scholarly journals Preparation and Characterization of Hydrophobically Grafted Starches by In Situ Solid Phase Polymerization

Polymers ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 72 ◽  
Author(s):  
Yingfeng Zuo ◽  
Xiaoyu He ◽  
Ping Li ◽  
Wenhao Li ◽  
Yiqiang Wu
Keyword(s):  
Molecular Weight ◽  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Graft Polymer ◽  
X Ray ◽  
Grafting Reaction ◽  
Grafting Ratio ◽  
Ft Ir

Three kinds of hydrophobic groups grafted starches of maleic anhydride grafted starch (MAH-g-starch), lactic acid grafted starch (LA-g-starch), and methyl acrylate grafted starch (MA-g-starch) were prepared by in situ solid phase polymerization. The results of Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) confirmed successful grafting. The grafting ratios of MAH-g-starch, LA-g-starch, and MA-g-starch were 6.50%, 12.45%, and 0.57%, respectively. Influenced by the grafting ratio, LA-g-starch had the best relative hydrophobicity and the largest molecular weight, and those for MA-g-starch were the worst. The surfaces of grafted starches were covered with graft polymer, with obvious surface roughness and bond degree of MAH-g-starch and LA-g-starch. The crystalline structure of grafted starches showed some damage, with LA-g-starch exhibiting the greatest decrease in crystallinity, and less of a change for MA-g-starch. Overall, the grafting reaction improved thermoplasticity, with LA-g-starch the most improved, followed by MAH-g-starch, and then MA-g-starch.

scholarly journals Preparation and Characterization of Hydrophobic Groups Grafted Starches by In-Situ Solid Phase Polymerization

2018 ◽  
Author(s):  
Yinfeng Zuo ◽  
Xiaoyu He ◽  
Ping Li ◽  
Wenhao Li ◽  
Yiqiang Wu
Keyword(s):  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Graft Polymer ◽  
Hydrophobic Properties ◽  
X Ray ◽  
Grafting Reaction ◽  
Grafting Ratio ◽  
Ft Ir

Three kinds of hydrophobic groups grafted starches of maleic anhydride grafted starch (MAH-g-starch), lactic acid grafted starch (LA-g-starch), and methyl acrylate grafted starch (MA-g-starch) were prepared by in-situ solid phase polymerization. The results of Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) were confirmed successful grafting. The grafting ratios of MAH-g-starch, LA-g-starch and MA-g-starch were 6.50%, 12.45%, and 0.57%, respectively. Influenced by the grafting ratio, LA-g-starch had the best hydrophobic properties and the largest molecular weight, and those for MA-g-starch was the worst. The surfaces of grafted starches were covered with graft polymer, with obvious surface roughness and bond degree of MAH-g-starch and LA-g-starch. The crystalline structure of grafted starches showed some damage, with LA-g-starch exhibiting the greatest decrease in crystallinity, and less of a change for MA-g-starch. Overall, the grafting reaction improved thermoplasticity, with LA-g-starch the most improved, followed by MAH-g-starch, and then MA-g-starch.

scholarly journals Hydrogenative Cyclization of Levulinic Acid to γ-Valerolactone with Methanol and Ni-Fe Bimetallic Catalysts

Catalysts ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1096
Author(s):  
Ligang Luo ◽  
Xiao Han ◽  
Qin Zeng
Keyword(s):  
Photoelectron Spectroscopy ◽  
Levulinic Acid ◽  
Hydrogen Donor ◽  
Effect Of Temperature ◽  
X Ray ◽  
Transmission Electron ◽  
Ft Ir ◽  
Temperature Programmed

A series of Ni-Fe/SBA-15 catalysts was prepared and tested for the catalytic hydrogenation of levulinic acid to γ-valerolactone, adopting methanol as the only hydrogen donor, and investigating the synergism between Fe and Ni, both supported on SBA-15, towards this reaction. The characterization of the synthesized catalysts was carried out by XRD (X-ray powder diffraction), TEM (transmission electron microscopy), H2-TPD (hydrogen temperature-programmed desorption), XPS (X-ray photoelectron spectroscopy), and in situ FT-IR (Fourier transform–infrared spectroscopy) techniques. H2-TPD and XPS results have shown that electron transfer occurs from Fe to Ni, which is helpful both for the activation of the C=O bond and for the dissociative activation of H2 molecules, also in agreement with the results of the in situ FT-IR spectroscopy. The effect of temperature and reaction time on γ-valerolactone production was also investigated, identifying the best reaction conditions at 200 °C and 180 min, allowing for the complete conversion of levulinic acid and the complete selectivity to γ-valerolactone. Moreover, methanol was identified as an efficient hydrogen donor, if used in combination with the Ni-Fe/SBA-15 catalyst. The obtained results are promising, especially if compared with those obtained with the traditional and more expensive molecular hydrogen and noble-based catalysts.

scholarly journals Characterization of Ti/SnO2 Interface by X-ray Photoelectron Spectroscopy

