Fabrication of 2D Vanadium MXene Polyphenylsulfone Ultrafiltration Membrane for Enhancing the Water Flux and for Effective Separation of Humic Acid and Dyes from Wastewater.

MXene, a new 2D transition metal carbide-based material, is gaining outstanding attention in recent days in the area of separation and purification. In this study, we have successfully synthesized vanadium-based MXene-V2CT x (where T represents functional groups such as -OH, O, and F) by etching an aluminum layer from V2AlC. For the first time, a vanadium-based MXene-V2CT x -embedded mixed matrix membrane was fabricated and utilized for removal of hazardous dye and humic acid from wastewater. With an increase in V2CT x loading, the hydrophilicity of the polyphenylsulfone (PPSU) membrane reasonably improved, and its water contact angle was reduced from 82.8 to 70.9°. V2CT x nanosheet-embedded PPSU membrane exhibited an excellent pure water permeability of 247 L m-2 h-1, which was 266% elevated than the pristine PPSU membrane. The V2CT x -PPSU membrane revealed a good antifouling nature, thermal stability, and 98.5% removal of humic acid. The optimal membrane exhibited 96.6 and 82.02% expulsion of Reactive Black 5 (RB 5) dye and Reactive Orange 16 (RO 16) dye, respectively. The flux for RO 16 and RB 5 dyes and humic acid were remarkable with a value of 202.02, 161.61, and 141.41 L m-2 h-1, respectively. This work provides a new V2CT x -incorporated PPSU ultrafiltration membrane to effectively treat humic acid and dye wastewater.

Evaluation of the surface characteristics and antibacterial properties of Titanium dioxide nanotube and methacryloyloxyethylphosphorylcholine (MPC) coated orthodontic brackets-a comparative invitro study.

OBJECTIVES: White spot lesions are the most common iatrogenic effect observed during orthodontic treatment. This study aimed to compare the surface characteristics and antibacterial action of uncoated and coated orthodontic brackets. MATERIALS AND METHODS: Sixty commercially available stainless steel brackets were coated with TiO2 nanotubes and methacryloyloxyethylphosphorylcholine. The sample was divided into Group 1: uncoated orthodontic brackets, Group 2: Stainless steel brackets with TiO2 nanotubes coating, Group 3: Stainless steel brackets with methacryloyloxyethylphosphorylcholine coating, and Group 4: Stainless steel brackets with TiO2 nanotubes combined with methacryloyloxyethylphosphorylcholine coating. Surface characterization was assessed using atomic force microscopy and scanning electron microscopy. Streptococcus mutans was selected to test the antibacterial ability of the orthodontic brackets, total bacterial adhesion and bacterial viability were assessed. The brackets were subjected to scanning electron microscopy to detect the presence of biofilm. RESULTS: The surface roughness was the greatest in Group 1 and least in Group 2 followed by Group 4 and Group 3 coated brackets. The optical density values were highest in Group 1 and lowest in Group 4. Comparison of colony counts revealed high counts in Group 1 and low counts in Group 4. A positive correlation between surface roughness and colony counts was obtained, however, was not statistically significant. CONCLUSIONS: The coated orthodontic brackets exhibited less surface roughness than the uncoated orthodontic brackets. Group 4 coated orthodontic brackets showed the best antibacterial properties. CLINICAL RELEVANCE: Coated orthodontic brackets prevent adhesion of streptococcus mutans and reduces plaque accumulation around the brackets thereby preventing formation of white spot lesions during orthodontic treatment.

Vetting of New 2,5-Bis (2,2,2-trifluoroethoxy) Phenyl-Linked 1,3-Thiazolidine-4-one Derivatives as AURKA and VEGFR-2 Inhibitor Antiglioma Agents Assisted with In Vitro and In Silico Studies.

