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1.
Frying oils were studied by Fourier-transform infrared (FT-IR) spectroscopy, in the range 4,000–200 cm?1, at different temperatures, in the liquid and solid states. The infrared spectrum at 15 °C was similar to that at 200 °C. The band at 730 cm?1 which was assigned to the rocking mode of (–CH2) disappeared at higher temperature because of the rotational isomerism which occurred in the oil structure. The activation energy (E a) of the disappearing (–CH2) band, calculated by use of the chemical dynamic method using the Arrhenius equation, is 8.45 kJ mol?1. The enthalpy difference (ΔH) between the two rotational isomer bands of the conformational structures of the oil at 730 and 1,790 cm?1, at different high temperatures, was also calculated, by use of the Van’t Hoff equation; the value obtained was ?10.85 kJ mol?1.  相似文献   

2.
《Analytical letters》2012,45(16):2597-2609
A multistep infrared macro-fingerprint method was applied to identify two Chinese herbal drugs, Rhizoma Curcumas Longae (RCL) and Radix Curcumae (RC). Fourier transform infrared (FT-IR) spectra of the two were similar to each other and consistent with the 11 peaks of the spectrum of starch. RCL had a characteristic absorption peak at approximately 1514 cm?1 that correlated to the strong peak near 1509 cm?1 of curcumin. Between 900 cm?1–1700 cm?1 of the second derivative infrared (SD-IR) spectra, with higher resolution, RCL, and curcumin had 10 common peaks. In the FT-IR and SD-IR spectra of the ethanol extract, the spectra of the RCL extract and curcumin were similar, but RC was different. According to the fingerprint characteristics of the infrared spectra for RC and its extracts, the strongest peak at 1055 cm?1; the C-O absorption peaks at 1124 cm?1, 1106 cm?1, and 996 cm?1; and the strong methylene peaks at 2925 cm?1 and 2853 cm?1 suggest that RC contains more saccharides. In the range of 1350 cm?1–1700 cm?1, RCL and RC had similar two-dimensional infrared (2D-IR) correlation spectra. Both of them had three autopeaks, but the autopeaks were located at 1458 cm?1, 1560 cm?1, and 1641 cm?1 for RCL and 1458 cm?1, 1560 cm?1, and 1669 cm?1 for RC, suggested that the aromatic components of the two were not identical. The average correlation for the 18 RCL and 18 RC samples were 0.9906 and 0.9878, respectively, and this method achieves a good classification of the sample type.  相似文献   

3.
This work presents thermal studies of nanocomposites based on the flexible polyurethane (PU) matrix and filled using montmorillonite organically modified with organophosphorus flame retardant compound. Flexible PU nanocomposite foams were prepared in the reaction carried out between reactive alcoholic hydroxyl and isocyanate groups with the ratio of NCO to OH groups equal to 1.05. The amount of an organoclay ranging from 3 to 9 vol% was added to the polyol component of the resin before mixing with isocyanate. The apparent density of PU foams was ranging from 0.066 to 0.077 g cm?1. Thermal properties of the flexible PU nanocomposite foams were investigated by thermogravimetry and dynamical mechanical analysis. Glass transition temperatures (T g) were defined as maximum peak on tanδ curve. Thermal decomposition was observed at 310–320 °C (calculated from the onset of TG curve). Tensile strength of the PU foams was determined using mechanical test. The microstructure of the nanoparticles and the composites was investigated by X-ray diffraction. Finally, it was confirmed that the thermal and mechanical properties of flexible PU nanocomposite depend on the amount of nanoclay.  相似文献   