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 202
Author(s):  
Miranda Martinez ◽  
Anil R. Chourasia
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Chemical Interaction ◽  
Photoelectron Spectra ◽  
X Ray ◽  
Increasing Trend ◽  
Substrate Temperatures ◽  
Beam Technique

The Ti/SnO2 interface has been investigated in situ via the technique of x-ray photoelectron spectroscopy. Thin films (in the range from 0.3 to 1.1 nm) of titanium were deposited on SnO2 substrates via the e-beam technique. The deposition was carried out at two different substrate temperatures, namely room temperature and 200 °C. The photoelectron spectra of tin and titanium in the samples were found to exhibit significant differences upon comparison with the corresponding elemental and the oxide spectra. These changes result from chemical interaction between SnO2 and the titanium overlayer at the interface. The SnO2 was observed to be reduced to elemental tin while the titanium overlayer was observed to become oxidized. Complete reduction of SnO2 to elemental tin did not occur even for the lowest thickness of the titanium overlayer. The interfaces in both the types of the samples were observed to consist of elemental Sn, SnO2, elemental titanium, TiO2, and Ti-suboxide. The relative percentages of the constituents at the interface have been estimated by curve fitting the spectral data with the corresponding elemental and the oxide spectra. In the 200 °C samples, thermal diffusion of the titanium overlayer was observed. This resulted in the complete oxidation of the titanium overlayer to TiO2 upto a thickness of 0.9 nm of the overlayer. Elemental titanium resulting from the unreacted overlayer was observed to be more in the room temperature samples. The room temperature samples showed variation around 20% for the Ti-suboxide while an increasing trend was observed in the 200 °C samples.

Study on the Synthesis and Characterization of PANi/Nano-CeO2 Composites

2007 ◽  
Vol 124-126 ◽  
pp. 287-290 ◽  
Author(s):  
Fei Liu ◽  
Yong Jun He ◽  
Jeung Soo Huh
Keyword(s):  
In Situ Polymerization ◽  
Solid Phase ◽  
Polymerization Reaction ◽  
Solid Phase Reaction ◽  
Phase Reaction ◽  
Vis Spectroscopy ◽  
Ft Ir ◽  
Average Size

The nano-CeO2 was synthesized by two-step solid-phase reaction. The image of TEM showed that nano-CeO2 with an average size of about 70 nm. The series of polyaniline/nano-CeO2 composites with different PANi: CeO2 ratios were prepared by in-situ polymerization in the presence of hydrochloric acid (HCl) as dopant by adding nano-CeO2 into the polymerization reaction mixture of aniline. The composites obtained were characterized by FT-IR and UV-vis spectroscopy analysis. The FT-IR spectra of nanocomposites indicate different blue-shifts, attributed to C–N stretching mode for benzenoid unit. The UV-vis spectra of nanocomposites display einstein-shifts compared with PANi at 620nm. The conductivity properties of the composites are also changed compare to the pure PANi. These results suggest that the interactions between the polymer matrix and nanoparticles take place in polyaniline/nano- CeO2 composites.

Synthesis and characterization of the solid uranium(VI) dioxo-diacetohydroxamate complex

2007 ◽  
Vol 95 (8) ◽  
Author(s):  
Cynthia-May S. Gong ◽  
Frédéric Poineau ◽  
Kenneth R. Czerwinski
Keyword(s):  
Solid Phase ◽  
Uranyl Acetate ◽  
Proton Nuclear Magnetic Resonance ◽  
Acetohydroxamic Acid ◽  
Acetate Dihydrate ◽  
Reaction Conditions ◽  
X Ray ◽  
Ft Ir ◽  
X Ray Absorption

A novel dry synthesis for the uranium(VI) dioxo-diacetohydroxamate (UAHA) complex has been developed. The complex was generated in >80% yield by mechanically grinding solid uranyl acetate dihydrate (UAc) with solid acetohydroxamic acid in stoichiometric amounts. The resulting UOThe UAHA solid was extensively characterized by ultraviolet-visible (UV-vis), Fourier-transform infrared (FT-IR), and extended X-ray absorption fine structure (EXAFS) spectroscopies. The compound did not fluoresce after laser excitation. Proton nuclear magnetic resonance (NMR) spectra were obtained of the complex in DThe easy synthesis and purification of UAHA enables researchers to strictly control reaction conditions; to eliminate interfering salts and water; and to study the complex in the solid-phase.

scholarly journals “PdO vs. PtO”—The Influence of PGM Oxide Promotion of Co3O4 Spinel on Direct NO Decomposition Activity

Catalysts ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 62 ◽  
Author(s):  
Gunugunuri K. Reddy ◽  
Torin C. Peck ◽  
Charles A. Roberts
Keyword(s):  
Photoelectron Spectroscopy ◽  
No Decomposition ◽  
Single Element ◽  
X Ray Diffraction ◽  
X Ray ◽  
Promotional Effect ◽  
Ft Ir ◽  
Temperature Programmed ◽  
Thermal Stability Of

