Synthesis and antimicrobial activity of the Schiff base from polyoxyalkylene‐montmorillonite nanocomposites and aldehydes

Vanillin (4‐hydroxy‐3‐methoxy benzaldehyde) and 5‐formylamino salicylic acid microbicides were reacted with polyoxyalkylene‐montmorillonite (D_230–2000‐MMT) nanocomposites. The microstructure of these Schiff base nanocomposites was characterized by TEM and XRD. D_230–2000‐MMT nanocomposites were prepared by an ion exchange process of sodium montmorillonite (Na‐MMT) and NH₃ ⁺ groups in polyoxyalkylene amine hydrochloride with three different molecular masses of D₂₃₀, D₄₀₀, and D₂₀₀₀. Wide‐angle X‐ray diffraction confirms the intercalation of the polymer between the silicate layers. Electrostatic interaction between the positively charged NH₃ ⁺ groups and the negatively charged surface of MMT was observed. The nanocomposites were tested for antimicrobial activity against the Gram‐negative bacteria (Escherichia coli NCIM 2065), Gram‐positive bacteria (Bacillus subtillus ATCC), and fungi (Candida albicans SC5314 and Cryptococcus neoformans). The D₂₀₀₀‐MMT/vanillin Schiff base nanocomposite strongly inhibited the growth of all microorganisms that can be used in different applications. The amount of loaded polymer and the structure of the nanocomposite play an important role in inhibiting the bacterial and fungal strains. It is found that the Schiff base nanocomposite affect the morphology, oxygen consumption, and the release of cytoplasmic constituents such as potassium (K⁺), sodium (Na⁺), and calcium (Ca²⁺) ions leading to death of the cells. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

Polyamide‐montmorillonite nanocomposites as a drug delivery system: Preparation,release of 1,3,4‐oxa(thia)diazoles,and antimicrobial activity

New microbicidal polyamides were prepared by the reaction of 5‐phenyl‐1,3,4,‐oxadiazole‐2‐thiol, 5‐phenyl‐1,3,4‐oxadiazole‐2‐amine, and 5‐(4‐chlorophenyl)?1,3,4‐thiadiazole‐2‐thiol with ethyl chloroformate followed by polycondensation with polyoxypropylenetriamine (Jeffamine T₄₀₃). The polyamides were modified to yield amine hydrochloride. The intercalation of polyamides into montmorillonite (MMT) was achieved through an ion exchange process between sodium cations in MMT and amine hydrochloride in the polyamides. The structure of the resulting materials was characterized with elemental analysis, proton nuclear magnetic resonance, Fourier transform infrared‐spectroscopy, X‐ray diffraction, thermogravimetric analysis, and transmission electron microscope. The release behavior of 1,3,4‐oxa(thia)diazoles was investigated in buffered aqueous solution at different pH values (2.3, 5.8, and 7.4). A slow release was recorded from the nanocomposites whereas; the release reaches almost 90% from polyamides. The in vitro antimicrobial activity of the polyamides and nanocomposites was studied against Gram‐negative bacteria, Gram‐positive bacteria, Yeast and the filamentous fungi by well diffusion method. The polymers showed good or moderate antimicrobial activities. However, nanocomposites showed no antimicrobial effect. Furthermore, in vivo study showed that nanocomposites had good antimicrobial activity. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41177.     