4.
《Analytical letters》2012,45(18):2909-2918
The fermentation of xylitol is a promising alternative to conventional chemical processes. Micro-Raman spectroscopy was used to monitor the process involving Candida tropicalis, including the medium and yeast cells during xylitol fermentation. The spectra of the fermentation medium showed that the characteristic xylitol peak at 866 cm?1 was enhanced from 18 h and that the characteristic xylose peak at 901 cm?1 gradually diminished as the reaction progressed. The characteristic ethanol peak at 880 cm?1 indicated the production of by-products. Intracellular biological macromolecules, such as nucleic acids, proteins, lipids, and carbohydrates, were identified in the spectra of yeast cells. The intensity of nucleic acids at 783 cm?1 reached the highest value after 3 h. The xylose band at 901 cm?1 and the peaks in the carbohydrate region reached a maximum in the logarithmic phase, indicating the carbohydrate metabolism was the most active. The amide I band located at 1658 cm?1 indicated the major secondary structure of proteins was α-helix; its intensity gradually reduced during the fermentation. The 853 cm?1 band due to buried tyrosine was predominant at 21 h. In addition, the 1275 cm?1 band corresponded to the presence of a random coil only at 27 h. These results provided a perspective to understand fermentation and verified the applicability of Raman spectroscopy in xylitol fermentation.  相似文献   

5.
In the present work effect of 90 MeV O7+ ions with five different fluences on poly(ethylene oxide) (PEO)/Na+-montmorillonite (MMT) nanocomposites has been investigated. PEO/MMT nanocomposites were synthesized by solution intercalation technique. With the increase in irradiation fluence, gallery spacing of MMT increases in the composite and an exfoliated nanostructure is obtained at the fluence of 5?×?1012 ions/cm2 as revealed by X-ray diffraction results. Highest room temperature ionic conductivity of 4.2?×?10?6?S?cm?1 was found for the fluence 5?×?1012 ions/cm2, while the conductivity for unirradiated polymer electrolyte was found to be 7.5?×?10-8?S?cm?1. The increase in intercalation of PEO chains inside the galleries of MMT results in the increase in interaction between Na+ cation and oxygen heteroatom leading to the increase in ionic conductivity of the composites. Surface morphology and interactions among the various constituents in the nanocomposites at different fluence have been examined by scanning electron microscopy and Fourier transform infrared spectroscopy, respectively. The appearance of peak for each fluence in the loss tangent suggests the presence of relaxing dipoles in the polymer nanocomposite electrolyte films. With the increase in ion fluence the peak shifts towards higher frequency side, suggesting decrease in the relaxation time.  相似文献   

6.
A series of novel type bisphthalonitriles with different molecular weight main-chain polybenzoxazines as linkages have been successfully synthesized using 4, 4′-diaminodiphenyl methane, paraformaldehyde, bisphenol A and 4-nitrophthalonitrile as initial materials. The structures were characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance (1H-NMR). The formation of benzoxazine and the existence of nitrile groups were confirmed by the absorbance at 950cm?1 of benzene attached with oxazine ring and 2231 cm?1 of nitrile groups. The characteristic resonance peaks observed at about 4.52 (C-CH2-N) and 5.28 ppm (N-CH2-O) also determined the structure of benzoxazine ring. The curing behaviors were monitored by differential scanning calorimetry (DSC) and FT-IR. Two-stage polymerization mechanisms were observed according to the ring-opening of benzoxazine and the polymerization of nitrile groups catalyzed by phenolic hydroxyl groups, which generated during the curing reaction of benzoxazine. The polymerization of these bisphthalonitriles exhibited self-promoted curing behaviors. The completion of polymerization was proved by the disappearance of the band located at 950 cm?1 in FT-IR. Thermogravimetric analysis (TGA) was used to investigate the thermal stability, and the results showed that the cured polymers achieved extremely high char yield from 61.1% up to 74.2% at 800°C under nitrogen and exhibited increasing decomposition temperature as the contents of phthalonitrile groups increased, which indicated that the polymerization of phthalonitriles could improve the thermal stability.  相似文献   

