.
2：Sample Selection and Data Sources:
Sixty-five standard samples were prepared by mixing H2O, EtOH, and methyltriethoxysilane with varying concentrations. Hydrolysis reactions were conducted for four silane coupling agents (PTES, VTES, 3-MTES, 3-CTES) under different catalyst concentrations ([H+]) and temperatures.
3：List of Experimental Equipment and Materials:
FT-NIR spectrometer (NICOLET iS10, Thermo SCIENTIFIC), cuvette with 2 mm optical path, quantitative analysis software TQ Analyst, chemicals including PTES, VTES, 3-CTES from Shandong Qufu Chemical Co., Ltd., 3-MTES from Shanghai Macklin Biochemical Co., Ltd., EtOH from Sinopharm Chemical Reagent Co., Ltd., hydrochloric acid from Laiyang Fine Chemical Factory.
4：Experimental Procedures and Operational Workflow:
Standard samples were prepared and their FT-NIR spectra collected. The PLS model was established and optimized using TQ Analyst. Hydrolysis reactions were carried out in a cuvette, with FT-NIR spectra collected at intervals. Reactions were monitored online at 15°C or in an ice-water bath for other temperatures.
5：Data Analysis Methods:
PLS regression was used to correlate FT-NIR spectra with H2O concentration. Kinetic parameters (rate constants, activation energy) were derived using second-order reaction kinetics and Arrhenius equation.
独家科研数据包，助您复现前沿成果，加速创新突破
获取完整内容