Synthesis and antimicrobial activity of biocidal polymer–montmorillonite nanocomposites

The bioactive agents p‐hydroxymethylbenzoate, 2,4‐dihydroxymethylbenzoate and methylsalicylate were reacted with polyoxyalkylene (D_230–2000)–montmorillonite (MMT) intercalated nanocomposites. D_230–2000–MMT were prepared by an ion exchange process of Na‐MMT and? NH₃⁺ groups in polyoxyalkylene amine hydrochloride of three different molecular masses (D₂₃₀, D₄₀₀ and D₂₀₀₀). The results of X‐ray analysis and transmission electron microscopy show that D₂₀₀₀–MMT/p‐hydroxymethylbenzoate is an exfoliated nanocomposite, whereas in D₂₃₀–MMT/p‐hydroxymethylbenzoate, D₂₃₀–MMT/2,4‐dihydroxymethylbenzoate, D₂₃₀–MMT/methylsalicylate and D₄₀₀–MMT/p‐hydroxymethylbenzoate, having lower molecular mass and polymer loading, the MMT rearranges in an intercalated and flocculated structure. The amount of intercalated polymer and interaction between polymer and layered silicate were determined using thermogravimetric analysis and Infrared spectroscopy. The antimicrobial activities of the nanocomposites were qualitatively and quantitatively assessed by agar diffusion tests and minimal inhibitory concentration values against a Gram‐negative bacterium (Escherichia coli NCIM 2065), a Gram‐positive bacterium (Bacillus subtilis ATCC) and fungi (Candida albicans SC5314 and Cryptococcus neoformans). The D₂₀₀₀–MMT/p‐hydroxymethylbenzoate nanocomposite strongly inhibits the growth of all the micro‐organisms tested. The diameter of the inhibition zone varies according to the type of micro‐organism tested. The effect of nanocomposite concentration on morphology, respiration and release of calcium, potassium and sodium ions of the test micro‐organisms was examined. Copyright © 2011 Society of Chemical Industry     

Synthesis and characterization of polyaniline–organoclay nanocomposites

Polyaniline (PANI)–organoclay nanocomposites were prepared. Intercalation of aniline monomer into montmorillonite (MMT) modified by polyoxyalkylene was followed by subsequent oxidative polymerization of the aniline in the interlayer spacing. The organoclay was prepared by cation exchange process between sodium cation in MMT and onium ion in four different types of polyoxyalkylene diamine and triamine with different molecular weight. Infrared spectra confirm the electrostatic interaction between the positively charged onium group (NH₃⁺) and the negatively charged surface of MMT. X‐ray diffraction analysis provides a structural information. The absence of d₀₀₁ diffraction band in the nanocomposites was observed at certain types and contents of organoclay. Scanning electron microscopy and transmission electron microscopy were employed to determine the dispersion of the clay into PANI. The thermal degradation behavior of PANI in the nanocomposites has been investigated by thermogravimetric analysis. The weight loss suggests that the PANI chains in the nanocomposites are more thermally stable than pristine PANI. This improvement is attributed to the presence of nanolayers with high aspect ratio acting as barriers, thus shielding the diffusion of degraded PANI from the nanocomposites. The electrical conductivity of the nanocomposites was increased 30 times more than that of pure MMT at a certain concentration. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

High performance epoxy resin nanocomposites containing both organic montmorillonite and castor oil-polyurethane

Summary Epoxy resin/polyurethane interpenetrating polymer network nanocomposites with various contents of organophilic montmorillonite (oM-EP/PU nanocomposites) were prepared by a sequential polymeric technique and an in situ intercalation method. X-ray diffraction(XRD), and transmission electronic microscopy(TEM) analysis showed that organophilic montmorillonite (oMMT) disperses uniformly in epoxy resin/polyurethane interpenetrating networks(IPNs), and the intercalated or exfoliated microstructures of oMMT are formed. Differential scanning calorimetry(DSC) test proved that oMMT promotes the compatibility of EP phase and PU phase, and glass transition temperature(T_g) of oM-EP/PU nanocomposites improves with increasing oMMT content. Mechanical properties tests and thermal gravity analysis (TGA) indicated that oMMT and the IPNs of EP and PU exhibit synergistic effect on improving mechanical and thermal properties of pure EP. The mechanism of toughing and reinforcing of oM-EP/PU nanocomposites was further discussed by scanning electronic microscope(SEM).     

