Synthesis and properties of BCDA‐based polyimide–clay nanocomposites

Bicyclo[2.2.2]oct‐7‐ene‐2,3,5,6‐tetracarboxylic dianhydride (BCDA)‐based polyimide–clay nanocomposites were prepared from their precursor, namely polyamic acid, by a solution‐casting method. The organoclay was prepared by treating sodium montmorillonite (Kunipia F) clay with dodecyltrimethylammonium bromide at 80 °C. Polyamic acid solutions containing various weight percentages of organoclay were prepared from 4,4′‐(4,4′‐isopropylidenediphenyl‐1,1′‐diyldioxy)‐dianiline and BCDA in N‐methyl‐2‐pyrrolidone containing dispersed particles of organoclay at 20 °C. These solutions were cast on a glass plate using a Doctor's blade and then heated subsequently to obtain nanocomposite films. The nanocomposites were characterized using Fourier transform infrared spectroscopy, differential scanning calorimetry, thermal mechanical analysis, dynamic mechanical analysis, polarizing microscopy, scanning electron microscopy, transmission electron microscopy, wide‐angle X‐ray diffraction (WAXD) and thermogravimetric analysis. The glass transition temperature of the nanocomposites was found to be higher than that of pristine polymer. The coefficient of thermal expansion of the nanocomposites decreased with increasing organoclay content. WAXD studies indicated that the extent of silicate layer separation in the nanocomposite films depended upon the organoclay content. Tensile strength and modulus of the nanocomposite containing 1% organoclay were significantly higher when compared to pristine polymer and other nanocomposites. The thermal stability of the nanocomposites was found to be higher than that of pristine polymer in air and nitrogen atmosphere. Copyright © 2007 Society of Chemical Industry     

Preparation and characterisation of polyamide–polyimide organoclay nanocomposites

BACKGROUND: Ternary nanocomposites containing an organomodified layered silicate polyimide additive within a polyamide matrix have been investigated to gain greater insight into structure–property relationships and potential high‐temperature automotive applications. RESULTS: Polyamide nanocomposite blends, containing 3 wt% of organoclay, were prepared and compared with organoclay‐reinforced polyamide and neat polyamide. Nanoclay addition significantly increased heat distortion temperature, as well as both the tensile and flexural moduli and strength. The addition of polyimide demonstrated further increases in heat distortion temperature, glass transition temperature and the flexural and tensile moduli by about 17, 21 and 40%, respectively. The tensile and flexural strengths were either unaffected or decreased modestly, although the strain‐to‐failure decreased substantially. Morphological studies using transmission electron microscopy (TEM) and X‐ray diffraction showed that the nanoclay was dispersed within the ternary blends forming highly intercalated nanocomposites, regardless of the presence and level of polyimide. However, TEM revealed clay agglomeration at the polyamide–polyimide interface which degraded the mechanical properties. CONCLUSIONS: A range of improvements in mechanical properties have been achieved through the addition of a polyimide additive to a polyamide nanocomposite. The decrease in ductility, arising from the poor polyamide–polyimide interface and nanoclay clustering, clearly requires improving for this deficiency to be overcome. Copyright © 2008 Society of Chemical Industry     

Preparation and characterization of poly(hydroxybutyrate‐co‐hydroxyvalerate)–organoclay nanocomposites

This study describes the microstructure and thermal and mechanical properties of poly(hydroxybutyrate‐co‐hydroxyvalerate) (PHB/HV)–organoclay nanocomposites prepared by melt intercalation using Cloisite 30B, a monotallow bis‐hydroxyethyl ammonium‐modified montmorillonite clay. X‐ray diffractometry and transmission electron microscopy analyses clearly confirm that an intercalated microstructure is formed and finely distributed in the PHB/HV copolymer matrix because PHB/HV has a strong hydrogen bond interaction with the hydroxyl group in the organic modifier of Cloisite 30B. The nanodispersed organoclay also acts a nucleating agent, increasing the temperature and rate of crystallization of PHB/HV; therefore, the thermal stability and tensile properties of the organoclay‐based nanocomposites are enhanced. These results confirm that the organoclay nanocomposite greatly improves the material properties of PHB/HV. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 525–529, 2003     