7.
Rigid polyurethane (PU) foams having saccharide and castor oil structures in the molecular chain were prepared by reaction between reactive alcoholic hydroxyl group and isocyanate. The apparent density of PU foams was in a range from 0.05 to 0.15 g cm?3. Thermal properties of the above polyurethane foams were studied by differential scanning calorimetry, thermogravimetry and thermal conductivity measurement. Glass transitions were observed in two steps. The low-temperature side glass transition was observed at around 220 K, regardless of castor oil content. This transition is attributed to the molecular motion of alkyl chain groups of castor oil. The high-temperature side glass transition observed in the temperature range from 350 to 390 K depends on the amount of molasses polyol content. The high-temperature side glass transition is attributed to the molecular motion of saccharides, such as sucrose, glucose, fructose as well as isocyanate phenyl rings, which act as rigid components. Thermal decomposition was observed in two steps at 570 and 620–670 K. Thermal conductivity was observed at around 0.032 J sec?1 m?1 K?1. Compression strength and modulus of PU foams were obtained by mechanical test. It was confirmed that the thermal and mechanical properties of PU foams could be controlled by changing the mixing ratio of castor oil and molasses for suitable practical applications.  相似文献   

8.
Vapor-grown carbon nanofiber (CNF)-modified soy polyol-based polyurethane (PU) nanocomposites with different hydroxyl value of polyols (OH) were synthesized. The glass transition, thermal stability, mechanical properties, and morphology of the PU nanocomposites were characterized through differential scanning calorimetry, thermogravimetry, universal test machine, and scanning electron microscopy. The addition of CNFs increased the glass transition temperature as well as significantly improved tensile strength and Young’s modulus of PU nanocomposites. Meanwhile, thermal and mechanical properties of PU composites were influenced by the different hydroxyl value of polyols due to those different structures. In particular, in the case of 2 mass% CNF addition in PU derived from soy polyol with the OH number of 164 mg KOH g?1, 20.8 °C improvement in the glass transition temperature, 115 % increment in tensile strength, and nearly eightfold increase in Young’s modulus were obtained.  相似文献   

9.
Maize is one of the important cereal crops grown in India and is accompanied by enormous amount of agro wastes generation. About 30 % of this agro waste is corn cobs. In this study, cellulose is extracted from corn cobic agro waste. Three samples of methylcellulose were synthesized employing three different solvent conditions which are (a) solvent free, (b) using toluene, and (c) using acetone. The methylcelluloses, thus produced, were characterized by FT-IR, NMR, DSC, TG, and XRD techniques. The determination of the methoxyl group content was made through the modified procedure of Viebock and Schwappach. The product properties were differentiated by thermal analysis and XRD. The ratio between the absorption intensities of the C–H stretching band at around 2,900 cm?1 and O–H stretching band at around 3,400 cm?1 was observed to evaluate the degree of substitution also. The DS values were found in the order of 0.82, 0.95, and 1.14 for solvent free, toluene, and acetone solvent conditions, respectively.  相似文献   

10.
A recent study on the Raman spectrum of the cysteine zwitterion and anion, and the 2:1 (Cys)2Zn complex was reanalyzed employing B3LYP/6-311++G(3df,2pd) calculations in a simulated water environment. The spectra were rediscussed in light of the apparent incorrect structure determined in the original paper for this complex. The complex turns out to be tetrahedral and tetracoordinated instead of octahedral hexacoordinated, as initially proposed. The calculated Raman spectrum of the complex agrees very well with the experimental data, showing that both the geometrical and electronic structures are well represented. Three metal–ligand bands are found, two of them involving mostly the symmetrical and asymmetrical stretching of the Zn–N and Zn–S bonds. They were measured at 334 and 296 cm?1 and calculated at 319 and 249 cm?1, respectively. The third band involves the stretching of Zn–S bonds but also skeletal vibrations of the ligand. This band, measured at 399 cm?1 and calculated at 444 cm?1, has been previously assigned incorrectly to a Zn–O bond which does not actually exists since the CO 2 ?1 fragments are located away from the Zn ion.  相似文献   

