Preparation and characterization of glutaraldehyde crosslinked chitosan nanofiltration membrane

In this article, we prepare chitosan (CS) membrane on polyacrylonitrile (PAN) ultrafiltration membrane, and utilize the protonated amine group (? NH₃⁺) on the CS to retain γ‐aminobutyric acid (GABA) in a solution with a pH condition below the amino acid isoelectric point, so as to separate the amino acid from a mixture with sodium acetate that simulates the amino acid fermentation broth. To improve the acid resistance of the composite membrane, we chelate the amine groups on the CS by copper sulfate first, then crosslink the hydroxyl groups in glutaraldehyde solution, and remove the copper ion in hydrochloric acid finally to release the amine groups. This crosslinked CS/PAN composite membrane achieves 95% GABA rejection in pH 4.69 solution under the operation pressure of 0.2 MPa, while over 90% of the sodium acetate permeates the membrane. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation of a polyimide nanofiltration membrane for lubricant solvent recovery

Polyimide (PI) membrane has been proven to be an efficient approach for solvent recovery. However, the inherent fragility of the PI membrane limits the range of separation conditions and process economics. In this study, copolyimides were synthesized from 3,3′,4,4′‐benzophenone–tetracarboxylic dianhydride (BTDA) and 4,4′‐biamino‐3,3′‐dimethyldiphenyl–methane (DMMDA) by chemical imidization in a two‐step procedure. Then, a PI nanofiltration (NF) membrane was prepared through a phase‐inversion process for solvent recovery from lube oil filtrates. The results indicated that the immersion of the PI (BTDA–DMMDA) NF membrane in a 1,6‐diaminohexane/ethanol crosslinking agent solution carried on the chemical crosslinking modification, which could effectively improve the solvent resistance of the NF membrane. Moreover, the addition of inorganic salt in the polymer solution further enhanced the solvent resistance and pressure resistance of the membrane, which was favorable for the solvent recovery. The lubricant rejection was above 93%, and the solvent flux was about 30 L m^?2 h^?1 with the NF membrane prepared in optimum conditions, and this membrane showed great potential for future development in the application of solvent recovery from lube oil filtrates. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40338.     

Preparation and characterization of chloromethylated/quaternized poly(phthalazinone ether sulfone ketone) for positively charged nanofiltration membranes

Chloromethylated poly(phthalazinone ether sulfone ketone) (CMPPESK) as a novel membrane material was successfully prepared from poly(phthalazinone ether sulfone ketone), with concentrated sulfuric acid as the solvent and catalyst, and chloromethyl octyl ether with lower toxicity as the chloromethylated regent. The effects of the reaction conditions on the preparation of CMPPESKs with different degrees of chloromethylation were examined. The quantity of chloromethyl groups per repeated unit (DCM) of CMPPESK was determined by the method of analysis of the chlorine element, and structures were characterized by ¹H‐NMR spectroscopy. The introduction of chloromethyl groups into the polymer chains led to a decrease in the decomposition temperature. With increasing DCM, the initial degradation temperature declined. CMPPESK had good solubility and was soluble in N‐methyl‐2‐pyrrolidone (NMP), N,N‐dimethylacetamide (DMAc), and chloroform. However, quaternized poly(phthalazinone ether sulfone ketone) (QAPPESK) had excellent solvent resistance, was only partly soluble in sulfuric acid (98%), and was swollen in N,N‐dimethylformamide. QAPPESK nanofiltration (NF) membranes had about 90% rejection for MgCl₂, and the performance of the NF membrane prepared with DMAc as the solvent was superior to that of the NF membrane prepared with NMP as the solvent. In addition, the rejection to the different salt solutions followed the following sequence: MgCl₂ > MgSO₄ > NaCl > Na₂SO₄. Furthermore, the thermotolerance of the QAPPESK NF membrane was examined, and the results show that when the solution temperature rose from 11 to 90°C, the water flux increased more than threefold with stable salt rejection. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Positively charged hollow‐fiber composite nanofiltration membrane prepared by quaternization crosslinking