The bioactivity of 1,3-thiazolidin-4-one derivatives with a 2,5-bis (2,2,2-trifluoroethoxy) phenyl moiety was computationally developed and evaluated. All of the synthesized thiazolidin-4-one derivatives have their chemical structures characterized using a variety of methods, including nuclear magnetic resonance (NMR) (1H and 13C), high-resolution mass spectrometry (HRMS), and Fourier transform infrared (FTIR) radiation. A human glioblastoma cancer cell line (LN229) was used to investigate the purified derivatives' antiglioma cancer efficacy. By using the MTT, colony formation, and tunnel tests, respectively, the in vitro cytotoxic and apoptotic effects of these compounds were assessed. Thiazolidin-4-one derivatives 5b, 5c, and 5e were discovered to have the best efficacy against glioblastoma cells out of all of these compounds. The derivatives 5b, 5c, and 5e were determined to have respective IC50 values of 9.48, 12.16, and 6.43 g/mL. Computation results showed that the bioactivity evaluations of the compounds were quite significant. The bridging -NH group forms a hydrogen bond with Glu 260 of synthesized derivatives 5b, 5c, 5d, 5e, and 5h. The vast majority of freshly developed compounds obeyed Lipinski's rule of five, which is in line with the results that the ADMET model predicted. Additionally, molecular docking evaluation and molecular dynamics simulation investigations against the proteins AURKA and VEGFR-2 were conducted for the synthesized compounds to incorporate both in silico and in vitro data. The findings revealed that almost all of the compounds had considerable binding to AURKA and VEGFR-2 residues, with binding affinities ranging from -9.8 to -7.9 kcal/mol. Consequently, the results of the biological investigations and the docking scores demonstrated that thiazolidinone molecule 5e containing 4-chlorophenyl substituent may be considered as a potential moiety for glioblastoma cancer treatments.

2,5-Bis(2,2,2-trifluoroethoxy)phenyl-tethered 1,3,4-Oxadiazoles Derivatives: Synthesis, In Silico Studies, and Biological Assessment as Potential Candidates for Anti-Cancer and Anti-Diabetic Agent.

In the present work, a series of new 1-{5-[2,5-bis(2,2,2-trifluoroethoxy)phenyl]-1,3,4-oxadiazol-3-acetyl-2-aryl-2H/methyl derivatives were synthesized through a multistep reaction sequence. The compounds were synthesized by the condensation of various aldehydes and acetophenones with the laboratory-synthesized acid hydrazide, which afforded the Schiff's bases. Cyclization of the Schiff bases yielded 1,3,4-oxadiazole derivatives. By spectral analysis, the structures of the newly synthesized compounds were elucidated, and further, their anti-cancer and anti-diabetic properties were investigated. To examine the dynamic behavior of the candidates at the binding site of the protein, molecular docking experiments on the synthesized compounds were performed, followed by a molecular dynamic simulation. ADMET (chemical absorption, distribution, metabolism, excretion, and toxicity) prediction revealed that most of the synthesized compounds follow Lipinski's rule of 5. The results were further correlated with biological studies. Using a cytotoxic assay, the newly synthesized 1,3,4-Oxadiazoles were screened for their in vitro cytotoxic efficacy against the LN229 Glioblastoma cell line. From the cytotoxic assay, the compounds 5b, 5d, and 5m were taken for colony formation assay and tunnel assay have shown significant cell apoptosis by damaging the DNA of cancer cells. The in vivo studies using a genetically modified diabetic model, Drosophila melanogaster, indicated that compounds 5d and 5f have better anti-diabetic activity among the different synthesized compounds. These compounds lowered the glucose levels significantly in the tested model.

Catalyst- and Stabilizer-Free Rational Synthesis of Ionic Polymer Nanoparticles in One Step for Oil/Water Separation Membranes.

Ionic polymer nanoparticles (IPNs) were synthesized in one pot by quaternization precipitation polymerization (QPP) as a novel polymerization technique. QPP eliminated the usage of high-cost ionic monomers and reduced the number of steps for the preparation of IPN. The monomers 2-(dimethylamino)ethyl methacrylate (DMAEMA) and 4-vinylbenzyl chloride (VBC) polymerized in the presence of azobisisobutyronitrile (AIBN) and underwent quaternization simultaneously, which yielded ionic poly(DMAEMA-co-VBC) nanoparticles in one step with the size of 50-80 nm without any stabilizer and catalyst. Similarly, 4-vinylpyridine (VP) and VBC polymerized in the presence of AIBN and underwent quaternization simultaneously, which yielded ionic poly(VP-co-VBC) nanoparticles in one step with the size of 70-90 nm without any stabilizer and catalyst. The as-synthesized IPN was further utilized for the fabrication of hydrophilic nanocomposite ultrafiltration membranes for oil/water separation. Fabricated hybrid membranes were characterized and studied for oil rejection properties. It exhibited an oil rejection of >96% with a pure water permeability of 219 L/m2 h bar.