Synthesis and properties of polyimide (containing naphthalene) nanocomposites with organo‐modified montmorillonites

2,7‐Bis(4‐aminophenoxy) naphthalene (BAPN), a naphthalene‐containing diamine, was synthesized and polymerized with a 3,3′,4,4′‐benzophenone tetracarboxylic dianhydride (BTDA) to obtain a polyimide (PI) via thermal imidization. To enhance the thermal and mechanical properties of the polymer, PI–Montmorillonite (MMT) nanocomposites were prepared from a DMAc solution of poly(amic acid) and a DMAc dispersion of MMT, which were organo‐modified with various amounts of n‐dodecylamine (DOA) or cetylpyridium chloride (CPC). FTIR, XRD, and TEM (transmission electron microscopy) were used to verify the incorporation of the modifying agents into the clay structure and the intercalation of the organoclay into the PI matrix. Results demonstrated that the introduction of a small amount of MMT (up to 5%) led to the improvement in thermal stability and mechanical properties of PI. The decomposition temperature of 5% weight loss (T_d,5%) in N₂ was increased by 46 and 36°C in comparison with pristine PI for the organoclay content of 5% with DOA and CPC, respectively. The nanocomposites were simultaneously strengthened and toughened. The dielectric constant, CTE, and water absorption were decreased. However, at higher organoclay contents (5–10%), these properties were reduced because the organoclay was poorly dispersed and resulted in aggregate formation. The effects of different organo‐modifiers on the properties of PI–MMT nanocomposite were also studied; the results showed that DOA was comparable with CPC. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

Photosensitive poly(amic acid)/organoclay nanocomposites

A project was carried out aimed at reducing the coefficient of thermal expansion (CTE) of photosensitive polyimide formulations (photoresists) through the incorporation of small amounts of an organoclay. The organoclay was formed by a cation exchange reaction between a NA⁺-montmorillonite clay and an ammonium salt of dodecylamine. Two polyimide precursors, a poly(amic ester) (PAE) and a poly(amic acid) (PAA), were used in this study. The PAE was prepared by direct polymerization of 2,2′-bis-(3-amino-4-hydroxyphenyl)hexafluoropropane and bis(n-butyl)ester of pyromellitic acid in the presence of phenylphosphonic dichloride as an activator. The polymer had an inherent viscosity of 0.23 dL/g. The PAA copolymer was prepared by polymerization of pyromellitic dianhydride, oxydiphthalic anhydride and oxydianiline. The polymer had an inherent viscosity of 1.00 dL/g. Two photosensitive resin/clay formulations were prepared from these two PI precursors using 2,3,4-tris(1-oxo-2-diazonaphthoquinone-5-sulfonyloxy)-benzophenone as the photosensitizer and 3 wt% organoclay. The films obtained from the PAA formulation were transparent and tough, while the films prepared from the PAE formulation were opaque and brittle. Both X-ray diffraction and transmission electron microscope analyses showed that, although the organoclay was not dispersed well in the PAE matrix, it was dispersed in the PAA matrix on a nanometer scale. The clay particles remained well dispersed after the PAA film was thermally imidized. The CTE of the polyimide film obtained was 23% lower than that of a similar film that did not contain the organoclay. The temperature at which the polyimide underwent a 5% weight loss when subjected to TGA in nitrogen was also increased by 13%. The photosensitive PAA/clay nanocomposite showed a sensitivity of 301 mJ/cm² and a contrast of 1.66 when a 0.2 wt% tetramethylammonium hydroxide developer was used. A line/space pattern with a resolution of 10 μm was obtained from this formulation.     