11.
Mesoporous carbon nitride (MCN-1) and functionalized MCN-1 with melamine-based dendrimer amine (MDA-MCN-1) have been synthesized. These materials are characterized by means of nitrogen adsorption–desorption isotherms, thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) spectroscopy, small-angle X-ray scattering (SAXS), wide angle X-ray diffraction (XRD) pattern and Energy dispersive X-ray (EDX). Two bands at 1,434 and 1,550 cm?1 in FT-IR spectrum of MDA-MCN-1 are clear evidence of an aromatic triazine ring and confirm that the melamine-based dendrimer is formed. The pore diameter is centered at 4.74 nm with a relatively high BET surface area of 102.2 m2 g?1 and a pore volume of 0.12 cm3 g?1. TGA curves show that samples (MCN-1 and MDA-MCN-1) have high thermal stability compared to the earlier species. The carbon-to-nitrogen ratio calculated from the EDX analysis significantly decreases from 3.87–4.35 to 1.26 in MDA-MCN-1 than MCN-1 material. This indicates that MDA-MCN-1 has high nitrogen content and active adsorption sites in comparison to MCN-1 species.  相似文献   

12.
ZnO nanoparticles (NPs) with tunable morphologies were synthesized by a hybrid electrochemical–thermal method at different calcination temperatures without the use of any surfactant or template. The NPs were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction, dynamic light scattering, thermogravimetry–differential thermal analysis, scanning electron microscope and N2 gas adsorption–desorption studies. The FT-IR spectra of ZnO NPs showed a band at 450 cm?1, a characteristic of ZnO, which remained fairly unchanged at calcination temperatures even above 300 °C, indicating complete conversion of the precursor to ZnO. The products were thermally stable above 300 °C. The ZnO NPs were present in a hexagonal wurtzite phase and the crystallinity of ZnO increased with an increasing calcination temperature. The ZnO NPs calcined at lower temperature were mesoporous in nature. The surface areas of ZnO NPs calcined at 300 and 400 °C were 51.10 and 40.60 m2 g?1, respectively, which are significantly larger than commercial ZnO nanopowder. Surface diffusion has been found to be the key mechanism of sintering during heating from 300 to 700 °C with the activation energy of sintering as 8.33 kJ mol?1. The photocatalytic activity of ZnO NPs calcined at different temperatures evaluated by photocatalytic degradation of methylene blue under sunlight showed strong dependence on the surface area of ZnO NPs. The ZnO NPs with high surface area showed enhanced photocatalytic activity.  相似文献   

13.
In this work, at first alkylferrocene derivatives were synthesized according to procedure described in the literature. (5-Chloropentanoyl)ferrocene derivatives were prepared by Friedel–Crafts acylation of ferrocene and alkylferrocene derivatives with 5-chloropentanoyl chloride in dichloromethane, and AlCl3 was used as catalyst. The corresponding 5-chloropentylferrocene derivatives were synthesized from reduction of these products by NaBH4 in diglyme at 0 °C. Finally (5-alkylferrocenylpentyl)dimethylsilane was synthesized from reaction of 5-chloropentylferrocene derivatives with magnesium in THF and reaction of corresponding Grignard reagents with chlorodimethylsilane in 82–87% yields. 1H and 13C NMR, FT-IR spectroscopy supported the predicted structure of the product. Nine samples of alkylferrocene-grafted hydroxyl-terminated polybutadiene (alkylFc-HTPB) derivatives, containing different percent of iron, were synthesized by hydrosilylation reaction of [5-(alkylferrocenyl)pentyl]dimethylsilane with hydroxy-terminated polybutadiene (HTPB), in the presence of catalytic amount of the hexachloroplatinic acid (Speier’s catalyst). FT-IR spectroscopy was utilized to follow the progress of the reaction, by monitoring the loss of the Si–H absorption at 2110 cm?1, and the reaction was completed in 24 h. Some properties of resulting prepolymer like viscosity, glass transition temperature and iron percentage as important parameters in production of composite propellants were investigated. For example, the viscosity increased with increasing iron content because of the greater extent of ferrocene grafting in the polymer.  相似文献   