Poly(N,N‐dimethylaminoethyl methacrylate) (PDMAEMA) can be crosslinked by interfacial polymerization to develop a positively charged dense network structure. According to this mechanism, a positively charged hollow‐fiber composite nanofiltration (NF) membrane was prepared by quaternization to achieve a crosslinked PDMAEMA gel layer on the outer surface of polysulfone hollow‐fiber ultrafiltration (UF) membranes with a PDMAEMA aqueous solution as a coating solution and p‐xylylene dichloride as an agent. The preparation conditions, including the PDMAEMA concentration, content of additive in the coating solution, catalyzer, alkali, crosslinking temperature, and hollow‐fiber substrate membrane, were studied. Fourier transform infrared spectroscopy and scanning electron microscopy were used to characterize the structure of the membranes. This membrane had a rejection to inorganic salts in aqueous solution. The rejection of MgSO₄ (2 g/L aqueous solution at 0.7 MPa and 25°C) was above 98%, and the flux was about 19.5 L m^?2 h^?1. Moreover, the composite NF membranes showed good stability in the water‐phase filtration process. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation of highly selective nanofiltration composite membranes based on a novel soluble rigidly contorted monomer

Nanofiltration composite membranes with high selectivity are one of the most critical cores in water treatment, and regulating the surface charge and pore structure of active separation layers in thin film composite membranes is one of the most effective means to improve the selectivity of composite membranes. This article synthesized a novel monomer with positive charge and a rigid twisted Tröger's base structure (named TBDA-SO₃), which was manipulated to improve the microporous structure and surface charge of the composite membrane. By interfacial polymerization, TBDA-SO₃, and piperazine were co-reacted with trimesoyl chloride to successfully prepare positively charged, highly selective, and strongly microporous polyamide composite nanofiltration membranes. The best-performing composite nanofiltration membrane in this article has a permeability similar to that of the control group's poly(piperazine amide) (PPA) membrane (pure water flux, 7.8 L m⁻² h⁻¹ bar⁻¹), but has excellent divalent cation selectivity (52.57), which is 4.4 times that of the control group's PPA membrane.     

Preparation and characterization of polysulfone–cyclodextrin composite nanofiltration membrane: Solvent effect

α-Cyclodextrin membranes were prepared by the phase inversion method using four types of casting solvents such as N-methyl pyrrolidone (NMP), dimethyl sulfoxide (DMSO), dimethyl acetamide (DMAc), and dimethyl formamide (DMF) herein-after termed as α-CD-NMP, α-CD-DMSO, α-CD-DMAc, and α-CD-DMF, respectively. The membranes were characterized by IR, XRD, TGA-DTA, DSC, and SEM analysis and show that solvents like NMP, DMA, DMF give good uniform morphological membranes and are better than that of DMSO. Thermal decompositions of the pure polymer and composite membranes indicate different range of thermal degradation of the membrane. This study reveals that the casting solvents NMP, DMF, DMAC have nearly same significant effect on morphology and other properties of the membranes. This is explained in terms of demixing behavior of the polymer and the combined effect of solvent volatility and polymer–solvent interactions as estimated from Hansen solubility parameter. Solvent hydrophobicity also affects the performance of the membrane and can be determined in terms of water permeability. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Preparation and characterization of a poly(vinyl alcohol)/tetraethoxysilane ultrafiltration membrane by a sol–gel method

Using poly(vinyl alcohol) (PVA) with highly hydrophilic properties as membrane material and poly(ethylene glycol) (PEG) as an additive, we prepared PVA/tetraethoxysilane (TEOS) ultrafiltration (UF) membranes with good antifouling properties by a sol–gel method. The PVA/TEOS UF membranes were characterized by X‐ray diffraction patterns, Fourier transform infrared spectroscopy, scanning electron microscopy, and static contact angle of measurement of water. The hybridization of TEOS to PVA for preparing the PVA/TEOS UF membranes achieved the required permeation performance and good antifouling behaviors. The morphology and permeation performance of the PVA/TEOS membranes varied with the different TEOS loadings and PEG contents. The pure water fluxes (J_W) increased and the rejections (Rs) decreased with increasing TEOS loading and PEG content. The PVA/TEOS UF membrane with a PVA/TEOS/PEG/H₂O composition mass ratio of 10/3/4/83 in the dope solution had a J_W of 66.5 L m^?2 h^?1 and an R of 60.3% when we filtered it with 300 ppm of bovine serum albumin aqueous solution at an operational pressure difference of 0.1 MPa. In addition, the filtration and backwashing experiment proved that the PVA/TEOS membranes possessed good long‐term antifouling abilities. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 4066–4074, 2013     

Taurine as an additive for improving the fouling resistance of nanofiltration composite membranes

A hydrophilic compound, taurine, was investigated as an additive in the interfacial polymerization between piperazine (PIP) and trimesoyl chloride (TMC) to prepare thin‐film composite (TFC) membranes. The resulting membranes were characterized by X‐ray photoelectron spectroscopy and attenuated total reflectance–Fourier transform infrared spectroscopy. The morphology and hydrophilicity of the membranes were investigated through scanning electronic microscopy and water contact angle measurements. The separation performance of the TFC membranes was investigated through water flux and salt rejection tests. The protein‐fouling resistance of the films was evaluated by water recovery rate measurements after the treatment of bovine serum albumin. The membrane containing 0.2 wt % taurine showed the best performance of 92% MgSO₄ rejection at a flux of 31 L m^?2 h^?1 and better antifouling properties than the PIP–TMC membranes. An appropriately low concentration of taurine showed the same MgSO₄ rejection as the PIP–TMC membranes but a better fouling resistance performance. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41620.     