Synthesis and photoconductive characteristics of biphenylporphyrin‐containing poly(amic acid)s and polyimides

Three series of biphenylporphyrin (BPP)‐containing poly(amic acid)s (PAAs) were synthesized and converted into heat‐treated polyimides (HPIs) and chemically treated polyimides (CPIs). Viscosity measurements, UV–vis and IR spectroscopies, as well as thermogravimetric analysis (TGA), were used to characterize the structures of the polymers. UV–vis spectra revealed that the BPP units formed aggregates in PAA and CPI films, rather than in HPI films. Photoinduced discharge was used to characterize the photoconductive properties of these polymer films. It was found that the photosensitivity was greatly enhanced by introducing BPP units into the polymer chains. For these three series of polymers, the photosensitivity increased in the order PAA < HPI < CPI according to the content of BPP in the polymers. The photoconductive characteristics were interpreted by the intrinsic π—π* process of BPP aggregation and the extrinsic process of charge‐transfer complex formation. The best photoconductive performances of the CPIs were attributed to the existence of two charge‐carrier‐generation processes. Copyright © 2004 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     

Influence of organic modification on mechanical properties of melt processed intercalated poly(methyl methacrylate)–organoclay nanocomposites

The influence of organic modifiers on intercalation extent, structure, thermal and mechanical properties of poly(methyl methacrylate) (PMMA)–clay nanocomposites were studied. Two different organic modifiers with varying hydrophobicity (single tallow versus ditallow) were investigated. The nanocomposites were prepared from melt processing method and characterized using wide angle X‐ray diffraction, transmission electron microscopy, thermogravimetric analysis, differential scanning calorimetry (DSC), and tensile tests. Mechanical properties such as tensile modulus (E), break stress (σ_brk), and % break strain (ε_brk) were determined for nanocomposites at various clay loadings. Extent of PMMA intercalation is sufficient and in the range 9–15 Å depending on organoclay and filler loading. Overall thermal stability of nanocomposites increases by 16–30°C. The enhancement in T_g of nanocomposite is merely by 2–4°C. With increase in clay loading, tensile modulus increases linearly while % break strain decreases. Break stress is found to increase till 4 wt % and further decreases at higher clay loadings. The overall improvement in thermal and mechanical properties was higher for the organoclay containing organic modifier with lower hydrophobicity and single tallow amine chemical structure. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synthesis and characterization of novel oligomeric poly(styrene‐co‐acrylonitrile)–clay complexes

Oligomeric poly(styrene‐co‐acrylonitrile) quaternary ammonium salts were prepared through reactions of trimethylamine with corresponding poly(styrene–acrylonitrile–vinyl benzyl chloride)s, which were synthesized by the free‐radical polymerization of a mixture of styrene, acrylonitrile, and vinyl benzyl chloride. Then, oligomeric poly(styrene‐co‐acrylonitrile)‐modified clays were prepared through the cation exchange of the sodium ions in the clay with the corresponding poly(styrene‐co‐acrylonitrile) quaternary ammonium salts. The poly(styrene–acrylonitrile–vinyl benzyl chloride)s, poly(styrene‐co‐acrylonitrile) quaternary ammonium salts, and their clay complexes were characterized with infrared spectroscopy, gel permeation chromatography, thermogravimetric analysis, proton nuclear magnetic resonance, X‐ray diffraction, and transmission electron microscopy. X‐ray diffraction and transmission electron microscopy studies showed that these novel clay complexes were well intercalated. Furthermore, thermogravimetric analysis data indicated that this series of polymerically modified clays had high enough thermal stability for nanocomposites by melt blending. The thermal treatment of one of these novel clays at 250°C under nitrogen was also conducted. Solubility and infrared studies of this thermally treated clay complex revealed that a novel polyimine/enamine structure clay complex had been formed in the gallery of the clay. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

聚酰胺酸的合成及其酰亚胺化研究

采用均苯四酸二酐(PMDA)和4,4'-二氨基二苯醚(ODA)为单体,N,N-二甲基乙酰胺(DMAc)为溶剂,合成聚酰亚胺的前驱体聚酰胺酸(PAA)。研究了溶剂体系、反应温度、时间、投料比和总固含量等因素对所得聚酰胺酸特性黏度的影响。试制了聚酰胺酸和聚酰亚胺(PI)薄膜,对其进行了红外光谱分析及力学性能测试。     

