Preparation of a novel composite material by emulsion polymerization of vinyl acetate and vinyl polyhedral oligomeric silsesquioxane

A novel material containing polyhedral oligomeric silsesquioxane (POSS) was prepared by semi-continuous emulsion polymerization. Incompletely condensed, phenyl POSS (Na₃O₁₂Si₇(C₆H₅)₇) with the highly reactive group of trisodium silanolate was used to prepare 1, 3, 5, 7, 9, 11, 13-heptaphenyl-15-vinyl silsesquioxane (vinyl-POSS) by “corner-capping” method. Then this cubic structure molecule was chemically bonded with PVAc chain to synthesize POSS/PVAc composite. The structures of POSS and composite were characterized by FTIR, ¹H-NMR and XRD. The results confirmed that vinyl-POSS could be successfully incorporated into the PVAc matrix via emulsion polymerization. Transmission electron microscope (TEM) was used to observe the morphology of copolymers. The thermal properties were investigated by differential scanning calorimetry and thermal gravimetric analysis. Data indicated that the POSS/PVAc composite displayed higher thermal stability than that of the parent PVAc homopolymer.     

Phase behavior and properties of poly(methyl methacrylate)/poly(vinyl acetate) blends prepared via in situ polymerization

Polymer blends composed of poly(methyl methacrylate) (PMMA) and poly(vinyl acetate) (PVAc) were prepared via radical-initiated polymerization of methyl methacrylate (MMA) in the presence of PVAc. Differential scanning calorimetry and dynamic mechanical analysis were employed to investigate the miscibility and phase behavior of the blends. The PMMA/PVAc blends of in situ polymerization were found to be phase separated and exhibited a two-phase structure, although some chain transferring reaction between the components occurred. The phase separation resulted from the solvent effect of MMA during the in situ polymerization, which was confirmed by the investigation of phase behavior based on solution cast blending. Solubility analysis of the polymerized blends indicated that some chain transferring reaction between the components occurred during the polymerization. An abrupt increase in gel content from 21.2 to 72.4 wt % was observed when the inclusion of PVAc increased from 30 to 40 wt %, and the gel component consisted of the component polymers as shown by infrared spectroscopy studies. The thermogravimetric analysis study indicated that the inclusion of a small amount of PVAc gives rise to a marked stabilization effect on the thermal stability. The PMMA/PVAc blends exhibited increased notched impact properties with the inclusion of 5 wt % PVAc. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 675–684, 1998     

Stabilization of CO2‐in‐water emulsions with high internal phase volume using PVAc‐b‐PVP and PVP‐b‐PVAc‐b‐PVP as emulsifying agents

Two newly‐designed hydrocarbon surfactants, that is, poly(vinyl acetate)‐block‐poly(1‐vinyl‐2‐pyrrolidone) (PVAc‐b‐PVP) and PVP‐b‐PVAc‐b‐PVP, were synthesized using reversible addition–fragmentation chain transfer polymerization and used to form CO₂/water (C/W) emulsions with high internal phase volume and good stability against flocculation and coalescence up to 60 h. Their structures were precisely determined by nuclear magnetic resonance, gel permeation chromatography, thermal gravimetric analysis, and differential scanning calorimetry. Besides low temperature and high CO₂ pressure, the surfactant structures were the key factors affecting the formation and stability of high internal phase C/W emulsions, including the polymerization degrees of CO₂‐philic block (PVAc) and hydrophilic block (PVP), as well as the number of hydrophilic tail. The surface tension of the surfactant aqueous solution and the apparent viscosity of the C/W emulsions were also measured to characterize the surfactants efficiency and effectiveness. The surfactants with double hydrophilic tails showed stronger emulsifying ability than those with single hydrophilic tail. The great enhancement of the emulsions stability was due to decrease of the interface tension as well as increase of the steric hindrance in the water lamellae, preventing a frequent collision of CO₂ droplets and their fast coalescence. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46351.     

