Abstract

The interfacial polymerization (IP) of piperazine (PIP) and trimesoyl chloride (TMC) has been extensively utilized to synthesize nanofiltration (NF) membranes. However, it is still a huge challenge to monitor the IP reaction, because of the fast reaction rate and the formed ultra-thin film. Herein, two effective strategies were applied to reduce the IP reaction rate: (1) the introduction of hydrophilic interlayers between the porous substrate and the formed polyamide layer, and (2) the addition of macromolecular additives in the aqueous solution of PIP. As a result, in situ Fourier transform infrared (FT-IR) spectroscopy was firstly used to monitor the IP reaction of PIP/TMC with hydrophilic interlayers or macromolecular additives in the aqueous solution of PIP. Moreover, the formed polyamide layer growth on the substrate was studied in a real-time manner. The in situ FT-IR experimental results confirmed that the IP reaction rates were effectively suppressed and that the formed polyamide thickness was reduced from 138 ± 24 nm to 46 ± 2 nm according to TEM observation. Furthermore, an optimized NF membrane with excellent performance was consequently obtained, which included boosted water permeation of about 141–238 (L/m2·h·MPa) and superior salt rejection of Na2SO4 > 98.4%.

Highlights

  • The interfacial polymerization (IP) method has been widely employed to fabricate polyamide-based membranes with a thin-film composite (TFC) structure, which include top polyamide layer, middle ultrafiltration support, and bottom non-woven fabric

  • In situ Fourier transform infrared (FT-IR) can be used to monitor a reaction for several hours; in this case of a fast IP reaction, the monitoring time was fixed between 0–300 s, with the minimum interval of 15 s

  • In situ FT-IR spectroscopy was for the first time employed to measure the IP reaction

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Summary

Introduction

The interfacial polymerization (IP) method has been widely employed to fabricate polyamide-based membranes with a thin-film composite (TFC) structure, which include top polyamide layer, middle ultrafiltration support, and bottom non-woven fabric. TFC membranes are extensively used in the waste-water treatment field of reverse osmosis (RO) [1,2], nanofiltration (NF) [3], forward osmosis (FO) [4,5], and gas separation (GS). As it is reported in the literature, the IP process usually takes place at the interface of two immiscible solvents, such as the water/hexane interface. The IP reaction has been successfully utilized to synthesize an ultra-thin and dense polyamide layer on the top surface on a porous substrate, which serves both as the storage location of the diamine monomer, and as the support of the formed ultra-thin polyamide film [8,9]

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