Poly(m‐xylene adipamide)–kaolinite and poly(m‐xylene adipamide)–montmorillonite nanocomposites

Two clay compounds, montmorillonite (Cloisite 30B) and kaolinite, were dispersed in a poly(m‐xylene adipamide) resin at loading levels of 2 wt % clay. The samples were melt‐compounded and extruded. The extruded samples were injection‐molded into preforms and then blow‐molded into multilayer bottles. Rheology, calorimetry, electron microscopy, and gas‐transport measurements were performed. Both clays were nucleating agents, giving crystallite sizes that did not cause haze. Kaolinite was more difficult to exfoliate than montmorillonite, and under similar processing conditions, kaolinite resulted in a higher degree of crystallinity. Both nanocomposites exhibited improved gas‐barrier properties over the neat resin. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 1377–1381, 2007     

Synthesis and characterization of poly(acrylate amic acid) and its application as negative‐tone photosensitive polyimides

The dianhydride monomer 3,3′,4,4′‐benzophenone tetracarboxylic acid dianhydride and two diamine monomers, 4,4′‐diamino‐3,3′‐biphenyldiol (HAB) and 2,4‐diaminophenol dihydrochloride (DAP), were used to synthesize a series of poly(hydroxyl amic acid). Further functionalization by grafting acrylate groups yields the corresponding poly(acrylate amic acid) that underwent a crosslinking reaction on exposure to UV‐light and was used as a negative‐tone photosensitive polyimide (PSPI). The analysis of chemical composition and molecular weight of these poly(amic acid)s determined by nuclear magnetic resonance (NMR) spectroscopy, Fourier transform infrared spectroscopy, and gel permeation chromatography revealed that the molecular weight of the poly(hydroxyl amic acid) increased with the molar content of HAB in the feedstock, because HAB exhibited higher polymerization reactivity than DAP. Moreover, the degree of grafting acrylate groups onto poly(hydroxyl amic acid) was determined by ¹H‐NMR spectroscopy. The photoresist was formulated by adding 2‐benzyl‐2‐N,N‐dimethylamino‐1‐(4‐morpholinophenyl) butanone (IRG369) and isopropylthioxanthone as a photoinitiator, tetra(ethylene glycol) diacrylate as a crosslinker, and tribromomethyl phenyl sulfone as a photosensitizer. The PSPI precursor exhibited a photosensitivity of 200 mJ/cm² and a contrast of 1.78. A pattern with a resolution of 10 μm was observed in an optical micrograph after thermal imidization at 300°C. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Thermal behavior of poly(acrylic acid)–poly(vinyl pyrrolidone) and poly(acrylic acid)–metal–poly(vinyl pyrrolidone) complexes

Thermal analysis (TGA and DTA) of samples of PAA, PVP, PAA–PVP complexes, containing different weight fractions of PAA and ternary polymer–metal–polymer complexes, were studied. The activation energy parameters for the thermal degradation were also calculated. The study of the effect of FeCl₃, NiCl₂, and Ni(NO₃)₂ on the TGA and DTA curves of the complexes showed that the decompositions are dependent on the concentrations and the nature of the metal ions. The DTA traces of PAA–PVP complex containing FeCl₃, NiCl₂, and Ni(NO₃)₂ showed that the treatment of the complex with these metal ions causes considerable changes in the thermal decomposition of PAA–PVP complex. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 4049–4057, 2006     

Plasticized and nanofilled poly(lactic acid)‐based cast films: Effect of plasticizer and organoclay on processability and final properties

PLA‐based nanocomposites filled with the commercial organomodified montmorillonite Dellite 43B (D43B) and containing acetyl tri‐n‐butyl citrate (ATBC) as plasticizer were prepared by extrusion in a pilot‐scale twin‐screw extruder and melt casted into flexible films. A preliminary investigation was carried out in a laboratory batch mixer by varying blending conditions and addition procedures of the components. Indeed, the method of addition of ATBC and D43B considerably affected thermo‐mechanical properties and morphology of the resultant nanocomposites. The simultaneous introduction of both ATBC and D43B during the extrusion process allowed producing clearly exfoliated nanocomposite materials with modulated mechanical and thermal properties. Moreover, rheological results, obtained during melt extrusion, assessed the processability of nanofilled‐plasticized PLA, making this simple procedure interesting in view of the industrial production of nanostructured biomaterials based on plasticized PLA. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2013     

