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1.
Hydrophobic organic montmorillonite (OMMT) which exists as stable dispersions in cyclohexane has been prepared by the combined modification of quaternary ammonium salts and coupling agents, and polybutadiene (PB)/OMMT nanocomposites (NCs) were successfully synthesized by in situ living anionic polymerization. The results showed that the interlayer spacing of OMMT increased dramatically on increasing the length of the long alkyl chain of C12, C16, C18 and C22 in n‐alkyltrimethylammonium ions and the number of long alkyl chains of 1C16, 2C16 and 3C16 in hexadecylmethylammonium ions. The interlayer spacings reached 4.9 and 5.07 nm, respectively, when C22 and 3C16 were used. The dispersion of MMT intercalated by quaternary ammonium salts was improved significantly after surface modification by different coupling agents, and the OMMTs could be disperses stably in cyclohexane for at least 72 h. In addition, the coupling agents did not change the inherent intercalation structure of OMMT. The results from a kinetic study and 1H NMR analysis indicated that the incorporation of OMMT had little influence on the living polymerization and PB microstructure (proportions of 1,2‐ and 1,4‐units) when the OMMT content was below 3 wt%. However, the OMMT modified by different coupling agents had some influence on the molecular weight distribution. The results from transmission electron microscopy and X‐ray diffraction revealed that exfoliated structures of clay were obtained for all NCs. Furthermore, the results of differential scanning calorimetry and thermogravimetric analysis indicated that Tg and Tdc of NCs were increased compared to those of PB. Copyright © 2006 Society of Chemical Industry  相似文献   

2.
A novel elastomeric polyurethane (EPU)/organic montmorillonite (OMMT) nanocomposite has been synthesized. 18 Alkane‐3 methyl‐amine chloride and dihydroxethyl‐12 alkane‐3 methyl‐amine chloride were used as intercalation agents to treat Na+‐montmorillonite and for forming two kinds of OMMTs. The better OMMT was chosen according to fourier transform infrared spectroscopy (FTIR) and wide angle X‐ray diffraction (WAXD). Three types of EPU/OMMT nanocomposites were synthesized by in situ polymerization of EPU, with different amounts of OMMT. A combination of FTIR, WAXD, and transmission electronic microscopy (TEM) studies showed that EPU/OMMT composites were on the nanometer scale and the segmented structure of EPU was hindered by the presence of the OMMT, due to the reaction between toluene diisocyanate (TDI) and the intercalation agents. Properties such as tensile property, differential scanning calorimeter (DSC), and thermogravimetric analysis (TGA) were researched and compared. Results showed that the EPU/3% OMMT had the best physical and mechanical properties because of its uniform dispersion of the organic silicate layers. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3578–3585, 2006  相似文献   

3.
The compounds 1,4‐butanediol, succinic anhydride, and nanocellulose (NCC) were used to synthesize poly(butylene succinate)‐grafted Nanocrystalline Cellulose (PBS‐g‐NCC) nanocomposites via polymerization in situ. The resulting structures were examined by transmission electron microscopic (TEM), scanning electron microscope (SEM), 1H and 13C‐nuclear magnetic resonance spectroscopic (NMR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and X‐ray diffraction (XRD) analyses. TEM showed the cellulose to be nanoscale and SEM analysis indicated that 3 wt% NCC dispersed well in PBS matrix. 1H and 13C‐NMR analyses indicated the product to possess peaks characteristic of PBS. DSC analysis clearly showed that the NCC increased the PBS crystallinity when 3 wt% NCC was introduced into PBS matrixes by polymerization in situ, compared to pure PBS. TGA illustrated that the thermal stability of PBS‐g‐NCC was better than that of pure PBS, when 3 wt% NCC was added. XRD analysis suggested that 3 wt% NCC improved PBS crystallinity, which was in good agreement with the present DSC results. POLYM. ENG. SCI., 59:928–934, 2019. © 2018 Society of Plastics Engineers  相似文献   