Remarkable improvement of thermal stability of main‐chain benzoxazine oligomer by incorporating o‐norbornene as terminal functionality

A new main‐chain benzoxazine oligomer with o‐norbornene functionality as end groups has been designed and synthesized. As compared to traditional main‐chain type benzoxazine polymers, this benzoxazine oligomer with o‐norbornene terminal functionality can undergo further crosslinking polymerization after general ring‐opening polymerization of oxazine rings. Another main‐chain benzoxazine oligomer has also been designed based on the reaction of bisphenol‐A, 4,4′‐diaminodiphenylmethane, paraformaldehyde, and phenol for comparison. The structure of the synthesized oligomers is confirmed by ¹H nuclear magnetic resonance spectroscopy and Fourier transform infrared spectroscopy (FTIR). The molecular weight has been determined by using gel permeation chromatography (GPC). The benzoxazine oligomer containing o‐norbornene functionality can polymerize with multiple polymerization mechanisms rather than the single mechanism common to traditional 1,3‐benzoxazine resins. The polymerization mechanisms are monitored by in situ FTIR and differential scanning calorimetry (DSC). Moreover, the thermoset derived from the benzoxazine oligomer containing o‐norbornene functionality exhibits high thermal stability with the transition temperature of 360 °C and a high T_d5 of 404 °C. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45408.     

In situ synthesis and characterization of polypropylene/polyvinyl acetate‐organophilic montmorillonite nanocomposite

A novel polymer‐nanoclay hybrid nanocomposite based on polyvinyl acetate (PVAc)‐organophilic montmorillonite (OMMT) has been reported via an in situ intercalated polymerization technique. The hybrid material was synthesized by one‐step emulsion polymerization of vinyl acetate in the presence of OMMT using polyvinyl alcohol as the stabilizing agent. The intercalated polymerization was characterized by X‐ray diffraction (XRD). The XRD patterns show that the interlayer spacing of OMMT after polymerization increased from 2.64 to 3.78 nm, indicating that the large macromolecular chain of PVAc was formed in the OMMT interlayer space. The Fourier transform infrared spectrum showed the characteristic absorption of PVAc in the OMMT particles separated from the nanocomposite, and the position of peaks shifted to high wave numbers. This showed that there was an interaction between PVAc and OMMT nanoparticles. A two‐fold blend composed of PVAc‐nano‐OMMT/PP was prepared by the melt‐blending technique. XRD and transmission electron microscopy images of the PVAc‐nano‐OMMT/PP composite further confirmed the formation of a partially delaminated nanocomposite structure. Thermogravimetry results showed that the thermal stability of PVAc‐nano‐OMMT/PP was greater than that of either polypropylene (PP) or Nano‐OMMT/PP blend. PVAc‐nano‐OMMT/PP had better toughness, as the mass fraction of OMMT was 5 wt %. The flame retardancy of PP, Nano‐OMMT/PP, and PVAc‐nano‐OMMT/PP composites was also studied. According to the limiting oxygen index (LOI) data and Cone calorimeter test, the addition of PVAc‐OMMT resulted in higher LOI and lower heat release rate, effective heat of combustion, smoke release course, and better flame retardancy and barrier properties. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Phase separation,cure kinetics,and morphology of epoxy/poly(vinyl acetate) blends

Epoxy based on diglycidyl ether of bisphenol A + 4,4′diaminodiphenylsulfone blended with poly(vinyl acetate) (PVAc) was investigated through differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA) and environmental scanning electron microscopy (ESEM). The influence of PVAc content on reaction induced phase separation, cure kinetics, morphology and dynamic‐mechanical properties of cured blends at 180°C is reported. Epoxy/PVAc blends (5, 10 and 15 wt % of PVAc content) are initially miscible but phase separate upon curing. DMTA α‐relaxations of cured blends agree with T_g results by DSC. The conversion‐time data revealed the cure reaction was slower in the blends than in the neat system, although the autocatalytic cure mechanism was not affected by the addition of PVAc. ESEM showed the cured epoxy/PVAc blends had different morphologies as a function of PVAc content: an inversion in morphology took place for blends containing 15 wt % PVAc. The changes in the blend morphology with PVAc content had a clear effect on the DMTA behavior. Inverted morphology blends had low storage modulus values and a high capability to dissipate energy at temperatures higher than the PVAc glass‐transition temperature, in contrast to the behavior of neat epoxy and blends with a low PVAc content. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1507–1516, 2007     

In situ emulsion polymerization and characterization of PVAc nanocomposites including colloidal silica nanoparticles for wood specimens bonding

Polyvinyl acetate (PVAc) nanocomposites for wood adhesives containing different amounts of colloidal silica nanoparticles (CSNs) were synthesized via in situ one-step emulsion polymerization. The adhesion strength of wood specimens bonded by PVAc nanocomposites was investigated by the tensile test. Thermal properties of PVAc nanocomposites were also characterized by differential scanning calorimetry and thermogravimetric analysis. Rheological and morphological properties of the PVAc nanocomposites were investigated using rheometric mechanical spectrometry and field emission scanning electron microscopy (FESEM), respectively. The obtaining results showed that the shear strength of PVAc nanocomposite including 1 wt. % CSNs has the highest shear and tensile strength about 4.7 and 3.2 MPa, respectively. A small increment of T_g (~3 °C) and considerable increment of the ash content proved the enhancement of PVAc thermal characterization in the presence of CSNs. FESEM results showed uniform dispersion of nanoparticles throughout the PVAc matrix due to using the in situ emulsion polymerization process. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48570.     