Preparation and degradability of poly(lactic acid)–poly(ethylene glycol)–poly(lactic acid)/SiO2 hybrid material

Poly(lactic acid)–poly(ethylene glycol)–poly(lactic acid) (PLA‐PEG‐PLA)/SiO₂ hybrid material is prepared by sol–gel method using tetraethoxysilane (TEOS) and PLA‐PEG‐PLA as raw material. From Fourier transform infrared spectroscopy (FTIR) and X‐ray photoelectron spectroscopy (XPS) spectra, the hydroxyl groups of the silica sol derived from partially hydrolysis of TEOS and the unhydrolyzed ethoxy groups of TEOS can react with PLA‐PEG‐PLA. Differential scanning calorimetry (DSC) curves imply that the glass transition temperature (T_g) of PLA‐PEG‐PLA/SiO₂ hybrid material is higher than that of PLA‐PEG‐PLA and increases with the increase of silica content. X‐ray diffraction (XRD) analysis results show that PLA‐PEG‐PLA and PLA‐PEG‐PLA/SiO₂ hybrid material are both amorphous. Field scanning electron microscope (FSEM) photographs show that when PLA‐PEG‐PLA/SiO₂ hybrid material has been degraded for 12 weeks in normal saline at 37°C, a three‐dimensional porous scaffold is obtained, which is available for cell growth and metabolism. Moreover, the hydroxyl (? OH) groups on SiO₂ of PLA‐PEG‐PLA/SiO₂ hybrid material could buffer the acidity resulted from the degradation of PLA, which is beneficial to proliferation of cell in tissue repairing. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and characterization of poly(2‐ethylaniline)–poly(styrenesulfonic acid) and poly(o‐phenetidine)–poly(styrenesulfonic acid) complexes

This research focuses on the synthesis of ethyl and ethoxy substituted polyaniline with poly(styrenesulfonic acid) comprising a poly(o‐phenetidine)–poly(styrenesulfonic acid) [P(O? P)‐PSSA] and poly(2‐ethylaniline)–poly(styrenesulfonic acid) [P(2‐E)‐PSSA]. The complexes P(O? P)‐PSSA and P(2‐E)‐PSSA were prepared by chemical polymerization of monomer (o‐phenetidine, 2‐ethylaniline) with PSSA using an oxidant of ammonium persulfate in 1M HCl solution; polyaniline (PANI), poly(2‐ethylaniline) (P2E), poly(o‐pheneditine) (POP), and polyaniline‐poly(styrenesulfonic acid) (PANI‐PSSA) also were prepared by chemical polymerization to be the reference samples. The products were characterized by IR, VIS, EPR, water solubility, elemental analysis, conductivity, SEM, and TEM. IR spectral studies shown that the structure of P(2‐E)‐PSSA and P(O? P)‐PSSA complexes is similar to that of polyaniline. EPR and visible spectra indicate the formation of polarons. The morphology of the blend was investigated by measured SEM and TEM, indicating the conducting component and electrically conductive property of the polymer complexes. The pH value for deprotonation [pH ≥ 9.5 for P(2‐E)‐PSSA and pH ≥ 8.0 for P(O? P)‐PSSA] are higher than that of corresponding HCl salts, indicating an intimate interaction between polymer chains. Elemental analysis results show that P(O? P)‐PSSA has a nitrogen‐to‐sulfur ratio of ～52%, larger than that for P(2‐E)‐PSSA, ～41%. The conductivity of the complexes is around 10^?2S/cm, and the solubility of P(2‐E)‐PSSA and P(O? P)‐PSSA in water is 2.9 and 1.9 g/L, respectively. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 1198–1205, 2005     