4.
Polyester‐based polyurethane/nano‐silica composites were obtained via in situ polymerization and investigated by Fourier‐transform infrared spectroscopy (FTIR), or FTIR coupled with attenuated total reflectance (FTIR‐ATR), Transmission electron microscopy (TEM), atomic force microscopy (AFM), an Instron testing machine, dynamic mechanical analysis (DMA) and ultraviolet‐visible spectrophotometry (UV‐vis). FTIR analysis showed that in situ polymerization provoked some chemical reactions between polyester molecules and nano‐silica particles. FTIR‐ATR, TEM and AFM analyses showed that both surface and interface contained nano‐silica particles. Instron testing and DMA data showed that introducing nano‐silica particles into polyurethane enhanced the hardness, glass temperature and adhesion strength of polyurethane to the substrate, but also increased the resin viscosity. UV‐vis spectrophotometry showed that nano‐silica obtained by the fumed method did not shield UV radiation in polyurethane films. Copyright © 2003 Society of Chemical Industry  相似文献   

5.
A novel reactive phosphorus–nitrogen‐containing monomer, N‐(2‐(5,5‐dimethyl‐1,3,2‐dioxaphosphinyl‐2‐ylamino)ethyl)‐acrylamide (DPEAA), was synthesize and characterized. Flame retardant poly(methyl methacrylate)/organic‐modified montmorillonite (PMMA‐DPEAA/OMMT) nanocomposites were prepared by in situ polymerization by incorporating methyl methacrylate, DPEAA, and OMMT. The results from X‐ray diffraction and transmission electron microscopy (TEM) showed that exfoliated PMMA‐DPEAA/OMMT nanocomposites were formed. Thermal stability and flammability properties were investigated by thermogravimetric analysis, cone calorimeter, and limiting oxygen index (LOI) tests. The synergistic effect of DPEAA and montmorillonite improved thermal stability and reduced significantly the flammability [including peak heat release rates (PHRR), total heat release, average mass loss rate, etc.]. The PHRR of PMMA‐DPEAA/OMMT was reduced by about 40% compared with pure PMMA. The LOI value of PMMA‐DPEAA/OMMT reached 27.3%. The morphology and composition of residues generated after cone calorimeter tests were investigated by scanning electronic microscopy (SEM), TEM, and energy dispersive X‐ray (EDX). The SEM and TEM images showed that a compact, dense, and uniform intumescent char was formed for PMMA‐DPEAA/OMMT nanocomposites after combustion. The results of EDX confirmed that the carbon content of the char for PMMA‐DPEAA/OMMT nanocomposites increased obviously by the synergistic effect of DPEAA and montmorillonite. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

6.
Polar polystyrene‐isoprene‐styrene (SIS) copolymers having epoxide groups and long polybutadiene (PB) branches were synthesized via the combination of in situ epoxidation, anionic polymerization and graft‐onto reaction. They were characterized with 1H NMR, GPC, FT‐IR, DSC, and contact angle test. Their polarity was determined by the epoxidation degree and graft efficiency. The epoxidation degree linearly increased with the epoxidation time. The graft efficiency decreased with the branch length, but increased with the epoxidation degrees. Although their glass transition temperature (Tg) of diene blocks and flexibility properties had been negatively affected by in situ epoxidation, they could be modulated by the epoxidation degree, branch length, and branch density. Their Tg could be tailored by the branch length and branch density since they fitted the Fox equation very well, especially as the longer branches were grafted. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40303.  相似文献   

7.
Water‐soluble high intrinsic viscosity organomontmorillonite modified polyacrylate sodium (OMMT‐modified PNaA) was prepared via an in situ intercalation adiabatic polymerization of sodium acrylate in the presence of OMMT. The FTIR and XRD analyses correspond to the OMMT‐modified PNaA with exfoliated structure of OMMT. The influences of prepared conditions on intrinsic viscosity and dissolving time of the modified polymers had been investigated in this study. It was found that the incorporation of as little as 0.1 wt % of OMMT added to PNaA matrix could be effective to enhance intrinsic viscosity of the modified PNaA. TGA and DSC studies confirmed the enhancement of the thermal stability of the OMMT‐modified PNaA when compared with PNaA. Furthermore, the solution behavior studies of the modified PNaA showed the “antipolyelectrolyte” effect and high “antishearing” property. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008  相似文献   