Synthesis,characterization and properties of organoclay‐modified polyurethane/epoxy interpenetrating polymer network nanocomposites

organoclay‐modified polyurethane/epoxy interpenetrating network nanocomposites (oM‐PU/EP nanocomposites) were prepared by adding organophilic montmorillonite (oMMT) to interpenetrating polymer networks (IPNs) of polyurethane and epoxy resin (PU/EP) which had been prepared by a sequential polymerization technique. Wide‐angle X‐ray diffraction (WAXD) and transmission electronic microscopy (TEM) analysis showed that the interpenetrating process of PU and EP improved the exfoliation and dispersion degree of oMMT. The effects of the NCO/OH ratio (isocyanate index), the weight ratio of PU/EP and oMMT content on the phase structure and the mechanical properties of the oM‐PU/EP nanocomposites were studied by tensile testing and scanning electronic microscopy (SEM). Water absorption tests showed that the PU/EP interpenetrating networks and oMMT had synergistic effects on improvement in the water resistance of the oM‐PU/EP nanocomposites. Differential scanning calorimetry (DSC) analysis showed that PU was compatible with EP and that the glass transition temperature (T_g) of the oM‐PU/EP nanocomposites increased with the oMMT content up to 3 wt%, and then decreased with further increasing oMMT content. The thermal stability of these nanocomposites with various oMMT contents was studied by thermogravimetric analysis (TGA), and the mechanism of thermal stability improvement was discussed according to the experimental results. Copyright © 2005 Society of Chemical Industry     

Polyurethane/clay nanocomposites foams: processing, structure and properties

Polyurethane (PU)/montmorillonite (MMT) nanocomposites were synthesized with organically modified layered silicates (organoclays) by in situ polymerization and foams were prepared by a batch process. Clay dispersion of polyurethane nanocomposites was investigated by X-ray diffraction and transmission electron microscopy. The morphology and properties of PU nanocomposites and foams greatly depend on the functional groups of the organic modifiers, synthesis procedure, and molecular weight of polyols because of the chemical reactions and physical interactions involved. Silicate layers of organoclay can be exfoliated in the PU matrix by adding hydroxyl and organotin functional groups on the clay surface. The presence of clay results in an increase in cell density and a reduction of cell size compared to pure PU foam. In the polyurethane with high molecular weight polyol, a 6 °C increase in T_g, 650% increase in reduced compressive strength, and 780% increase in reduced modulus were observed with the addition of 5% organically treated clays. Opposite effects were observed in PU nanocomposite foams with highly crosslinked structure. The interference of the H-bond in the presence of clay is probably the reason.     

The effect of polyoxypropylene‐montmorillonite intercalates on polymethylmethacrylate

Polymethylmethacrylate (PMMA)‐layered silicate nanocomposites have been prepared by in situ polymerization of commercial type of methylmethacrylate monomer (MMA), for denture base material, into organoclay. Organoclay was prepared through an ion exchange process between sodium cations in montmorillonite and NH₃⁺ groups in polyethertriamine hydrochloride and polyoxypropylene triamine hydrochloride with different molecular weight (5000, 440). X‐ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) have been used to investigate the structure of the resulting composites. Both intercalated and exfoliated nanocomposites were obtained depending on the type and amount of organoclay. The thermal decomposition temperatures of the nanocomposites were found to be higher than that of pristine polymer. PMMA was strongly fixed to inorganic surfaces, due to cooperative formation of electrostatic bonding between NH₃⁺ group and negatively charged surface of layered silicate and amide linkage between PMMA and polyethertriamine or polyoxypropylene triamine. The effect of the organoclay on the hardness, toughness, tensile stress, and elongation at break of the polymer was studied and was compared with pristine polymer. The hardness and Izod impact strength of PMMA‐organoclay nanocomposites were enhanced with the inclusion of clay. Tensile properties appear to be enhanced at certain organoclay content. However, the water absorption is slightly higher than the pristine PMMA. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Novel in situ carbon nanofiber/polydimethylsiloxane nanocomposites: Synthesis,morphology, and physico‐mechanical properties