14.
Au/graphene nanocomposites are prepared via a one-pot chemical reduction process at room temperature, using graphene oxide (GO) and chloroauric acid (HAuCl4) as precursors. The obtained Au/graphene nanocomposites are characterized with scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). TEM shows that the Au nanoparticles with size of approximately 8.7 nm disperse randomly on the surface of graphene. XPS confirms that the Au/graphene nanocomposites show a higher atomic percentage of C/O (6.3/1), in contrast to its precursor GO (2.2/1). Electrochemical studies reveal that the Au/graphene nanocomposites have electrochemically active surface area of 9.82 m2 g?1. Besides, the influence of borohydride concentration on the as-prepared Au/graphene nanocomposites is investigated in details by cyclic voltammetry, chronoamperometry, and chronopotentiometry. The results indicate that high concentration of borohydride can significantly improve the electrochemical performance of the Au/graphene catalyst.  相似文献   

15.
FTIR spectra of blends of lightly sulfonated polystyrene (PS-SSA) with polyurethanes (PU) containing a tertiary nitrogen in the chain extender were recorded. These blends exhibit a two-phase behavior, but the individual components are not phase separated. Earlier dynamic mechanical studies suggested the occurrence of proton transfer from the sulfonic acid to the tertiary nitrogen, which enhanced the miscibility via ionic interactions and resulted in the formation of a miscible blend between the PS-SSA and the hard segment of the PU, the soft segment being excluded. FTIR studies of these blends now confirm the proton transfer mechanism. A new absorption band at 3428 cm?1 corresponds to a stretching vibration of an N+?H bond. The 1012 cm?1 band of the SO3H group, which strongly depends on the degree of protonation, shifts to lower frequency. The symmetric stretching vibration of the SO group, which occurred at 1043 cm?1, shifts to lower frequency as well, suggesting a lower polarization of the S? O dipole due to the removal of H+.  相似文献   

16.
Polyester (HTPS) based polyurethane (PU) elastomers were currently established to be effective binders for high-energy composites with improved performances. Conventional PU binders are mostly non-energetic materials, and consequently reduce the energy performance significantly. Nitrocellulose (NC), is an energetic polymer widely used as an ingredient in propellants, explosives, fireworks, and gas generators, it may be introduced in PU-based compositions to overcome their performance drawback. Kinetic parameters must be specified in order to build PU binders with the most convenient and appropriate features. Therefore, the cure kinetics of polyester based polyurethane binder systems were investigated by Fourier transform infrared spectroscopy (FT-IR) isothermal method. The polyester prepolymer (Desmophen® 1200) was cured with hexamethylene diisocyanate (HDI: Desmodur® N100) at various molar ratios (R[NCO]/[OH] = 0.6, 1, 1.25, and 1.5) and under different isothermal conditions (T = 60°C, 80°C, 100°C, and 120°C). In addition, the effect of the addition of nitrocellulose on the kinetics of polymerization of PU was investigated. The progression of the reaction was followed based on the decrease of the peak intensity of –NCO group at 2271 cm−1 as a function of the reaction time. The curing kinetic model and the apparent activation energy (Eα) were determined by the use of Kamal autocatalytic model and Friedman isoconversional method, respectively.  相似文献   

17.
SnO2/graphene nanocomposites are synthesized by a new hydrothermal treatment strategy under the assistance of sucrose. From the images of the scanning electron microscope (SEM) and transmission electron microscope (TEM), it can be observed that SnO2 nanoparticles with the size of 4~5 nm uniformly distribute on the graphene nanosheets. The result demonstrates that sucrose can effectively prevent graphene nanosheets from restacking during hydrothermal treatment and subsequently treatment. The charging/discharging test result indicates that the SnO2/graphene nanocomposites exhibit high specific capacity and excellent cycleability. The first reversible specific capacity is 729 mAh.g?1 at the current density of 50 mA.g?1, and remains 646 mAh.g?1 after 30 cycles at the current density of 100 mA.g?1, 30 cycles at the current density of 200 mA.g?1, 30 cycles at the current density of 400 mA.g?1, 30 cycles at the current density of 800 mA.g?1, and 30 cycles at the current density of 50 mA.g?1.  相似文献   