8.
A new silicone containing macromonomer, 4‐(methacrylamido) phenoxy polymethylhydrosiloxane (4‐MPMHS) with a vinyl group, was successfully synthesized. Then poly (silicone‐co‐styrene‐co‐butylacrylate) with montmorillonite, P (Si‐co‐St‐co‐BA) with MMT nanocomposite emulsion was prepared by in situ intercalative emulsion polymerization of styrene (St), butyl acrylate (BA), and 4‐MPMHS, in the presence of organic modified montmorillonite (OMMT) with different OMMT contents (0, 0.5, 1.0, 1.5, and 2 wt %). Potassium persulphate (KPS) was used as an initiator and sodium lauryl sulfoacetate (SLSA) and nonyl phenol ethylene oxide—40 U (NP‐40) were used as anionic and nonionic emulsifiers, respectively. The resulting macromonomer was characterized by elemental analysis, Fourier transformer infrared (FT‐IR), proton (1H NMR), and carbon (13C NMR) nuclear magnetic resonance spectroscopes. The OMMT was characterized by FT‐IR and X‐ray diffraction (XRD). The nanocomposite emulsions were characterized by using Fourier Transform infrared spectroscopy (FT‐IR), laser light scattering, and surface tension method. Thermal properties of the copolymers were studied using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) and then the effects of OMMT percent on the water absorption ratio and drying speed were examined. Results showed that OMMT could improve the properties of emulsion. In other words, the properties of nanocomposite emulsions were better when compared with those of the silicone‐acrylate emulsion. The property of nanocomposite emulsion containing 1 wt % OMMT was the best one, and the following advantages were obtained: smaller particle size, faster drying speed, smaller surface tension, and improved water resistance by the incorporation of OMMT. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

9.
The nylon 6‐based composite materials containing untreated and surface‐treated TiO2 particles with 3‐aminopropyltriethoxysilane (APTEOS), as coupling agent were prepared by in situ anionic polymerization of ε‐caprolactam in the presence TiO2 as a filler using the rotational molding technique. The thermal behavior and mechanical properties of the neat nylon 6 and its composites were investigated using various techniques such as differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), a tensile and flexural test and impact strength. Experimental results revealed that both untreated and surface‐modified TiO2 had distinct influence on the melting temperature (Tm), crystallization temperature (Tc), and degree of crystallinity (αDSC), thermal stability, storage modulus (E′), and loss factor (tan δ), and mechanical properties of nylon 6 matrix. Dynamical mechanical analysis indicated that addition of TiO2 particles into nylon 6 matrix increased both the storage modulus and the glass transition temperature. The corresponding values of nylon 6 composites with modified filler were higher than that of nylon 6 composite with untreated TiO2 particles. Tensile and flexural characteristics of the nylon 6 composites were found to increase while the elongation at break and impact strength with increase in TiO2 concentration relative to neat nylon 6. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers  相似文献   

10.
Although organically modified montmorillonite (OMMT) has been incorporated into unsaturated polyester (UP) resin to enhance properties, the aggregation often leads to defects which directly affect the properties of nanocomposites. In this work, OMMT slurry modified by a new allyl surfactant with carbon–carbon double bond, hexadecyl allyl dimethyl ammonium chloride (C16‐DMAAC), was employed to prepare nanocomposites by in situ polymerization. The results illustrated that the existence of OMMT slurry helped monomers enter the OMMT galleries, leading to well‐dispersed OMMT in the UP matrix. The mechanical properties and thermal properties of OMMT nanocomposites were improved. With OMMT loading of 5 wt %, the tensile strength and flexural strength can be improved by 22% and 38%, respectively. Meanwhile, the onset thermal decomposition temperature (T–10) value was ameliorated from 310.6 °C to 330.6 °C. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45251.  相似文献   

11.
Poly(ethylene terephthalate) (PET)/SiO2 nanocomposites were prepared by in situ polymerization. The dispersion and crystallization behaviors of PET/SiO2 nanocomposites were characterized by means of transmission electron microscope (TEM), differential scanning calorimeter (DSC), and polarizing light microscope (PLM). TEM measurements show that SiO2 nanoparticles were well dispersed in the PET matrix at a size of 10–20 nm. The results of DSC and PLM, such as melt‐crystalline temperature, half‐time of crystallization and crystallization kinetic constant, suggest that SiO2 nanoparticles exhibited strong nucleating effects. It was found that SiO2 nanoparticles could effectively promote the nucleation and crystallization of PET, which may be due to reducing the specific surface free energy for nuclei formation during crystallization and consequently increase the crystallization rate. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 655–662, 2006  相似文献   