A series of carbon nanofiber (CNF)/polydimethylsiloxane (PDMS)‐based nanocomposites was prepared by anionic ring opening polymerization of octamethylcyclotetrasiloxane (D₄) in presence of pristine CNF and amine‐modified CNF. A detailed study of morphology–property relationship of the nanocomposites was carried out in order to understand the effect of chemical modification and loading of filler on property enhancement of the nanocomposites. An elaborate comparison of structure and properties was carried out for the nanocomposites prepared by in situ and conventional ex situ methods. Pronounced improvement in degree of dispersion of the fillers in the matrix on amine modification of CNFs was reflected in mechanical properties of the modified nanocomposites. Maximum upliftment in mechanical properties was observed for in situ prepared amine modified CNF/hydroxyl PDMS nanocomposites. For 8 phr filler loading, tensile strength increased by 370%, while tensile modulus showed an increase of 515% compared with the virgin elastomer. Furthermore, in situ prepared unmodified CNF/hydroxyl PDMS nanocomposites showed an increase of 141°C in temperature of maximum degradation (T_max) for 8 phr CNF loading. These results were correlated with the morphological analysis through transmission electron microscopic studies. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Effects of processing history and annealing on polymorphic structure of nylon-6/montmorillonite nanocomposites

The effects of processing history and annealing treatment on the thermal property and polymorphic structure of nylon-6/clay nanocomposites (NCNs) have been investigated. The nanocomposites, including intercalated and exfoliated ones, were prepared by extruding nylon-6 (N6) with sodium montmorillonite (Na-MMT) or organo-montmorillonite (OMMT), respectively. DSC analysis revealed multiple melting endotherms in either the extruded or the injection-molded N6 and NCNs samples. It has been observed that a small exothermic peak around 195 °C just before the lower melting peak in the skin regions. We demonstrated that this sub-T_m transition was directly related to the processing-induced shear stresses. WAXD analysis was further performed to characterize the polymorphic structure of injection-molded N6 and NCNs before and after annealing. Annealing at a temperature (80 °C) above the T_g of N6 resulted in increase of the absolute content of γ-form in the skin regions and of the relative content of γ-form in the core regions of NCNs. In particular, annealing only leaded to increase the fraction of γ-form in the exfoliated N6/OMMT nanocomposites, which might be related to a confining effect of MMT platelet on the polymer chains mobility.     

Mechanical,Morphological and Thermal Properties of Polycarbonate/SEBS-G-MA/Montmorillonite Nanocomposites

Nanocomposites based on polycarbonate (PC) containing sodium montmorillonite (NaMMT) and maleic anhydride grafted styrene-ethylene/butylene-styrene (SEBS-g-MA) were prepared by melt compounding method followed by injection molding. X-ray diffraction (XRD) and transmission electron microscopy (TEM) results revealed the formation of intercalated nanocomposites. Incorporation of SEBS-g-MA into the PC/MMT nanocomposites enhanced ductility and impact strength but slightly reduced tensile strength and stiffness. The glass transition temperature (T _g – detected from DMTA) and onset temperature (T _onset – detected from TGA) of the PC nanocomposites was increased in the presence of SEBS-g-MA. For this PC/NaMMT system, SEBS-g-MA could act as an effective toughening agent.     