Preparation and characterization of a composite nanofiltration membrane interfacially polymerized from cis,cis‐1,3,5‐triaminocyclohexane and trimesoyl chloride

cis,cis‐1,3,5‐Triaminocyclohexane (TAC) was synthesized and used to prepare composite nanofiltration (NF) membranes by interfacial polymerization with trimesoyl chloride (TMC). The surface elemental composition, morphology, and hydrophilicity of the prepared NF membranes were characterized. The separation performances were examined with various salts and polyethylene glycol (PEG400, PEG600) solutions. The effects of preparation conditions were also systematically studied. The NF membrane was negatively charged and exhibited a salt rejection in the order Na₂SO₄ (98.2%) > MgSO₄ (90.8%) > MgCl₂ (84.5%) > NaCl (54.6%). The water permeability was 1.56 L m^?2 h^?1 bar^?1, and the molecular weight cutoff was 600 Da. The TAC/TMC membrane exhibited some characteristics that were different from the ones made from common diamines such as m‐phenylenediamine: (1) the surface was smoother, without a ridge‐and‐valley structure; (2) there were two kinds of crosslinking points in the polyamide chains; (3) the active layer was formed faster (only 5 seconds was required to reach a Na₂SO₄ rejection of 98%). © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43511.     

Fabrication of efficient pervaporation desalination membrane by reinforcement of poly(vinyl alcohol)–silica film on porous polysulfone hollow fiber

Pervaporation membrane technology is commercially successful in the dehydration of organic solvents, and the technology has potential for seawater desalination with high recovery because of its capability to treat highly saline water. But to make the technology advantageous over the other available membrane desalination technologies in terms of productivity flux without additional energy cost, the selective barrier layer is required to be extremely thin, defect‐free, hydrophilic, and selective to water. In this work, we prepared an efficient membrane by reinforcing a highly water‐permeable but continuous barrier layer of poly(vinyl alcohol)–silica (PVA‐SiO₂) hybrid material on porous polysulfone hollow fibers. The PVA‐SiO₂ in acidified and hydrated ethanol was aged at room temperature for a period to allow solvent evaporation to obtain the solution concentration desired for the reinforcement. The reinforced hollow fiber membrane with optimal PVA‐SiO₂ barrier layer thickness exhibited a performance with a flux of 20.6 L m^?2 h^?1 and 99.9% salt rejection from a saline feed of 2000 ppm NaCl at 333 K. The effects of PVA‐SiO₂, temperature, and feed salinity on the pervaporation performance of the membrane were also studied. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45718.     

Preparation and characterization of antifouling and antibacterial polysulfone ultrafiltration membranes incorporated with a silver–polydopamine nanohybrid

A silver–polydopamine (Ag–PDA) nanohybird was used to produce polysulfone (PSf) ultrafiltration membranes with excellent antifouling and antibacterial properties. First, the catechol functional groups of polydopamine (PDA) helped with the in situ immobilization of silver (Ag) nanoparticles (<10 nm) on the PDA sphere surface; this led to the formation of the Ag–PDA nanohybrid. Then, Ag–PDA/PSf hybrid membranes were prepared via the phase‐inversion method, and the influence of Ag–PDA loading on the hybrid membrane properties was systematically investigated. When the content of Ag–PDA was 0.5 wt %, the hybrid membrane achieved optimal separation performance, including a dramatically increased pure water flux and a well‐maintained bovine serum albumin rejection. Furthermore, the Ag–PDA/PSf hybrid membranes presented a significantly enhanced protein‐fouling resistance and a good antibacterial activity. These improvements were attributed to the unique structure and properties of the Ag–PDA nanohybrid because of the synergistic effect of the hydrophilic PDA substrate and well‐distributed Ag nanoparticles. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46430.     