Synthesis and Characterization of Titanium Dioxide Hollow Nanofiber for Photocatalytic Degradation of Methylene Blue Dye.

Environmental crisis and water contamination have led to worldwide exploration for advanced technologies for wastewater treatment, and one of them is photocatalytic degradation. A one-dimensional hollow nanofiber with enhanced photocatalytic properties is considered a promising material to be applied in the field. Therefore, we synthesized titanium dioxide hollow nanofibers (THNF) with extended surface area, light-harvesting properties and an anatase-rutile heterojunction via a template synthesis method and followed by a calcination process. The effect of calcination temperature on the formation and properties of THNF were determined and the possible mechanism of THNF formation was proposed. THNF nanofibers produced at 600 °C consisted of a mixture of 24.2% anatase and 75.8% rutile, with a specific surface area of 81.2776 m2/g. The hollow nanofibers also outperformed the other catalysts in terms of photocatalytic degradation of MB dye, at 85.5%. The optimum catalyst loading, dye concentration, pH, and H2O2 concentration were determined at 0.75 g/L, 10 ppm, pH 11, and 10 mM, respectively. The highest degradation of methylene blue dye achieved was 95.2% after 4 h of UV irradiation.

New Preparation Methods for Pore Formation on Polysulfone Membranes.

This work described the preparation of membranes based on aromatic polysulfones through the phase-inversion method induced by a nonsolvent, generating the phase separation (NIPS) process. Three new techniques, including the nano iron acid etching method, base hydrolysis method of crosslinked polymers, and base hydrolysis method of a reactive component in a binary polymer blend, were developed for pore creation on membranes. The modified polymers and obtained membranes were carefully characterized. The uniform pores were successfully created by base hydrolysis of the crosslinked polymers and obtained at the size of the crosslinker. Moreover, homogeneous pores were created after base hydrolysis of the membranes prepared from binary polymer blends due to the internal changes in the polymer structure. The separation performance of membranes was tested with different inorganic salt solutions and compared with commercially known membranes. These new membranes exhibited high water flux (up to 3000 L/m-2·h-1 at 10 bar and at 25 °C) and reasonable rejections for monovalent (21-44%) and multivalent ions (18-60%), depending on the different etching of the hydrolysis times. The comparison of these membranes with commercial ones confirmed their good separation performance and high potential application for water treatment applications.

Poly(Homopiperazine-Amide) Thin-Film Composite Membrane for Nanofiltration of Heavy Metal Ions.

The development of membrane-based technologies for the treatment of wastewater streams and resources containing heavy metal ions is in high demand. Among various technologies, nanofiltration (NF) membranes are attractive choices, and the continuous development of novel materials to improve the state-of-the-art NF membranes is highly desired. Here, we report on the synthesis of poly(homopiperazine-amide) thin-film composite (HTFC)-NF membranes, using homopiperazine (HP) as a monomer. The surface charge, hydrophilicity, morphology, cross-linking density, water permeation, solute rejection, and antifouling properties of the fabricated NF membranes were evaluated. The fabricated HTFC NF membranes demonstrated water permeability of 7.0 ± 0.3 L/(m2 h bar) and rejected Na2SO4, MgSO4, and NaCl with rejection values of 97.0 ± 0.6, 97.4 ± 0.5, and 23.3 ± 0.6%, respectively. The membranes exhibit high rejection values of 98.1 ± 0.3 and 96.3 ± 0.4% for Pb2+ and Cd2+ ions, respectively. The fouling experiment with humic acid followed by cross-flow washing of the membranes indicates that a flux recovery ratio (FRR) of 96.9 ± 0.4% can be obtained.