12.
In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.  相似文献   

13.
In situ intercalative polymerization for ethylene monomers was carried out to produce PE‐based hybrids through a slurry polymerization method. In this approach, organic solvent for olefin polymerization was found to be one of the most significant factors for the dispersion of the OMMT‐intercalated Et[Ind]2ZrCl2 catalysts, which determines that whether olefin monomers polymerize is in a well‐defined confinement environment or not. Understanding the olefin polymerization occurring in between the nanoscale silicate layers of OMMT as well as the corresponding structure of OMMT in an organic polymerization solvent is a critical step toward tailoring and characterizing nanocomposites formed by OMMT in a polyolefin matrix. As we know, the Et[Ind]2ZrCl2 catalyst and MAO are both better dissolved in toluene than that in hexane because of the larger polarity of toluene. Thus, in hexane the active sites of the OMMT/Et[Ind]2ZrCl2 catalyst exist in the silicate layers of OMMT and the PE chains grow in the middle of them, while in toluene the active specimens are exposed in the gel formed by the OMMT‐intercalated catalyst with MAO, which cause that the PE chains propagated in the mixture liquids. Consequently, when hexane is selected as the polymerization solvent, the formed PE‐based nanocomposites have a good dispersion of OMMT and the nanofiller content (TGA measurement residue at 600°C) is thus higher (>7.0 wt %). However, in toluene, most of the silicate layers of OMMT are agglomerated in the PE matrix. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

14.
From in situ polycondensation, a poly(ethylene terephthalate)/Polyamide 6 copolymer/montmorillonite nanocomposite was prepared, after the treatment of montmorillonite (MMT) with a water soluble polymer. The resulting nanocomposites were characterized by X‐ray diffraction (XRD), differential scanning calorimeter (DSC), nuclear magnetic resonance (NMR), dynamic mechanical analysis (DMA), and transmission electron microscopy (TEM). The results of DSC, 1H NMR, and DMA proved that the nanocomposite synthesized was PET/PA6 copolymer/MMT nanocomposite, not the PET/PA6 blend/MMT nanocomposite. The results of XRD and TEM proved that the dispersion of MMT was improved observably after the introduction of PA6 molecular chain into PET. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2512–2517, 2006  相似文献   

15.
In this study, the structural and morphological properties of poly(methyl methacrylate)/poly(acrylonitrile‐g‐(ethylene‐co‐propylene‐co‐diene‐g‐styrene) (PMMA‐AES) blends were investigated with emphasis on the influence of the in situ polymerization conditions of methyl methacrylate. PMMA‐AES blends were obtained by in situ polymerization, varying the solvent (chloroform or toluene) and polymerization conditions: method A—no stirring and air atmosphere; method B—stirring and N2 atmosphere. The blends were characterized by infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and dynamic mechanical analysis (DMA). The results showed that the PMMA‐AES blends are immiscible and present complex morphologies. This morphology shows an elastomeric dispersed phase in a glassy matrix, with inclusion of the matrix in the elastomer domains, suggesting core shell or salami morphology. The occlusion of the glassy phase within the elastomeric domains can be due to the formation of graft copolymer and/or phase inversion during polymerization. However, this morphology is affected by the polymerization conditions (stirring and air or N2 atmosphere) and by the solvent used. The selective extraction of the blends' components and infrared spectroscopy showed that crosslinked and/or grafting reactions occur on the elastomer chains during MMA polymerization. The glass transition of the elastomer phase is influenced by morphology, crosslinking, and grafting degree and, therefore, Tg depends on the polymerization conditions. On the other hand, the behavior of Tg of the glassy phase with blend composition suggests miscibility or partial miscibility for the SAN phase of AES and PMMA. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

16.
A series of polymer–clay nanocomposite (PCN) materials consisting of 1,4‐bis(4‐aminophenoxy)‐2‐tert‐butylbenzene–4,4′‐oxydiphthalic anhydride (BATB–ODPA) polyimide (PI) and layered montmorillonite (MMT) clay were successfully prepared by an in situ polymerization reaction through thermal imidization up to 300°C. The synthesized PCN materials were subsequently characterized by Fourier‐Transform infrared (FTIR) spectroscopy, wide‐angle powder X‐ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of material composition on thermal stability, mechanical strength, molecular permeability and optical clarity of bulk PI and PCN materials in the form of membranes were studied by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), molecular permeability analysis (GPA) and ultraviolet‐visible (UV/VIS) transmission spectra, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1072–1079, 2004  相似文献   