Synthesis and characterization of oligomers containing the α‐aminoalkylphenone chromophore as oligomeric photoinitiator

An oligomeric photoinitiator containing α‐aminoalkylphenone photoactive chromophore in the main chain was prepared from diphenyl ether, α‐chloroisobutyryl chloride, and piperazine through acylation, bromination, epoxidation, and polycondensation. The obtained oligomeric photoinitiator was characterized by GPC, TGA, traditional DSC, FTIR, NMR, UV–vis absorption, and fluorescence spectroscopy. The number‐average molecular weight (M_n) of the oligomeric photoinitiator was determined to be 2000–4000. The excitation and emission wavelengths of the fluorescence spectra were 376 and 473 nm, respectively. The thermal stability of the oligomer was found to be perfect with a decomposition temperature greater than 300°C. All the spectroscopic and thermal analyses clearly confirmed the consistence of property and structure. In a comparative photo‐DSC investigation, the oligomeric photoinitiator showed high photoinitiating efficiency while using 1,6‐hexanediol diacrylate as monomer. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3417–3424, 2006     

Poly(ε‐caprolactone)‐grafted acetylated anhydroglucose oligomer by ring‐opening polymerization—Synthesis and characterization

A novel acetylated anhydroglucose oligomer (AGU‐oligomer), prepared by acid catalyzed transglycosidation of potato starch triacetate and ethylene glycol, was used as a multifunctional coinitiator for the ring‐opening polymerization of ε‐caprolactone (ε‐CL). The polymers were synthesized using different weight ratios of the starting materials and were characterized by NMR, SEC, and MALLS. The results confirmed the expected P(AGU/CL) polymer structure, namely a ‘comb‐like’ graft‐copolymer having the AGU oligomer as backbone with PCL grafts of variable chain lengths (L_CL = 4–21). Thermal and mechanical properties of graft‐copolymers with different ε‐CL block lengths were examined. By changing the graft length, crystallinity was controlled and amorphous polymers were obtained with AGU‐oligomer contents higher than 50 wt %. The tensile properties varied with the composition and a copolymer having 40 wt % of AGU‐oligomer behaved like soft elastomer, showing high elongation at break. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1633–1641, 2006     

Morphology and rheological behaviors of poly(ethylene terephthalate) nanocomposites containing polyhedral oligomeric silsesquioxanes

Poly(ethylene terephthalate) (PET)/polyhedral oligomeric silsesquioxane (POSS) nanocomposites were prepared by in situ polymerization. Light scattering measurement suggested that there is significant change in molecular weight arising from gel formation by chemical crosslinking during polymerization. The thermal decomposition temperatures of the composites measured at 5 wt % weight loss were 5–10°C higher than that of PET. There is no significant change in other thermal properties. Scanning electron microscopy observations suggest that there is obvious phase separation in PET/POSS composites, composites containing 1 wt % of disilanolisobutyl and trisilanolisobytyl‐POSS show fine dispersions of POSS (30–40 nm in diameter), which arise from strong interfacial interactions between POSS and PET during polymerization. The viscosity of the composites increased with the addition of POSS. The observation of a plateau region of composites containing 1 wt % of POSS in the plot of log G′ vs. log G″ indicates strong interfacial interactions between POSS and PET. Sixty‐three percent and 41% increase in tensile strength and 300 and 380% increase in modulus were achieved in the composites containing 1 wt % of disilanol‐ and trisilanol‐POSS, respectively. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Preparation and characterization of biodegradable polymer blends from poly(3‐hydroxybutyrate)/poly(vinyl acetate)‐modified corn starch