Preparation of syndiotactic polystyrene/montmorillonite nanocomposites via in situ intercalative polymerization of styrene with monotitanocene catalyst

Syndiotactic polystyrene (sPS)/montmorillonite nanocomposites were prepared via in situ intercalative coordination polymerization using mono‐(η⁵‐pentamethylcyclopenta‐ dienyl) tribenzyloxy titanium [Cp*Ti(OBz)₃] complex activated by methylaluminoxanes (MAO) and triisobutylaluminum (TIBA). The influences of polymerization conditions, such as the weight ratio of montmorillonite and styrene, temperature, and monomer concentration, on the preparation of sPS/montmorillonite nanocomposites was investigated. The intercalation spacing in the nanocomposites, as well as the exfoliation of the montmorillonite interlayers, was characterized with wide angle X‐ray diffraction (WAXD) and transmission electron microscopy (TEM). The dispersibility of the nanoscale elements depended on the polymerization conditions and the surfactant treatment. The crystallizability and thermal properties of these nanocomposites were determined by differential scanning calorimetry (DSC) analysis and thermogravimetric analysis (TGA). Experimental results indicated that the degree of crystallinity of the sPS nanocomposite increased with increasing montmorillonite content and with higher T_g and thermal decomposition temperature than pure sPS. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1412–1417, 2005     

Thermoplastic elastomeric nanocomposites from poly[styrene–(ethylene‐co‐butylene)–styrene] triblock copolymer and clay: Preparation and characterization

Thermoplastic elastomer (TPE)–clay nanocomposites based on poly[styrene–(ethylene‐co‐butylene)–styrene] triblock copolymer (SEBS) were prepared. Natural sodium montmorillonite (MMT) clay was organically modified by octadecyl amine to produce an amine‐modified hydrophobic nanoclay (OC). Commercially available Cloisite 20A (CL20) and Cloisite 10A, tallow ammine modified nanoclays, were also used. The intergallery spacing of MMT increased on amine modification as suggested by the shifting of the X‐ray diffraction (XRD) peak from 7.6 to 4.5 and 3.8° in the cases of OC and CL20, respectively. The latter demonstrated no XRD peak when it was used at 2 and 4 parts phr in the SEBS system. Transmission electron microscopy studies showed the intercalation–exfoliation morphology in SEBS containing 4 parts of CL20₄–SEBS, agglomeration in SEBS having 4 parts of MMT, and mixed morphology in SEBS with 4 parts of OC systems. Locations of the clay particles were indicated by the atomic force micrographs. Mechanical and dynamic mechanical thermal analysis studies confirmed the best properties with the CL20₄–SEBS nanocomposites. Significant improvements in mechanical properties such as tensile strength, modulus, work to break, and elongation at break were achieved with the CL20₄–SEBS in polymer‐layered silicate nanocomposites. Dynamic mechanical studies further showed the affinity of the organoclays toward both segments of the TPE and a compatibilization effect with CL20 at a 4‐phr loading. Atomic force microscopy showed distinctly different morphologies in nanocomposites prepared through solution and melt processing. Comparisons of the mechanical, dynamic mechanical, and morphological properties of the nanocomposites prepared by melt and solution intercalation processes were done. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2040–2052, 2006     

Evaluation of amine functionalized polypropylenes as compatibilizers for polypropylene nanocomposites

The compatibilization effects provided by amine functionalized polypropylenes versus those of a maleated polypropylene, PP-g-MA, for forming polypropylene-based nanocomposites were compared. Amine functionalized polypropylenes were prepared by reaction of maleated polypropylene, PP-g-MA, with 1,12-diaminododecane in the melt to form PP-g-NH₂ which was subsequently protonated to form PP-g-NH₃⁺. Nanocomposites were prepared by melt processing using a DSM microcompounder (residence time of 10 min) by blending polypropylene and these functionalized materials with sodium montmorillonite, Na-MMT, and with an organoclay. X-ray and transmission electron microscopy plus tensile modulus tests were used to characterize those nanocomposites. Composites based on Na-MMT as the filler showed almost no improvement of tensile modulus compared to the polymer matrix using any of these functionalized polypropylenes, which indicated that almost no exfoliation was achieved. All the compatibilized nanocomposites using an organoclay, based on quaternary ammonium surfactant modified MMT, as the filler had better clay exfoliation compared to the uncompatibilized PP nanocomposites. Binary and ternary nanocomposites using amine functionalized polypropylenes had good clay exfoliation, but no advantage over those using PP-g-MA. The PP-g-MA/organoclay and PP/PP-g-MA/organoclay nanocomposites showed the most substantial improvements in terms of both mechanical properties and clay exfoliation.     

