Direct solid state polycondensation of tetra‐ and hexa‐methylenediammonium terephthalate: Scaling up from the TGA micro‐reactor to a laboratory autoclave

Abstract

ABSTRACTThe direct solid state polycondensation (DSSP) reaction of tetramethylenediammonium and hexamethylenediammonium terephthalate (4 T and 6 T salts) in a laboratory scale autoclave reactor was investigated. The autoclave reactor is 3 orders of magnitude larger than the TGA micro‐reactor we used previously. The larger scale reactor allows more extensive analyses such as analysis of the formed condensate by titration and allows investigation of operating conditions that are important on industrial scale, such as batch (closed system) versus semibatch (open system) operation and flow of nitrogen used. Comparing the two scales has given important insight into the parameters that are important in scaling‐up direct solid‐state polycondensation. Furthermore, the effect of scaling up on the quality of the final semiaromatic polyamide products was determined, by comparing the obtained thermal properties, the solution viscosity and the end‐group concentrations obtained by 1H‐NMR spectroscopy. When operating the open reactor with a gentle nitrogen stream, the results show that products of similar properties were obtained from the micro and the laboratory scale reactors if critical parameters like temperature and pressure time profile were kept the same. The solid character of the reacting mass was retained only when maintaining the reactor at atmospheric pressure, allowing the condensation water to be removed. When keeping the autoclave reactor closed, both polyamide (PA) products (i.e., PA4T and PA6T) were agglomerated as a result of a solid melt transition during the direct solid state polycondensation. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017, 134, 45080.