Biodegradable polymer blends prepared by blending poly(3‐hydroxybutyrate) (PHB) and corn starch do not form intact films due to their incompatibility and brittle behavior. For improving their compatibility and flexibility, poly(vinyl acetate) (PVAc) was grafted from the corn starch to prepare the PVAc‐modified corn starch (CSV). The resulting CSV consisted of 47.2 wt% starch‐g‐PVAc copolymer and 52.8 wt% PVAc homopolymer and its structure was verified by FT‐IR analysis. In comparison with 35°C of the neat PVAc, the glass transition temperature (T_g) of the grafted PVAc chains on starch‐g‐PVAc was higher at 44°C because of the hindered molecular mobility imposed from starch on the grafted PVAc. After blending PHB with the CSV, structure and thermal properties of the blends were investigated. Only a single T_g was found for all the PHB/CSV blends and increased with increasing the CSV content. The T_g‐composition dependence of the PHB/CSV blends was well‐fitted with the Gordon‐Taylor equation, indicating that the CSV was compatible with the PHB. In addition, the presence of the CSV could raise the thermal stability of the PHB component. It was also found that the presence of the PHB and PVAc components would not hinder the enzymatic degradation of the corn starch by α‐amylase. POLYM. ENG. SCI., 55:1321–1329, 2015. © 2015 Society of Plastics Engineers     

Effects of hetero-armed star-shaped PCL-PLA polymers with POSS core on thermal,mechanical, and morphological properties of PLA

In this study, AB type-heteroarm star-shaped poly(ε-caprolactone)-poly(lactic acid) (PCL-PLA) polymers with polyhedral oligomeric silsesquioxane (POSS) core ((PCL)₄-POSS-(PLA)₄, coded as SPLA) were synthesized successfully by using ring opening polymerization and click chemistry techniques together. The synthesized polymers were compounded with commercial PLA at different blending ratios (PLA/SPLA = 100/0, 95/5, 90/10, and 80/20% wt). The effects of heteroarm SPLA polymers having different arm lengths (n = 10, 20, 30, and 50) on morphological, mechanical, and thermal behaviors of PLA were investigated. It is determined that SPLA polymers with four PLA and four PCL arms on its structure enhanced mechanical properties of PLA. The tensile modulus decreased, and lowest modulus values were observed with blends prepared at 80/20 ratio. Elongation at break values increased in all blends, maximum increment was observed with 1,4-phenylene diisocyanate (PDI) containing SPLA20 blends prepared at 90/10 ratio. This result showed that SPLA20 had optimum chain length for chain extension reactions of between PLA chains. Besides, a trade compatibilizer PDI was utilized to enhance the intercompatibility of binary polymer blends.     

Enhanced fracture toughness of epoxy resins with novel amine‐terminated poly(arylene ether sulfone)–carboxylic‐terminated butadiene‐acrylonitrile–poly(arylene ether sulfone) triblock copolymers

Amine‐terminated poly(arylene ether sulfone)–carboxylic‐terminated butadiene‐acrylonitrile–poly(arylene ether sulfone) (PES‐CTBN‐PES) triblock copolymers with controlled molecular weights of 15,000 (15K) or 20,000 (20K) g/mol were synthesized from amine‐terminated PES oligomer and commercial CTBN rubber (CTBN 1300x13). The copolymers were utilized to modify a diglycidyl ether of bisphenol A epoxy resin by varying the loading from 5 to 40 wt %. The epoxy resins were cured with 4,4′‐diaminodiphenylsulfone and subjected to tests for thermal properties, plane strain fracture toughness (K_IC), flexural properties, and solvent resistance measurements. The fracture surfaces were analyzed with SEM to elucidate the toughening mechanism. The properties of copolymer‐toughened epoxy resins were compared to those of samples modified by PES/CTBN blends, PES oligomer, or CTBN. The PES‐CTBN‐PES copolymer (20K) showed a K_IC of 2.33 MPa m^0.5 at 40 wt % loading while maintaining good flexural properties and chemical resistance. However, the epoxy resin modified with a CTBN/8K PES blend (2:1) exhibited lower K_IC (1.82 MPa m^0.5), lower flexural properties, and poorer thermal properties and solvent resistance compared to the 20K PES‐CTBN‐PES copolymer‐toughened samples. The high fracture toughness with the PES‐CTBN‐PES copolymer is believed to be due to the ductile fracture of the continuous PES‐rich phases, as well as the cavitation of the rubber‐rich phases. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 1556–1565, 2002; DOI 10.1002/app.10390     

Incorporation of metallic POSS,POSS copolymers,and new functionalized POSS compounds into commercial dental resins