Polybenzoxazine/clay hybrid nanocomposites: influence of preparation method on the curing behavior and properties of polybenzoxazines

Several types of polybenzoxazine/clay hybrid nanocomposites have been prepared from organically modified montmorillonite (OMMT) and mono- or bifunctional benzoxazine, 3-phenyl-3,4-dihydro-2H-1,3-benzoxazine (Pa) or bis(3-phenyl-3,4-dihydro-2H-1,3-benzoxazinyl) isopropane (Ba), respectively. OMMT was prepared by a cation exchange of montmorillonite (MMT) with ammonium salts of amines such as tyramine, phenylethylamine, aminolauric acid, and dodecyl amine. Polybenzoxazine/clay nanocomposites were prepared by two different methods, namely melt method and solvent method. Melt method employs the blending of benzoxazine and OMMT above the melting point of benzoxazine without solvent. In the solvent method, OMMT was dispersed in an organic solvent and then blended with benzoxazine. XRD measurements of the polybenzoxazine/clay hybrid nanocomposites showed that the blending method and the kind of solvent play crucial roles in the dispersion of OMMT in the polybenzoxazine matrix. DSC showed that the inclusion of any type of OMMT significantly lowered the curing exotherm of benzoxazines. The hybrid nanocomposites exhibited higher T_g values than the pristine resins. Dynamic and isothermal TGA clearly showed that the thermal stability was improved by the inclusion of clay.     

Preparation and characteristics of nitrile rubber (NBR) nanocomposites based on organophilic layered clay

The effect of clay modification on organo‐montmorillonite/NBR nanocomposites has been studied. Organo‐montmorillonite/NBR nanocomposites were prepared through a melt intercalation process. NBR nanocomposites were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM), dynamic mechanical thermal analysis (DMTA) and a universal testing machine (UTM). XRD showed that the basal spacing in the clay increased, which means that the NBR matrix was intercalated in the clay layer galleries. On TEM images, organo‐montmorillonite (MMT) particles were clearly observed, having been exfoliated into nanoscale layers of about 10–20 nm thickness from their original 40 µm particle size. These layers were uniformly dispersed in the NBR matrix. The DMTA test showed that for these nanocomposites the plateau modulus and glass transition temperature (T_g) increased with respect to the corresponding values of pure NBR (without clay). UTM test showed that the nanocomposites had superior mechanical properties, ie strength and modulus. These improved properties are due to the nanoscale effects and strong interactions between the NBR matrix and the clay interface. Copyright © 2003 Society of Chemical Industry     

Synthesis,characterization, and mechanical performance of various functionalized carbon nanotubes-polyurethanes nanocomposites

Nanocomposites of functionalized carbon nanotubes (CNTs_f) used as a reinforcement agent, and a polyurethane (PU), as a polymeric matrix were synthesized via in situ polymerization. Carbon nanotubes (CNTs) were chemically functionalized using four different chemical treatments to obtain (1) oxidized CNTs (CNTs_{OH, COOH}), (2) CNTs containing aliphatic amine groups (CNTs_{et diam}), (3) CNTs attached to an aromatic amine group (CNTs_4AB), and (4) CNTs containing a combination of aromatic amine, hydroxyl, and carboxyl functional groups (CNTs_{4AB, OH, COOH}). The nanocomposites (prepared using 0.25, 0.5 or 1.0 wt % CNTs_f) were synthesized by two processes: (1) one-step using a PU made from PCL-diol (α-ω-telechelic polyester diol) obtained by biocatalysis from ε-caprolactone (ε-CL) and diethylene glycol (DEG) and 4,4′-methylenebis (cyclohexyl isocyanate) (H₁₂MDI) in stoichiometric amounts, (2) two-step process (chain extended PU) using hexamethylene diamine (HMDA). Depending on the chemical route used to synthesized the nanocomposites, CNTs_f form, in some cases, covalent bonds and hydrogen bonding with the soft and/or hard segments of the PU matrix. Also, the presence of CNTs_f improves the thermal stability of the nanocomposites and some of their mechanical properties, compared to the pure PU properties. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47319.     