One-step synthesis of zwitterionic graphene oxide nanohybrid: Application to polysulfone tight ultrafiltration hollow fiber membrane.

In this paper, novel zwitterionic graphene oxide (GO) nanohybrid was synthesized using monomers [2-(Methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide (SBMA) and N,N'-methylenebis(acrylamide) (MBAAm) (GO@poly(SBMA-co-MBAAm), and incorporated into polysulfone (PSF) hollow fiber membrane for the effectual rejection of dye from the wastewater. The synthesized nanohybrid was characterized using FT-IR, PXRD, TGA, EDX, TEM and zeta potential analysis. The occurrence of nanohybrid on the membrane matrix and the elemental composition were analyzed by XPS. The as-prepared tight ultrafiltration hollow fiber membrane exhibited high rejection of reactive black 5 (RB-5, 99%) and reactive orange 16 (RO-16, 74%) at a dye concentration of 10 ppm and pure water flux (PWF) of 49.6 L/m2h. Fabricated nanocomposite membranes were also studied for their efficacy in the removal of both monovalent (NaCl) and divalent salts (Na2SO4). The results revealed that the membrane possesses complete permeation to NaCl with less rejection of Na2SO4 (<5%). In addition, the nanocomposite membrane revealed outstanding antifouling performance with the flux recovery ratio (FRR) of 73% towards bovine serum albumin (BSA). Therefore, the in-house prepared novel nanocomposite membrane is a good candidate for the effective decolorization of wastewater containing dye.

Assessment of sulfonated homo and co-polyimides incorporated polysulfone ultrafiltration blend membranes for effective removal of heavy metals and proteins.

Sulfonated homo and co- polyimide (sPI) were synthesized with new compositional ratios, and used as additives (0.5 wt%, 0.75 wt%, and 1.0 wt%) to prepare blend membranes with polysulfone (PSf). Flat sheet membranes for ultrafiltration (UF) were casted using the phase inversion technique. Surface morphology of the prepared UF membranes were characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM). Surface charge of the membranes were determined by zeta potential, and hydrophilicity was studied by contact angle measurement. The contact angle of the membrane decreased with increasing sPI additive indicates increasing the hydrophilicity of the blend membranes. Filtration studies were conducted for rejection of heavy metals (Pb2+ and Cd2+) and proteins (pepsin and BSA). Blend membranes showed better rejection than pure PSf membrane. Among the blend membranes it was observed that with increasing amount of sPIs enhance the membrane properties and finally, PSf-sPI5 membrane with 1 wt% of sPI5 showed the improved permeability (72.1 L m-2 h-1 bar-1), and the best rejection properties were found for both metal ions (≈98% of Pb2+; ≈92% of Cd2+) and proteins (>98% of BSA; > 86% of Pepsin). Over all, this membrane was having better hydrophilicity, porosity and higher number of sites to attach the metal ions. Its performance was even better than several-reported sulfonic acid based UF membranes. All these intriguing properties directed this new UF membrane for its potential application in wastewater treatment.

Nanohydroxyapatite Reinforced Chitosan Composite Hydrogel with Tunable Mechanical and Biological Properties for Cartilage Regeneration.

With the continuous quest of developing hydrogel for cartilage regeneration with superior mechanobiological properties are still becoming a challenge. Chitosan (CS) hydrogels are the promising implant materials due to an analogous character of the soft tissue; however, their low mechanical strength and durability together with its lack of integrity with surrounding tissues hinder the load-bearing application. This can be solved by developing a composite chitosan hydrogel reinforced with Hydroxyapatite Nanorods (HANr). The objective of this work is to develop and characterize (physically, chemically, mechanically and biologically) the composite hydrogels loaded with different concentration of hydroxyapatite nanorod. The concentration of hydroxyapatite in the composite hydrogel was optimized and it was found that, reinforcement modifies the hydrogel network by promoting the secondary crosslinking. The compression strength could reach 1.62 ± 0.02 MPa with a significant deformation of 32% and exhibits time-dependent, rapid self-recoverable and fatigue resistant behavior based on the cyclic loading-unloading compression test. The storage modulus value can reach nearly 10 kPa which is needed for the proposed application. Besides, composite hydrogels show an excellent antimicrobial activity against Escherichia coli, Staphylococcus aureus bacteria's and Candida albicans fungi and their cytocompatibility towards L929 mouse fibroblasts provide a potential pathway to developing a composite hydrogel for cartilage regeneration.