聚酰胺荷电镶嵌膜的制备及表征(英文)

A novel composite charged mosaic membrane(CCMM) was prepared via interfacial polymerization(IP) of polyamine[poly(epichlorohydrin amine) ]and trimesoyl chloride(TMC) on the polyethersulfone(PES) support. Fourier transform infrared spectroscopy(FT-IR) ,environmental scanning electron microscopy(ESEM) ,atomic force microscopy(AFM) and water contact angle analysis were applied to characterize the resulted CCMM.The FT-IR spectrum indicates that TMC reacts sufficiently with polyamine.ESEM and AFM pictures show that the IP process produces a dense selective layer on the support membrane.The water contact angle of the CCMM is smaller than that of the substrate membrane because of the cross-linked hydrophilic polyamine network.Several factors affecting the IP reaction and the performance of the CCMM,such as monomer concentration,reaction time,pH value of aqueous phase solution and post-treatment,were studied.The pure water flux of the optimized CCMM is 14.73 L·m -2 ·h -1 ·MPa -1 at the operating pressure of 0.4 MPa.The values of separation factorαfor NaCl/PEG1000/water and MgCl2/PEG1000/water are 11.89 and 9.96,respectively.These results demonstrate that CCMM is promising for the separation of low-molecular-weight organics from their salt aqueous solutions.     

Preparation and characterization of positively charged composite nanofiltration membranes by coating poly(ether ether ketone) containing quaternary ammonium groups on polysulfone ultrafiltration membranes

The novel positively charged poly(ether ether ketone)s (PEEKs) with pendant quaternary ammonium groups were synthesized by copolymerization of 3, 3′‐dimethylaminemethylene‐4,4′‐biphenol (DABP), 3,3′,4,4′‐tetramethylbiphenol, and 4,4′‐bisfluorobenzophenone followed by reaction with iodomethane. The resulting copolymers were used to prepare thin film composite (TFC) nanofiltration (NF) membranes via the dip‐coating method. The effects of different parameters such as copolymer concentration and curing time on the membrane performance (flux and rejection of inorganic salts) were investigated. The optimum parameters were that 1.5 wt % quaternary ammonium PEEK containing 1.8 quaternary ammonium groups per unit with 0.5 wt % DMSO coated on the polysulfone (PSf) support membrane and cured at 100°C. The results of the performance testing showed that the trend for rejection was R > R > R_NaCl > R (R = rejection), which was a typical positively charged membrane. The best performance of these composite nanofiltration membranes was 91.3% rejection for 500 ppm MgCl₂ and 62.5 L/m² h water permeability at 0.4 MPa. The MWCO of the membrane was 800 Da. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Positively charged composite nanofiltration membrane prepared by poly(N,N‐dimethylaminoethyl methacrylate)/polysulfone

Poly(N,N‐dimethylaminoethyl methacrylate) (PDMAEMA) can be crosslinked by quaternization to develop a positively charged dense network structure. According to this mechanism, PDMAEMA/polysulfone (PSF) positively charged nanofiltration membrane was developed by interfacial crosslinking polymerization using PSF plate microfiltration membrane as support layer, PDMAEMA aqueous solution as coating solution, and p‐xylylene dichloride/n‐heptane as crosslinking agent. Technique and condition of developing membrane such as concentration of coating solution, coating time, pH value of coating solution, content of low molecular weight additive in coating solution, concentration of crosslinking agent, crosslinking time, and number of coatings were studied. FTIR, SEM, and X‐ray photoelectron spectroscopy were used to characterize the structure of membranes. This membrane had rejection to inorganic salts in water solution, the rejection rate to MgSO₄ (1 g/L water solution at 0.8 MPa and 30°C) was about 90%, and permeation flux was about 10–20 L m^?2 h^?1. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 2721–2728, 2004     

Novel,positively charged membrane from a blending,crosslinking, and coagulation procedure

A novel, positively charged membrane was prepared through a blending, crosslinking, and coagulation procedure in which poly(N,N‐dimethylaminoethyl methacrylate) (PDM) and polyacrylonitrile (PAN) were used as the functional and substrate component, respectively. Because 1,4‐dibromobutane (DBT) was used as the crosslinker and quaternizing agent, PDM was crosslinked and quaternized simultaneously. The effects of PDM content, polymer concentration, and additive dosage of the casting solution on the membrane performances are discussed in detail, and differences between the PAN membrane, PDM/PAN blend membrane, and crosslinked PDM/PAN blend membrane are also discussed. We also studied the adsorption behaviors of the membranes to a positively charged dye and a negatively charged dye. Environmental scanning electron microscopy observation showed that the resulting positively charged membrane from such a blending, crosslinking, and coagulation procedure possessed a unique and uniform structure. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 1847–1854, 2005     

Preparation of PEI nanofiber membrane based on in situ and solution crosslinking technology and their adsorption properties

