Preparation and thermal properties of Alkoxy Silane functionalized polyether sulfone/well‐defined poly(trimethoxysilyl) propyl methacrylate‐based hybrid materials

In this study, novel polyethersulfone (PES) and poly(trimethoxysilyl) propyl methacrylate (PMPS) containing hybrid materials were prepared. PES was functionalized with trimethoxysilane groups by UV‐induced grafting reaction. PMPS was synthesized by atom transfer radical polymerization. In the followed process, the functionalized PES mixed with different amount of PMPS, thermally treated to promote sol–gel crosslinking process to prepare the PES‐based hybrid materials. The trimethoxysilane grafted PES chains are covalently bonded with the well‐defined trimethoxysilane groups of PMPS. The chemical structure of the prepared PES and PMPS is confirmed by Fourier transform infrared analysis. The morphology of the hybrids was investigated by scanning electron microscopy. The results of thermogravimetric analysis show that the thermal stability of the hybrid materials was significantly affected with the addition of PMPS. POLYM. ENG. SCI., 58:1346–1352, 2018. © 2017 Society of Plastics Engineers     

Photosensitized free radical polymerization using pyridinium salts

Summary The polymerization of methyl methacrylate (MMA), ethyl acrylate (EA), styrene (St) and 2-vinyl pyridine (VP) is initiated upon irradiation at >350 nm of dichloromethane solutions containing N-ethoxy-2-methylpyridinium hexafluorophosphate (EMP⁺PF₆ ^-) and anthracene or thioxanthone. Initiation mechanisms involving the formation of ethoxyl radicals during the decomposition of EMP⁺ ions via electron transfer are proposed.     

Synthesis of fluorinated/methacrylated epoxy based oligomers and investigation of its performance in the UV curable hybrid coatings

Organic–inorganic hybrid coatings based on fluorinated/methacrylated soybean oil and bisphenol A/F epoxy methacrylate were obtained by combining photopolymerization and sol–gel process. Hard and transparent hybrid coatings were prepared on polycarbonate panels and their physical and mechanical properties such as gel content, hardness, adhesion, gloss, contact angle as well as tensile strength were measured. Results from the mechanical measurements showed that the properties of hybrid coatings improved with the increase in fluorine and sol–gel precursor contents. Thermo gravimetric analysis results demonstrated that fluorine and silica incorporations significantly enhanced the thermal oxidative stability of the hybrid coating materials. The surface morphology was also characterized by scanning electron microscopy (SEM). SEM studies indicated that inorganic particles were dispersed homogenously throughout the organic matrix.     

Preparation and characterization of phosphine oxide containing organosilica hybrid coatings by photopolymerization and sol–gel process

A series of UV-cured organic–inorganic hybrid coating materials containing up to 20 wt.% silica were prepared by sol–gel method from tetraethoxy silane (TEOS) which is used as the primary inorganic precursor, and diallylphenylphosphine oxide monomer (DAPPO), aliphatic urethane diacrylate resin (Ebecryl 210) are employed as the source of the organic components. In addition, methacryloxypropyltrimethoxy silane (MAPTMS) was used as both a secondary inorganic source and a silane-coupling agent to improve the compatibility of the organic and inorganic phases. The DAPPO content in all the coating formulations were from 0 to 20 wt.%. The physical and mechanical properties such as gel content, hardness, adhesion, gloss, contact angle as well as tensile strength were measured. These measurements revealed that all the properties of the hybrid coatings improved effectively, in case of adding the sol–gel precursor and DAPPO monomer content in the hybrid systems. The photo-calorimetric-DSC studies showed that the double bond conversion of the hybrid coatings was faster than the coating materials without silica. The thermal stabilities of the UV-cured hybrid materials were investigated by thermogravimetric analysis. The results showed that the addition of sol–gel precursor and DAPPO into the organic network also improves the thermal-oxidative stability of the hybrid coating materials. The surface morphology was also characterized by scanning electron microscopy (SEM). SEM studies indicated that inorganic particles were dispersed homogenously throughout the organic matrix.     

Highly porous starch/poly(ethylene‐alt‐maleic anhydride) composite nanofiber mesh

In this study, starch‐based hybrid electrospun nanofiber meshes were fabricated by electrospinning. Spinning solutions were prepared by mixing starch and certain amounts of poly(ethylene‐alt‐maleic anhydride). Starch‐based nanofiber meshes became insoluble in water with thermal‐induced esterification of hydroxyl groups onto starch backbone. Morphologic and structure analysis of the electrospun nanofiber meshes were investigated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) techniques. Thermal properties of nanofiber meshes were characterized by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). Thermal stability of nanofiber meshes were increased with formation of intermolecular bonds between starch and poly(ethylene‐alt‐maleic anhydride). POLYM. COMPOS. 34:1321–1324, 2013. © 2013 Society of Plastics Engineers     

Synthesis and characterization of polyimide/hexagonal boron nitride composite

Polyimide (PI)/hexagonal boron nitride (h‐BN) composites were produced via the thermal imidization procedure from solution mixtures of a polyamicacid, which is prepared from 3,3′,4,4′‐benzophenonetetracarboxylic dianhydride and 3,3′‐diaminodiphenyl sulfone (DADPS) in N‐methyl‐2‐pyrrolidone (NMP), and alkoxysilane functionalized h‐BN. The structure, thermostability, thermal behavior, and surface properties of the resulting materials were characterized by means of Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM). The thermal characteristics of PI/h‐BN films were better than the pure PIs. The physical and mechanical properties of the films were evaluated by various techniques such as contact angle, chemical resistance, and tensile tests. The flame retardancy of the composite materials was also examined by the limiting oxygen index (LOI). The experiments showed that the LOI values of PIs increased from 32 to 43 for the materials containing hexagonal boron nitride. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis and drug-release properties of biodegradable hydrogels having β-cyclodextrin