An array of polyhedral oligomeric silsesquioxane (POSS) compounds, including metal, methacrylate, and amine functional POSS, and POSS copolymers were incorporated into aromatic and aliphatic dental resins. Heptaphenyl‐propylamine POSS and methacrylate derivatives were synthesized by corner‐capping and Michael addition reactions, respectively. The POSS compounds were tested for solubility in commercial resins at concentrations of 1, 5, 10, and 15 wt %, followed by UV polymerization of all soluble combinations. The POSS compounds generally increased modulus and had an unpredictable effect on T_g. The modulus of the aliphatic resin increased 83% by incorporation of 15 wt % aluminum‐phenyl POSS, while aromatic resins saw a maximum modulus improvement of 18% at 30°C and 72% at 160°C by incorporating 1 wt % of heptaphenyl‐methacrylate POSS. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 2856–2862, 2006     

Preparation of high molecular weight poly(vinyl alcohol) with high yield using low‐temperature solution polymerization of vinyl acetate

Vinyl acetate (VAc) was solution‐polymerized in tertiary butyl alcohol (TBA) and in dimethyl sulfoxide (DMSO) having low chain transfer constant at 30, 40, and 50°C, using a low temperature initiator, 2,2′‐azobis(2,4‐dimethylvaleronitrile) (ADMVN). The effects of polymerization temperature and initiator concentration were investigated in terms of polymerization behavior and molecular structures of poly(vinyl acetate) (PVAc) and corresponding poly(vinyl alcohol) (PVA) obtained by saponification with sodium hydroxide. The polymerization rates of VAc in TBA and in DMSO were proportional to the 0.49 and 0.72 powers of ADMVN concentration, respectively. For the same polymerization conditions, TBA was absolutely superior to DMSO in increasing the molecular weight of PVA. In contrast, TBA was inferior to DMSO in causing conversion to polymer, indicating that the initiation rate of VAc in TBA was lower than that in DMSO. These effects could be explained by a kinetic order of ADMVN concentration calculated using initial rate method and by an activation energy difference of polymerization obtained from the Arrhenius plot. Low‐temperature solution polymerization of VAc in TBA or DMSO by adopting ADMVN proved successful in obtaining PVA of high molecular weight (number–average degree of polymerization (P_n): 4100–6100) and of high yield (ultimate conversion of VAc into PVAc: 55–80%) with diminishing heat generated during polymerization. In the case of bulk polymerization of VAc at the same conditions, maximum P_n and conversion of 5200–6200 and 20–30% was obtained, respectively. The P_n and lightness were higher, and the degree of branching was lower with PVA prepared from PVAc polymerized at lower temperatures in TBA. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1003–1012, 2001     

Synthesis of random and block copolymers of vinyl chloride and vinyl acetate by RAFT miniemulsion polymerizations mediated by a fluorinated xanthate

Reversible addition–fragmentation chain transfer miniemulsion (co)polymerizations of vinyl acetate (VAc) and vinyl chloride (VC) are conducted in the presence of a fluorinated xthanate (X1). VAc miniemulsion polymerization can be well controlled by X1, and PVAc with small polydispersity index (PDI, <1.20) are obtained. X1 also shows well mediative effect to VC‐VAc miniemulsion copolymerization, while the PDI of VC‐VAc copolymer is greater than that of PVAc since a chain transfer rate to VC is greater than that to VAc. PVAc‐b‐PVC copolymers are synthesized by VC miniemulsion polymerizations mediated by X1‐terminated PVAc. PDIs of PVAc‐b‐PVC copolymers are greater than that of PVAc and VC‐VAc random copolymers with close monomer compositions, and increase with the increase of VC conversion. This is caused by the increased chain transfer to monomer and the formation of monomer‐rich and polymer‐rich phases during the VC polymerization stage. As‐prepared PVAc‐b‐PVC copolymers exhibit a micro‐phase separated morphology. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45074.     