Two kinds of PEI (Polyethyleneimine) nanofibers membrane were successfully prepared by electrospinning and crosslinking technology, which were insoluble in water. One Polyethyleneimine/ Epichlorohydrin/ Polyacrylonitrile nanofibrous films (abbreviated as PEI/ EPI/ PAN NFs) was prepared by in situ crosslinking of PEI/PAN nanofiber containing of EPI, and the other PEI/ PAN/ EPI NFs was prepared by crosslinking PEI/ PAN nanofibers using EPI solution. The composition and morphology of nanofibers before and after crosslinking were investigated by infrared spectroscopy and scanning electron microscopy. PEI/EPI/PAN nanofibers exhibited excellent adsorption properties toward heavy metal ions and methyl orange dyes, which can also be reused multiple times. The adsorption rate of methyl orange remained around 75% after 4 cycles, meanwhile, the adsorption rate of copper and lead still remained around 90% after 5 cycles. In addition, we found that PEI/ PAN/ EPI nanofibers prepared by solution crosslinking technology solved the problem of easy gel formation in in situ crosslinking technology and facilitated the continuous production of PEI/ EPI/ PAN nanofibers, which is better than in situ crosslinking technology. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48279.     

Evaluation of the antifouling and photocatalytic properties of novel poly(vinylidene fluoride) membranes with a reduced graphene oxide–Bi2WO6 active layer

Immobilization of reduced graphene oxide (RGO)–Bi₂WO₆ is an ideal method for obtaining antifouling membranes for membrane distillation (MD) processes. Poly(vinylidene fluoride) membranes modified with RGO–Bi₂WO₆ were successfully obtained with a double‐layer coating method through non‐solvent‐induced phase separation. The water contact angle was improved by about 30° by RGO–Bi₂WO₆; this indicated that the surface modification obviously increased the membrane hydrophobicity. The high desalination rate proved that all of the prepared membranes were appropriate for the MD process. The RGO–Bi₂WO₆‐modified membranes achieve 26.26%–59.95% removal rates in 10 mg/L aqueous ciprofloxacin under visible light for 7.5 h. It was possible to erase strongly bound foulants and recover the prepared membrane's permeation flux by 3 h of visible‐light irradiation. The RGO–Bi₂WO₆‐modified membrane with a high hydrophobicity, fouling mitigation, and photocatalytic capability presents huge potential for the treatment of high‐salt antibiotic wastewater use in the MD process. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45426.     

Cellulose acetate and sulfonated polysulfone blend ultrafiltration membranes. I. Preparation and characterization

Modification of polymeric membrane materials by incorporation of hydrophilicity results in membranes with low fouling behavior and high flux. Hence, Polysulfone was functionalized by sulfonation and ultrafiltration membranes were prepared based on sulfonated polysulfone and cellulose acetate in various blend compositions. Polyethyleneglycol 600 was employed as a nonsolvent additive in various concentrations to the casting solution to improve the ultrafiltration performance of the resulting membranes. The total polymer concentration, cellulose acetate, and sulfonated polysulfone polymer blend composition, additive concentration, and its compatibility with polymer blends were optimized. The membranes prepared were characterized in terms of compaction, pure water flux, membrane resistance, and water content. The compaction takes place within 3–4 h for all the membranes. The pure water flux is determined largely by the composition of sulfonated polysulfone and concentration of additive. Membrane resistance is inversely proportional to pure water flux, and water content is proportional to pure water flux for all the membranes. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 1749–1761, 2002     

A thin film composite membrane supported by a hydrophilic poly(vinyl alcohol‐co‐ethylene) nanofiber membrane: Preparation,characterization, and application in nanofiltration

In this study, a fabricated hydrophilic poly(vinyl alcohol‐co‐ethylene) (PVA‐co‐PE) nanofiber membrane was used as the middle support layer to prepare thin film composite (TFC) membranes for nanofiltration. The effects of the supporting nonwoven layer, grams per square meter (GSM) of nanofiber, reaction time, heat treatment, monomer concentration, operating pressure, and pH value on the separation performance of the TFC membranes were analyzed. These results show that the TFC membranes prepared with the PVA‐co‐PE nanofiber membrane can be used to filtrate different metal ions. For NaCl, Na₂SO₄, CaCl₂, CuCl₂, CuSO₄, and methyl orange solutions, the rejection rates of the TFC membrane with nonwoven polyester as the supporting layer and a nanofiber GSM of 12.8 g/m² are 87.9%, 93.4%, 92.0%, 93.1%, 95.8%, and 100%, respectively. This indicates the potential application of the PVA‐co‐PE nanofiber membrane in the preparation of nanofiltration and reverse‐osmosis TFC membranes. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46261.