17.
Butadiene‐isoprene copolymer/montmorillonite (BIR/MMT) nanocomposites were synthesized successfully via in situ anionic polymerization. The results of transmission electron microscopy and X‐ray diffractometer showed that the clay layers were exfoliated and high reaction temperature benefited the exfoliation of layers in BIR/MMT. The polymerization still exhibited “living” characteristics with the addition of organophilic montmorillonite (OMMT). However, the contents of 1,2‐polybutadiene and 3,4‐polyisoprene of the copolymer decreased with the addition of OMMT, because of its absorption effect on N,N,N′,N′‐tetramethylethanediamine as revealed by 1H NMR. Moreover, it was observed that the glass‐transition temperature of the BIR/MMT nanocomposites also decreased when compared with the BIR copolymers. The thermal stability of the nanocomposites was improved, because of the barrier property of exfoliated clay layers. © 2006 Wiley Periodicals, Inc. J Appl PolymSci 102: 1167–1172, 2006  相似文献   

18.
In this article, the surfactants, (2‐hydroxylethyl) octadecyl dimethylammonium nitrate (OH‐C18), hexadecyltrimethylammonium bromide(C16), and mixture of trimethylchlorosilane (TM) and OH‐C18 were ion‐exchanged with cations in the montmorillonite (MMT) to generate three organic MMTs (named as OH‐C18‐MMT, C16‐MMT, and MMMT), leading to different environments of catalyst species in MMT interlayer gallery. Et[Ind]2ZrCl2 (abbreviated as EI) was supported on the above three types of OMMTs to prepare the PE/OMMT nanocomposites via in situ polymerization. By contrast, EI/MMMT showed higher activity than EI/OH‐C18‐MMT and EI/C16‐MMT under the same polymerization conditions. The other two types of catalysts, such as [(tert‐Bu)NSi(Me2)C5Me4]TiCl2 (CGCT) and Bis[N‐(3‐tert‐butylsalicylidene)anilinato] titanium (IV) dichloride (FI) were also supported on the OH‐C18‐MMT for in situ ethylene polymerization. It was found that the activity of FI/OH‐C18‐MMT for ethylene polymerization was much lower than the other two corresponding catalysts under the similar reaction conditions. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

19.
A novel procedure to synthesize in situ clay/nylon‐6 composite suspension was explored via anionic solution polymerization. The suspension was efficiently blended with water‐based epoxy resin using mechanical stirrer at room temperature. Hence, a 3‐component coating system was obtained consisting of nano‐clay, nylon‐6 and epoxy resin. Large number of coatings and films were prepared with variation in clay and nylon‐6 loading. Concentration of clay was found to have profound effect on crystallinity of nylon‐6, thereby affecting the overall properties of clay/nylon/epoxy composite. All the films were characterized for thermal and dynamic mechanical behavior using differential scanning calorimeter (DSC) and dynamic mechanical analysis (DMA). Lower amount of clay was found to increase the crystallinity of nylon‐6 which in turn increased the plasticization of epoxy resin indicated by reduction in Tg. A multiphase morphology with distinct amorphous and crystalline zones was observed under scanning electron microscopy (SEM). A remarkable symmetrical morphology with branched dendritic crystal structure was observed for few of the clay/nylon/epoxy system. POLYM. COMPOS., 37:2206–2217, 2016. © 2015 Society of Plastics Engineers  相似文献   

20.
Mesua ferrea L. seed oil based highly branched polyester resin was modified by methyl methacrylate through grafting polymerization technique. The nanocomposites of this acrylate-modified polyester and 1–5 wt% loadings of organically modified montmorrilonite (OMMT) nanoclay were prepared by an ex situ technique using strong mechanical mixing and ultrasonication. Formation of nanocomposites was confirmed by X-ray diffractometeric (XRD), scanning electron microscopic (SEM) and transmission electron microscopic (TEM) analyses. The absence of d0 0 1 reflections of OMMT in XRD and TEM study revealed the partial exfoliation of OMMT by the polymer chain. The homogeneous surface morphology was also ascertained from SEM. Mechanical and thermal studies of the nanocomposites showed an appreciable improvement in tensile strength and thermal stability by OMMT loading. The enhancement of tensile strength by 2.5 times and thermal stability by 32 °C for 5 wt% OMMT filled nanocomposite was observed compared to that of pristine system. The rheological behavior of the nanocomposites was also investigated and shear thinning was observed. Biodegradation of the nanocomposite films was assayed using two strains of Pseudomonas aeruginosa, SD2 and SD3 and one strain of Bacillus subtilis, MTCC736. The nanocomposites exhibited enhanced biodegradability as compared to pristine acrylate modified polyester. All the results showed the potentiality of the nanocomposites as advanced thin film materials for suitable applications.  相似文献   

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