Premium
In‐Line Monitoring and Control of Conversion and Weight‐Average Molecular Weight of Polyurethanes in Solution Step‐Growth Polymerization Based on Near Infrared Spectroscopy and Torquemetry
Author(s) -
Nogueira Evandro S.,
Borges Cristiano P.,
Pinto José C.
Publication year - 2005
Publication title -
macromolecular materials and engineering
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.913
H-Index - 96
eISSN - 1439-2054
pISSN - 1438-7492
DOI - 10.1002/mame.200400308
Subject(s) - materials science , monomer , polymerization , infrared spectroscopy , spectroscopy , analytical chemistry (journal) , polymer , physics , composite material , chemistry , organic chemistry , quantum mechanics
Summary: It is well known that the weight‐average molecular weight ( $\overline M _{\rm w}$ ) is strictly dependent on conversion in step‐growth polymerizations performed in batch and that the $\overline M _{\rm w}$ is very sensitive to impurities and molar imbalance. This makes the work of controlling $\overline M _{\rm w}$ a non trivial job. In this paper a new methodology is introduced for in‐line monitoring and control of conversion and $\overline M _{\rm w}$ of polyurethanes produced in solution step‐growth polymerizations, based on near‐infrared spectroscopy (NIRS) and torquemetry. A calibration model based on the PLS method is obtained and validated for monomer conversion, while the weight‐average molecular weight is monitored indirectly with the relative shear signal provided by the agitator. Control procedures are then proposed and implemented experimentally to avoid gelation and allow for maximization of $\overline M _{\rm w}$ . The proposed monitoring and control procedures can also be applied to other step growth polymerizations.Proposed control scheme.