18.
The SnO/SnO2 nanocomposites were synthesized using semisolvothermal reaction technique. These nanocomposites were prepared using different combination of solvents viz., ethanol, water, and ethylene glycol at 180 °C for 24 h. The synthesized nanocomposites were analyzed with various characterization techniques. Structural analysis indicates the formation of tetragonal phase of SnO2 for the sample prepared in ethanol, whereas for other solvent combinations, the mixture of SnO and SnO2 having tetragonal crystal structures were observed. The optical study shows enhanced absorbance in the visible region for all the prepared SnO/SnO2 nanocomposites. The observed band gap was found to be in the range of 3.0 to 3.25 eV. Microstructural determinations confirm the formation of nanostructures having spherical as well as rod-like morphology. The size of nanoparticles in ethanol-mediated solvent was found to be in the range of 5 to 7 nm. Thermogravimetric analysis indicate the weight gain around 1.3 wt% confirming the conversion of SnO to SnO2 material. The photocatalytic activity of synthesized nanocomposites was evaluated by following the aqueous methylene blue (MB) degradation. The sample prepared in ethylene glycol-mediated solvent showed highest photoactivity having apparent rate constant (Kapp) 0.62 × 10?2 min?1.  相似文献   

19.
The electrochemical properties of anthraquinone monosulfonate (AQS) adsorbed on the basal plane of chemically-reduced graphene oxide (RGO) by π–π stacking interaction were investigated. The AQS/RGO nanocomposites were synthesized via a simple reduction–adsorption method and characterized with various techniques, and the surface concentration of AQS on the basal plane of RGO was estimated to be 1.72?×?10?12 mol cm?2. Electrochemical tests showed that the AQS/RGO nanocomposites accelerated the heterogeneous electron transfer, when ferro/ferricyanide was used as a redox probe, and RGO facilitated the electron transfer between AQS and the surface of glassy carbon electrode, producing a well-defined redox couple centered at ?0.490 V versus SCE at neutral medium. Compared with AQS and RGO modified glassy carbon (GC) electrode, the AQS/RGO nanocomposites showed better electrocatalytic activity towards oxygen reduction reaction. Rotating disk electrode data showed that the reduction of O2 on AQS/RGO/GC electrode underwent a two-electron process to H2O2 at low overpotential and shifted to four-electron reduction to H2O at relatively high overpotential. The present work demonstrates that AQS can be an efficient catalyst when noncovalently functionalized on the basal plane of RGO for electrochemical applications.  相似文献   

20.
In the present work, a set of polyaniline–graphene oxide (PANI–GO) nanocomposites which exhibit superior properties in terms of shelf life, processability and conductivity due to the synergistic effect of GO and PANI, have been synthesized by varying the concentration of highly non-conducting GO with respect to aniline. The obtained materials were characterized by UV–Vis, FTIR, XRD, Raman, TGA as well as FESEM, TEM analysis. The results reveal that nanocomposites show better dispersibility, crystallinity, thermal stability, and conductivity. Further, the synthesized composites have been tested for their anti-corrosion properties. The potentiodynamic results reveal that PANI nanocomposites with 1% GO exhibited long-term anti-corrosion behavior with a corrosion rate of 6.5 × 10?5 mm year?1, which is much lower than its individual components and commercial-grade red oxide. Also, it possesses highest impedance modulus ~33 kΩ cm2 and real impedance ~32 kΩ cm2, maximum coating resistance ~14.81 × 103 Ω cm2 and minimum coating capacitance after 96 h of immersion in 3.5% mass NaCl than those exhibited by all other coated samples. Higher concentration of GO could not retard the corrosion rate confirming that hydrophilicity of GO play an important role in the redox mechanism of PANI.  相似文献   

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