A new β-cyclodextrin (β-CD) methacrylated monomer was synthesized from the reaction of β-CD, glycidyl methacrylate. Based on inclusion character of β-CD, a series of hydrogels were prepared by irradiating the mixtures of β-CD methacrylate monomer (β-CD-Met), poly(ethylene glycol) monoacrylate, poly(ethylene glycol)diacrylate, fumaric acid monoethyl ester-functionalized poly(lactic-co-glycolic) acid, 1-vinyl-2-pyrrolidone, N,N′-methylene bisacrylamide, and the photoinitiator. Gel percentages and equilibrium swelling ratios (%) of hydrogels were investigated. It was observed that equilibrium-swelling ratio increased with increasing β-CD-Met content in the hydrogel composition. SEM images demonstrated that β-CD-Met-based hydrogel have lots of voids on the fractured surface. In this study, ibuprofen (IBU) which is capable of forming inclusion complex with β-CD was chosen. For the hydrogel with maximum CD content, the IBU drug loading was found as 9 mg/g dry gel. It can be concluded that the inclusion complex-formation capability of β-CD moiety increases the drug release by improving the aqueous solubility of hydrophilic drugs.     

UV cured thiol-ene flame retardant hybrid coatings

In this study, bis-(triethoxysilylpropyl) phenyl phosphamide (BESPPA) was synthesized by the reaction between dichlorophenyl phosphine oxide and 3-aminopropyltriethoxysilane. The chemical structure of the BESPPA was characterized with Fourier transform infrared and NMR techniques. Flame retardant, BESPPA and sol–gel precursor containing hybrid materials were prepared by thiol-ene polymerization with the aim to improve their final thermal and flame retardant properties. The thermal stabilities of the phosphorous/sol–gel containing UV-cured hybrid materials were investigated by thermogravimetric analysis. The results showed that the addition of sol-gel precursor and BESPPA into the organic network also improves the thermal-oxidative stability of the hybrid materials. The flame-retardant properties of the UV-cured hybrid materials were also studied. Furthermore, the phosphorus–silicon synergistic effect on LOI enhancement and increasing flame retardancy of the UV-cured hybrid materials were demonstrated. An LOI enhancement from 20.7 to 26.5 is observed for organic resins containing both phosphorus and silicon. The surface morphology was also characterized by scanning electron microscopy (SEM). SEM studies indicated that inorganic particles were dispersed homogenously throughout the organic matrix.     

Intrinsic factor and vitamin B12 complex‐loaded poly[lactic‐co‐(glycolic acid)] microspheres: preparation,characterization and drug release

BACKGROUND: Vitamin B12 is an essential vitamin required by all mammals. Absorption of vitamin B12 is facilitated by binding of intrinsic factor–vitamin B₁₂ complex to specific receptors in the ileum. In humans a deficiency of this vitamin or a lack of intrinsic factor leads to pernicious anaemia. The major objective of the present study was to prepare intrinsic factor–vitamin B12 complex‐loaded poly[lactic‐co‐(glycolic acid)] (PLGA)‐based microparticles and to investigate their release kinetics. RESULTS: PLGA copolymer was synthesized by the ring‐opening polymerization method and characterized using gel permeation chromatography, Fourier transform infrared spectroscopy and ¹H NMR. The glass transition temperature measurement showed a single T_g at 40 °C. The intrinsic factor–vitamin B12 complex‐loaded PLGA microspheres were prepared by a water‐in‐oil‐in‐water double emulsion solvent extraction/evaporation technique. An environmental scanning electron microscopy investigation demonstrated that the PLGA particles had a mean particle diameter of 38 µm. Interestingly, different drug release patterns (bi‐ and triphasic ones) were observed for vitamin B12‐loaded and intrinsic factor–vitamin B12 complex‐loaded microspheres. In contrast to the rapid release of vitamin B12 by itself, in vitro release tests showed that intrinsic factor and vitamin B12 in the complex were released from PLGA microspheres in a sustained manner over 15 days. CONCLUSION: PLGA microspheres can be an effective carrier for the intrinsic factor–vitamin B12 complex. Copyright © 2007 Society of Chemical Industry     

Synthesis and characterization of flame retarding UV‐curable organic–inorganic hybrid coatings

UV‐curable, organic–inorganic hybrid materials were synthesized via sol–gel reactions for tetraethylorthosilicate, and methacryloxypropyl trimethoxysilane in the presence of the acrylated phenylphosphine oxide resin (APPO) and a bisphenol‐A‐based epoxy acrylate resin. The sol–gel precursor content in the hybrid coatings was varied from 0 to 30 wt %. The adhesion, flexibility, and hardness of the coatings were characterized. The influences of the amounts of inorganic component incorporated into the coatings were studied. Results from the mechanical measurements show that the properties of hybrid coatings improve with the increase in sol–gel precursor content. In addition, thermal properties of the hybrids were studied by thermogravimetric analysis in air atmosphere. The char yield of pure organic coating was 32% and that of 30 wt % silicate containing hybrid coating was 30% at 500°C in air atmosphere. This result demonstrates the pronounced effect of APPO on the flame retardance of coatings. Gas chromatography/mass spectrometry analyses showed that the initial weight loss obtained in thermogravimetric analysis is due to the degradation products of the photoinitator and the reactive diluent. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 1906–1914, 2006