Study of morphological and mechanical performance of amine‐cured glassy epoxy–clay nanocomposites

The effect of three different alkylammonium‐modified montmorillonite on morphological and mechanical properties of glassy epoxy‐amine nanocomposites is reported. Small amounts of clays <10 phr (part per hundred of resin) were used in each system of nanocomposite. The morphology of the prepared nanocomposites was performed by means of X‐ray diffraction and transmission electron microscopy. Differential scanning calorimetry (DSC) was used to investigate the glass transition temperatures (T_g). Mechanical properties were based on tensile characteristics (Young's modulus), impact strength, and fracture toughness. The measured moduli were compared to theoretical predictions. Scanning electron microscopy was used to study the morphological structure of the fracture surfaces of impacted specimens. It was found that at a low content of 2 phr (1.2 wt %) of nanoclays, the impact strength and the fracture toughness were improved by 77 and 90% respectively, comparatively to the neat epoxy, whereas DSC revealed a reduction of the T_g of nanocomposites. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Novel vinyl-modified sepiolite-based polymer nanocomposites: synthesis and characterization

An environmental-friendly synthesis of polymer clay nanocomposites (PCNs) was carried out by incorporation of nanoclay into polymer matrix for their potential application as sorbent of metals present in aqueous media. Polyacrylonitrile was chemically grafted onto 77% vinyl triethoxysilane-modified sepiolite. The polymerization was carried out with benzoyl peroxide (BPO, C₁₄H₁₀O₄) initiator in three different weight ratios of 1.0, 2.0, and 3.0%. The maximum polymer grafting of about 83% was obtained in nanocomposite initiated by 2.0% ratio of BPO. The surface modification of nanocomposites was carried out using hydroxyl amine hydrochloride (NH₂OH·HCl). The prepared nanocomposites were characterized by Fourier transform infrared spectroscopy, X-ray diffractometry, thermogravimetric analysis, and Brunauer–Emmett–Teller technique. The copper removal tendency of nanocomposites was studied by atomic absorption spectroscopy. The maximum adsorption of copper was 86%, which could be achieved by nanocomposites synthesized with 2% initiator. The results have revealed the practical potential of the prepared PCN as efficient adsorbents.     

Thermal stability and thermal oxidation kinetics of PU/CA-MMT composites

In this work, we prepared three composites polyurethane (PU)/chlorhexidine acetate (CA), PU/montmorillonite (MMT), and PU/CA-MMT, and investigated their kinetics of thermal degradation at different heating rates at atmosphere. These materials had good thermal stability and aging resistance. The thermal stability of PU/CA (T_onset: 237.3°C) was not obviously enhanced by the addition of only CA when compared with that of PU (T_onset: 232.3°C), while the thermal stability of PU/MMT (T_onset: 273.4°C) was considerably enhanced by the addition of MMT due to the high thermal stability of MMT. CA-MMT filler was dispersed and exfoliated in PU more easily than CA or MMT in PU, so the composite PU/CA-MMT possessed the best thermal stability (T_onset: 285.8°C). In addition, PU/CA-MMT also had the best resistance to bacterial adhesion and antibacterial ability. The analysis with Flynn-Wall-Ozawa method showed that the activation energy of thermal oxidation of PU increased when CA-MMT was added and thus its anti-aging ability was enhanced, and the thermal oxidation of these four materials was first-order reaction. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47002.