Use of cellulose acetate/polyphenylsulfone derivatives to fabricate ultrafiltration hollow fiber membranes for the removal of arsenic from drinking water.

Cellulose acetate (CA) and cellulose acetate phthalate (CAP) were used as additives (1 wt%, 3 wt%, and 5 wt%) to prepare polyphenylsulfone (PPSU) hollow fiber membranes. Prepared hollow fiber membranes were characterized by surface morphology using scanning electron microscopy (SEM), surface roughness by atomic force microscopy (AFM), the surface charge of the membrane was analyzed by zeta potential measurement, hydrophilicity by contact angle measurement and the functional groups by fourier transform infrared spectroscopy (FTIR). Fouling resistant nature of the prepared hollow fiber membranes was evaluated by bovine serum albumin (BSA) and molecular weight cutoff was investigated using polyethylene glycol (PEG). By total organic carbon (TOC), the percentage rejection of PEG was found to be 14,489 Da. It was found that the hollow fiber membrane prepared by the addition of 5 wt% of CAP in PPSU confirmed increased arsenic removal from water as compared to hollow fiber membrane prepared by 5 wt% of CA in PPSU. The removal percentages of arsenic with CA-5 and CAP-5 hollow fiber membrane was 34% and 41% with arsenic removal permeability was 44.42 L/m2h bar and 40.11 L/m2h bar respectively. The increased pure water permeability for CA-5 and CAP-5 hollow fiber membrane was 61.47 L/m2h bar and 69.60 L/m2 h bar, respectively.

Removal of metal ions and humic acids through polyetherimide membrane with grafted bentonite clay.

Functional surfaces and polymers with branched structures have a major impact on physicochemical properties and performance of membrane materials. With the aim of greener approach for enhancement of permeation, fouling resistance and detrimental heavy metal ion rejection capacity of polyetherimide membrane, novel grafting of poly (4-styrenesulfonate) brushes on low cost, natural bentonite was carried out via distillation-precipitation polymerisation method and employed as a performance modifier. It has been demonstrated that, modified bentonite clay exhibited significant improvement in the hydrophilicity, porosity, and water uptake capacity with 3 wt. % of additive dosage. SEM and AFM analysis showed the increase in macrovoides and surface roughness with increased additive concentration. Moreover, the inclusion of modified bentonite displayed an increase in permeation rate and high anti-irreversible fouling properties with reversible fouling ratio of 75.6%. The humic acid rejection study revealed that, PEM-3 membrane having rejection efficiency up to 87.6% and foulants can be easily removed by simple hydraulic cleaning. Further, nanocomposite membranes can be significantly employed for the removal of hazardous heavy metal ions with a rejection rate of 80% and its tentative mechanism was discussed. Conspicuously, bentonite clay-bearing poly (4-styrenesulfonate) brushes are having a synergistic effect on physicochemical properties of nanocomposite membrane to enhance the performance in real field applications.

Novel, one-step synthesis of zwitterionic polymer nanoparticles via distillation-precipitation polymerization and its application for dye removal membrane.

In this work, poly(MBAAm-co-SBMA) zwitterionic polymer nanoparticles were synthesized in one-step via distillation-precipitation polymerization (DPP) and were characterized. [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide (SBMA) as monomer and N, N'-methylene bis(acrylamide) (MBAAm) as cross-linker are used for the synthesis of nanoparticles. As  far as our knowledge, this is the first such report on the synthesis of poly(MBAAm-co-SBMA) nanoparticles via DPP. The newly synthesized nanoparticles were further employed for the surface modification of polysulfone (PSF) hollow fiber membranes for dye removal. The modified hollow fiber membrane exhibited the improved permeability (56 L/ m2 h bar) and dye removal (>98% of Reactive Black 5 and >80.7% of Reactive orange 16) with the high permeation of salts. Therefore, the as-prepared membrane can have potential application in textile and industrial wastewater treatment.