Polyhedral oligomeric silsesquioxane/silica/polydimethylsiloxane rubber composites with enhanced mechanical and thermal properties

Composites of polydimethylsiloxane (PDMS) rubber modified by three kinds of polyhedral oligomeric silsesquioxanes (POSSs) as well as fumed silica were prepared through solution blending and then open two‐roll mill blending with curing agent. Subsequently, the influences of POSS on mechanical and thermal properties of the resulting composites were investigated in detail. The addition of POSS significantly enhanced the tensile strength and elongation at break of the composite but lowered the tensile modulus, which could be ascribed to the interruption of silica–silica and silica–PDMS interactions. Octamethylsilsesquioxane (OMS)/silica/PDMS and octaphenylsilsesquioxane (OPS)/silica/PDMS composites did not show desirable mechanical and thermal properties. Nevertheless, heptaphenylvinylsilsesquioxane (VPS)/silica/PDMS composite with 5 wt % VPS exhibited enhanced glass transition temperature (T_g), mechanical properties, and thermal stability. Further studies revealed that more VPS unfavorably affected properties of the composite. Scanning electron microscope and X‐ray diffraction demonstrated that owing to the grafting reaction, 5 wt % VPS in the rubber matrix could form microcrystal domains the most effectively. Thus, the improved mechanical properties and thermal stability just resulted from the the formation of microcrystal domains and the increase in stiffness of PDMS chains because of the graft of VPS onto PDMS. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42173.     

Polyimide aerogels crosslinked through cyclic ladder‐like and cage polyamine functionalized polysilsesquioxanes

Polyimide (PI) aerogels with high porosity, low thermal conductivity, flexibility, low density, and excellent mechanical properties have attracted attention. However, the effect of crosslinker on structures and properties has not been investigated. Preparation of non‐shrinkable, aerogels with excellent performance is still a challenge. A series of PI aerogels are prepared through the polyamic acid oligomer reacting with different crosslinking agents: 1,3,5‐triaminophenoxybenzene (TAB), caged octa(aminophenyl) silsesquioxane, and cyclic ladder‐like poly(aminophenyl) silsesquioxanes. The shrinkage, density, porosity, and compression measurements of the PI aerogels indicate that the PI–polyhedral oligomeric silsesquioxanes (POSS) aerogels show more stable and stronger structures than with the TAB. The physical properties reveal that the introduction of POSS brings more compact and stable crosslinking network structures. The thermal properties of the PI aerogels are tested by dynamic mechanical analysis, thermal gravimetric analysis, and Transient Hot Wire method. The PI–POSS aerogels showed much better thermal stability, lower thermal conductivities, and better thermal insulation. Stable inorganic cores and rigid molecular structures of POSS result in strong mechanical properties, high thermal stability, and low thermal conductivities of the PI aerogels which may have important application in thermal protection against high temperature. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45296.     

1H NMR,thermal, and conductivity studies on PVAc based gel polymer electrolytes

The lithium‐ion conducting gel polymer electrolytes (GPE), PVAc‐DMF‐LiClO₄ of various compositions have been prepared by solution casting technique. ¹H NMR results reveal the existence of DMF in the gel polymer electrolytes at ambient temperature. Structure and surface morphology characterization have been studied by X‐ray diffraction analysis (XRD) and scanning electron microscopy (SEM) measurements. Thermal and conductivity behavior of polymer‐ and plasticizer‐salt complexes have been studied by differential scanning calorimetry (DSC), TG/DTA, and impedance spectroscopy results. XRD and SEM analyses indicate the amorphous nature of the gel polymer‐salt complex. DSC measurements show a decrease in T_g with the increase in DMF concentrations. The thermal stability of the PVAc : DMF : LiClO₄ gel polymer electrolytes has been found to be in the range of (30–60°C). The dc conductivity of gel polymer electrolytes, obtained from impedance spectra, has been found to vary between 7.6 × 10^?7 and 4.1 × 10^?4 S cm^?1 at 303 K depending on the concentration of DMF (10–20 wt %) in the polymer electrolytes. The temperature dependence of conductivity of the polymer electrolyte complexes appears to obey the VTF behavior. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Properties of poly(butylene terephthalate) chain‐extended by epoxycyclohexyl polyhedral oligomeric silsesquioxane

Epoxycyclohexyl polyhedral oligomeric silsesquioxane (epoxy–POSS) was used to prepare a chain‐extended poly(butylene terephthalate) (PBT) with a twin‐screw extruder. The effect of epoxy–POSS on the melt flow index, mechanical properties, rheological behavior, and thermal properties of chain‐extended PBT was investigated. PBT had an intrinsic viscosity of 1.1 dL/g and a carboxy1 content of 21.6 equiv/10⁶ g, but the PBT chain‐extended with 2 wt % epoxy–POSS had an intrinsic viscosity of 1.7 dL/g and a carboxy1 content lower than 7 equiv/10⁶ g. After the addition of epoxy–POSS, the melt flow index of PBT dramatically decreased, the elongation at break increased greatly, the tensile strength increased slightly, and the thermal stability was also improved. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008