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Separations 2022, 9, 180 3 of 16 pure water and freeze-dried for 24 h. Similarly, g-C3N4 with different stripping times (24 h, 48 h, and 192 h) were also prepared. 2.2.2. Preparation of NF Membrane The schematic of the preparation of NF membranes is shown in Figure 1, and the preparation conditions are summarized in Table 1. First, PES UF membranes (M0) that were used as the base membranes for surface modification were soaked in ethanol for 2 h to remove air bubbles and impurities in and on the membranes, and then rinsed with pure water. After that, DA and g-C3N4-modified NF membranes were prepared as follows: (1) in Figure 1a, DA was immersed and then g-C3N4 was added to the PEI aqueous phase to prepare NF membrane (M4); and (2) in Figure 1b, g-C3N4 was dispersed in DA aqueous solution (2.0 g·L−1, pH = 8.5, DA hydrochloride in 50 mM·L−1 Tris buffer solution) using a probe sonicator (Biosafer 650-92, China) for 10 min to prepare DA-g- C3N4 aqueous solutions of different concentrations (0.01 wt%, 0.02 wt%, 0.03 wt%, and 0.04 wt%). PES membranes were immersed in DA-g-C3N4 aqueous solution at 25 ◦C for 2 h, and subsequently unreacted DA-g-C3N4 aqueous solution or low molecular weight PDA aggregates were removed to obtain PES membranes with PDA-g-C3N4 as the interlayer. Then, PEI aqueous solution (0.6 wt%) was poured on the interlayer for 2 min. Excess aqueous solution was removed, and then the membrane was covered with the TMC Separations 2022, 9, x FOR PEER REVIoErWganic solution (0.1 wt%) in n-hexane for 2 min to allow the IP process to occur. E4xocfes1s7 TMC was removed, and the membrane was cured at 70 ◦C for 15 min and then stored in pure water before use. (a) (b) Figure 1. The schematic of preparation of M4 (a) and M5 (b) NF membranes. Figure 1. The schematic of preparation of M4 (a) and M5 (b) NF membranes. 2.3. Characterization and Measurement Mmeimnebdrabnye Fourier transform DinefpraorseitdiosnpoefctPrDosAco(hp)y (FTIR, TChoenrmtenotFoifshg-eCr 6N70-096sp(wect%tro) me- 34 Table 1. Preparation conditions of NF membranes. The chemical functional groups of g-C3N4 and the membrane surfaces were deter- No. M0 M1 M2 M3 M4 M5 ter, Waltham, MA, USA). The morphologies of inorganic materials (g-C3N4-96) were meas- PES - - PESu/rPeEdIb/yTMtrCansmission electron microsco-py (TEM, a JEM-2100F, Tokyo, Jap- an). The element PES/PEI-g-C N -96/TMC - 0.02 com3po4sition was determined by X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, PES/DA/PEI/TMC 2 h - USA). The surface and cross-sectional morphologies of membranes were determined by PES/DA/PEI-g-C3N4-96/TMC 2 h 0.02 scanning electron microscopy (SEM, SU8010, S4800, Japan). The surface zeta potential of PES/DA-g-C3N4-96/PEI/TMC 2 h 0.02 membranes was characterized with a Sur-PASS electrokinetic analyzer (Anton Paar, Graz, Austria). Specifically, 1 mmol·L−1 KCl aqueous solution was used as the electrolyte, and 2.3. Chara−c1terization and Measu−r1ement 0.1 mol·L HCl and 0.1 mol·L KOH aqueous solution was used to control the pH value (3–10T).hTehcehgeampichaeligfuhntcotfiothneamlgeraosuprisnogfcge-llCwNasfaixnedtahte1m00eμmmbraandetshuermfaecmesbwraenresdweteerre- 34 msoiankeeddbiynFeoluecriterroltyratensfformatinlefarsatre4dhspbeecftororesctohpeym(FeTaIsRu,rTehmeernmto. TFhisehewra6t7e0r0csopnetcatcrtomanegteler, W(WalCthAa)mw,aMsAm,eUaSsuAr)e.dThoenmaocropnhtaoclotgainegsloefgionnoirogmaneitcemr (aJtCe2ri0a0ls0D(g2-,CCNhin-a9)6)atwreoroemteeamsuprerd- ature with 1.5 μL of pure water droplet. The cation concentrations were measured using an atomic absorption spectrometer (A3F-13, China). The total organic carbon (TOC) was determined by a TOC-VCPN analyzer (Japan). 2.4. Permeance and Separation Performance of NF Membranes 34PDF Image | Nanofiltration Membrane Using Polydopamine Carbon Nitride
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