Click chemistry approach: regioselective one-pot synthesis of some new 8-trifluoromethylquinoline based 1,2,3-triazoles as potent antimicrobial agents.

Three series of 8-trifluoromethylquinoline based 1,2,3-triazoles derivatives (5a-c, 6a-d and 7a-c) were synthesized by multi-step reactions by click chemistry approach. Synthesized compounds were characterized by spectral studies and X-ray analysis. The final compounds were screened for their in-vitro antimicrobial activity by well plate method (zone of inhibition). Compounds 5c, 6b, 8b, 11 and 12 were found to be active against tested microbial strains. The results are summarized in Tables 5 and 6.

Synthesis and biological evaluation of novel substituted 1,3,4-thiadiazole and 2,6-di aryl substituted imidazo [2,1-b] [1,3,4] thiadiazole derivatives.

A new series of N-[5-(4-(alkyl/aryl)-3-nitro-phenyl)-[1,3,4-thiadiazol-2-yl]-2,2-dimethyl-propionamide 4 (a-l) and 6-(4-Methoxy-phenyl)-2-(4-alkyl/aryl)-3-nitro-phenyl)-Imidazo [2,1-b] [1,3,4] thiadiazole 6 (a-l) were synthesized starting from 5-(4-Fluoro-3-nitro-phenyl)-[1,3,4] thiadiazole-2-ylamine. The synthesized compounds were characterized by IR, NMR, mass spectral and elemental analysis. All the compounds were tested for antibacterial and antifungal activities. The antimicrobial activities of the compounds were assessed by well plate method (zone of inhibition). Compounds 4a, 4c and 6e, 6g displayed appreciable activity at the concentration 0.5-1.0 mg/mL.

Design and regioselective synthesis of trifluoromethylquinolone derivatives as potent antimicrobial agents.

Three series of new trifluoromethyl substituted quinolone derivatives were synthesized (4a-f, 6a-f and 8a-f) from corresponding substituted anilines by multi-step reactions. The regioselective alkylation with different alkyl halides were carried out by approaching two different routes to get the final products in good yield. Newly synthesized compounds were characterized by spectral study and also by C, H, N analyses. Three dimensional structure of 2b and 4b were also confirmed by single crystal X-ray studies. The final compounds (4a-f, 6a-f and 8a-f) were screened for their in-vitro antibacterial and antifungal activity by well plate method (zone of inhibition). The results revealed that, compounds 4a, 6b, 6c and 8e showed significant antibacterial activity as compared to the standard drug Ciprofloxacin. The compound 8a was found to be a potent antifungal agent.

2-(4-Bromo-phen-yl)-2-oxoethyl naphthalene-1-carboxyl-ate.

In the title compound, C19H13BrO3, an ester of 1-naphthoic acid with an aromatic alcohol, the least-squares planes defined by the C atoms of the respective aromatic systems enclose an angle of 77.20 (5)°. In the crystal, C-H⋯O contacts connect the mol-ecules into undulating sheets parallel (100).

2,4-Dichloro-benzyl 2-meth-oxy-benzoate.

In the title compound, C15H12Cl2O3, the aromatic rings make a dihedral angle of 10.78 (4)°. In the molecule, there is a short C-H⋯O contact. In the crystal, C-H⋯O contacts connect the mol-ecules into C(7)C(8) chains along the b axis. The shortest inter-centroid distance between two benzoic acid aromatic systems is 3.7416 (8) Å.

2-(4-Chloro-phen-yl)-2-oxoethyl naphthalene-1-carboxyl-ate.

In the title compound, C19H13ClO3, an ester of 1-naphthoic acid with an aromatic alcohol, the least-squares planes defined by the C atoms of the respective aromatic systems enclose an angle of 77.16 (3)°. In the crystal, C-H⋯O contacts connect the mol-ecules into undulating sheets parallel to the bc plane.