Monitoramento em linha de reações de copolimerização em emulsão de acetato de vinila e acrilato de butila em um reator contínuo pulsado de pratos perfurados usando espectrocospia NIR. / In-line monitoring of vinyl acetate and butyl acrylate emulsion copolymerization in a continuous pulsed sieve plate reactor using NIR spectroscopy.

AUTOR(ES)

Dennis Chicoma Lara

DATA DE PUBLICAÇÃO

2009

RESUMO

This work deals with the study of the viability and sensitivity of the on-line monitoring, using NIR spectroscopy, of monomers and polymer concentration and average particle size during continuous vinyl acetatebutyl acrylate emulsion copolymerization carried out in a novel tubular pulsed sieve plate reactor. For the elaboration of NIR calibration models of these variables, reactions were performed in a stirred tank reactor, and the experimental data of residual monomers concentrations obtained by gravimetry and gas chromatography, and average particle size obtained by photon correlation spectroscopy were correlated with the spectra collected simultaneously in the process using an immersion probe in transflectance mode. The NIR calibration model was obtained by using the built-in computational package OPUS-QUANT in the NIR equipment (FT-NIR IFS 28N) based on PLS and PCA multivariate methods. The use of second derivative with 25- point-smoothing filter and the first derivative with 17-point smoothing filter were chosen as the best pre-treatments for the monomers concentration and the average particle size, respectively. The model validation was tested with reactions carried out in a continuous pulsed sieve plate tubular reactor, in which a NIR probe was inserted into different sections along the column. The results showed a reasonable agreement between experimental data and NIR predicted data. These results were also used to estimate other important variables in the copolymerization, such as the global and individual conversion, the copolymer composition and the number of particles. These estimated variables were also satisfactorily compared with corresponding data estimated from the experimental data. In addition, the NIR monitoring was able to detect some operational disturbances, such as the interruption of reagent feeding, thus showing its sensitivity for successfully detecting process disturbances in real time. The results indicate that NIR spectroscopy is a powerful tool for in-line, in-situ, real-time monitoring of different variables simultaneously during emulsion copolymerization process carried out in a novel continuous reactor, being a potential alternative for use in a real industrial environment.

ASSUNTO(S)

processos químicos in-line monitoring polimerização espectroscopia near infrared monitoramento emulsion polymerization infravermelho

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