Fiber spinning from poly(propylene)–organoclay nanocomposite

SOMASIF ME C16, a filler that enables generation of anisotropic nanoparticles by in situ exfoliation of organic layered silicates, was melt compounded with poly(propylene) (PP) in the presence of maleic anhydride‐grafted PP. Fibers were prepared from this composite by a spinning procedure. The prepared anisotropic fibers were partially oriented by using different drawing ratios. The morphological study showed that the drawing ratio of the fibers particularly influences the level of exfoliation of the SOMASIF ME C16 where the nanoparticles are formed. The layered sheets of the SOMASIF particles are oriented in the direction of the fiber axis. The tensile strength of the filled fibers increases with the increase of drawing ratio much more than that of unfilled PP fibers. This result is accounted for by the formation of exfoliated structures from the nanoparticles of SOMASIF ME C16 by fiber drawing. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 604–611, 2003     

Synthesis and characterization of poly(urethane‐benzoxazine)/clay hybrid nanocomposites

Poly(urethane‐benzoxazine)/clay hybrid nanocomposites (PU/Pa–OMMTs) were prepared from an in situ copolymerization of a polyurethane (PU) prepolymer and a monofunctional benzoxazine monomer, 3‐phenyl‐3,4‐dihydro‐2H‐1,3‐benzoxazine (Pa), in the presence of an organophilic montmorillonite (OMMT), by solvent method using DMAc. OMMT was made from cation‐exchange of Na‐montmorillonite (MMT) with dodecyl ammonium chloride. The formation of the exfoliated nanocomposite structures of PU/Pa‐OMMT was confirmed by XRD from the disappearance of the peak due to the basal diffraction of the layer‐structured clay found in both MMT and OMMT. DSC showed that, in the presence of OMMT, the curing temperature of PU/Pa lowered by ca. 60°C for the onset and ca. 20°C for the maximum. After curing at 190°C for 1 h, the exothermic peak on DSC disappeared. All the obtained films of PU/Pa–OMMT were deep yellow and transparent. As the content of OMMT increased, both the tensile modulus and strength of PU/Pa–OMMT films increased, while the elongation decreased. The characteristics of the PU/Pa–OMMT films changed from plastics to elastomers depending on OMMT content and PU/Pa ratio. PU/Pa–OMMT films also exhibited excellent resistance to the solvents such as tetrahydrofuran, N,N‐dimethylformamide and N‐methyl‐2‐pyrrolidinone. The thermal stability of PU/Pa were enhanced remarkably even with small amount of OMMT. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 4075–4083, 2003     

Morphology and thermal properties of poly(L‐lactic acid)/organoclay nanocomposites

A modified clay was used to prepare poly(L ‐lactic acid)/clay nanocomposite dispersions. X‐ray diffraction and transmission electron microscopy experiments revealed that poly(L ‐lactic acid) was able to intercalate the clay galleries. IR spectra of the poly(L ‐lactic acid)/clay nanocomposites showed the presence of interactions between the exfoliated clay platelets and the poly(L ‐lactic acid). Thermogravimetric analysis and differential scanning calorimetry were performed to study the thermal behavior of the prepared composites. The properties of the poly(L ‐lactic acid)/clay nanocomposites were also examined as functions of the organoclay content. The exfoliated organoclay layers acted as nucleating agents, and as the organoclay content increased, the crystallization temperature increased. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Phase segregation and viscoelastic behavior of poly(ether urethane urea)s

Two poly(ether urethane urea)s were synthesized, one based on poly(propylene glycol) and another one on poly(tetramethylene glycol). Hydrogenated MDI was used as the diisocyanate and propylenediamine as the chain extender. The diisocyanate : polyol : diamine molar ratio was 2 : 1 : 1 for both copolymers. Data from stress-relaxation tests were adjusted to a power law and to the Kohlraush-William-Watts equation. Phase separation and viscoelastic behavior were correlated through the calculation of the time-relaxation spectrum, the steady-state tensile compliance, and the tensile viscosity. The results indicated that the material based on poly(tetramethylene glycol) was the more effectively phase-segregated block copolymer. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 2227–2236, 1997