Recently, polybenzimidazole (PBI) membranes crosslinked with dibromoxylene (DBX) were shown to retain their molecular separation performance in the harsh conditions characteristic of organic solvent nanofiltration (OSN). This work is focused on better understanding of the crosslinking reaction between PBI and DBX, and finding the parameters important for achieving higher degrees of crosslinking. A statistical approach based on Design of Experiments was used to identify the most significant parameters and interactions affecting the crosslinking reaction. High gain in weight and high bromine content after the reaction are expected to be indirectly related to membranes with high crosslinking degrees. Hence, these two responses were measured as a function of reaction temperature, reaction time, excess of DBX, concentration of DBX and reaction solvent (acetonitrile and toluene). All parameters were found to have a positive effect on both responses, and the reaction was found to be faster in acetonitrile than in toluene. All obtained results were statistically evaluated using Analysis of Variance, and a physical interpretation of the statistical models was attempted.
Keywords

Polybenzimidazole (PBI); Crosslinking reaction; Alkylation; Design of Experiments (DoE); Organic solvent nanofiltration (OSN)