Direct decomposition of NO into N2 and O2 (2NO→N2 + O2) is recognized as the “ideal” reaction for NOx removal because it needs no reductant. It was reported that the spinel Co3O4 is one of the most active single-element oxide catalysts for NO decomposition at higher reaction temperatures, however, activity remains low below 650 °C. The present study aims to investigate new promoters for Co3O4, specifically PdO vs. PtO. Interestingly, the PdO promoter effect on Co3O4 was much greater than the PtO effect, yielding a 4 times higher activity for direct NO decomposition at 650 °C. Also, Co3O4 catalysts with the PdO promoter exhibit higher selectivity to N2 compared to PtO/Co3O4 catalysts. Several characterization measurements, including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), H2-temperature programmed reduction (H2-TPR), and in situ FT-IR, were performed to understand the effect of PdO vs. PtO on the properties of Co3O4. Structural and surface analysis measurements show that impregnation of PdO on Co3O4 leads to a greater ease of reduction of the catalysts and an increased thermal stability of surface adsorbed NOx species, which contribute to promotion of direct NO decomposition activity. In contrast, rather than remaining solely as a surface species, PtO enters the Co3O4 structure, and it promotes neither redox properties nor NO adsorption properties of Co3O4, resulting in a diminished promotional effect compared to PdO.

Structural Characterization of Ion Beam Enhanced Solid Phase Epitaxial Regrowth by Raman, RBS, and X-Ray Analysis

1988 ◽  
Vol 126 ◽  
Author(s):  
John F. Knudsen ◽  
R. C. Bowman ◽  
P. M. Adams ◽  
R. Newman ◽  
J. P. Hurrell ◽  
...  
Keyword(s):  
Solid Phase ◽  
Ion Beam ◽  
Beam Current ◽  
Crystalline Quality ◽  
X Ray Diffraction ◽  
X Ray ◽  
Epitaxial Regrowth ◽  
High Beam Current

ABSTRACTEpitaxial regrowth of deposited amorphous silicon has been previously described utilizing ion implantation amorphization, ion mixing and thermal anneal. This paper evaluates the effects of these process steps on crystalline quality utilizing Rutherford Backscattering (RBS), x-ray diffraction rocking curves and Raman scattering.In situ (during implantation) regrowth results in defective crystallinity. In contrast, when there is no in situ regrowth, the post anneal crystallinity is equivalent by RBS and x-ray evaluation to virgin single crystal wafers. In situ regrowth is most pronounced during the high beam current ion mixing type implants which produce wafer temperatures of about 250°C. The final crystalline quality which results from different sequences of amorphization and ion mixing implants, is strongly dependent upon the amount of in situ regrowth which has occurred. The greater the in situ regrowth the poorer the final crystalline quality.

Spectroscopic Characterization of Wilkinson's Catalyst Using X-ray Photoelectron Spectroscopy (ESCA)

1982 ◽  
Vol 36 (3) ◽  
pp. 290-296 ◽  
Author(s):  
Manuel Carvalho ◽  
Larry F. Wieserman ◽  
David M. Hercules
Keyword(s):  
Binding Energy ◽  
Photoelectron Spectroscopy ◽  
Analytical Techniques ◽  
Spectroscopic Characterization ◽  
Homogeneous Hydrogenation ◽  
X Ray ◽  
Wilkinson’S Catalyst ◽  
Ft Ir ◽  
Wilkinson's Catalyst

Wilkinson's catalyst, RhCl(PPh3)3 is a well known and widely used homogeneous hydrogenation catalyst. This catalyst was analyzed by ESCA which revealed that two rhodium species [Rh(I) and Rh(III)] were present, both for commercial preparations and for catalysts prepared in this laboratory. The ratio of Rh(I) to Rh(III) was 3:2 regardless of the source. A different method of synthesizing RhCl(PPh3)3 was used and produced a compound having only Rh(I) species. Additional analytical techniques such as elemental analysis, FT-IR, liquid chromatography, and 31P NMR were used to determine the origin of the higher binding energy peaks when Wilkinson's procedure was used to prepare RhCl(PPh3)3. Hydrogenation of cyclohexene was also performed to determine the effect of the higher binding energy species on catalytic activity.

scholarly journals Synthesis and Characterization of New Polyimide/Organoclay Nanocomposites Containing Benzophenone Moieties in the Main Chain

2017 ◽  
Vol 57 (2) ◽  
Author(s):  
Khalil Faghihi ◽  
Mostafa Ashouri ◽  
Akram Feyzi
Keyword(s):  
Main Chain ◽  
In Situ Polymerization ◽  
Clay Content ◽  
Nanocomposite Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

<p>A series of nanocomposites consist of organic polyimide and organo-modified clay content varying from 0 to 5 wt%, were successfully prepared by in situ polymerization. Polyimide used as a matrix of nanocomposite was prepared through the reaction of 1,4-bis [4-aminophenoxy] butane (APB) and 3،3΄،4،4΄-benzophenone tetra carboxylic dianhydride (BTDA) in N,N-dimethylacetamide (DMAc). The resulting nanocomposite films were characterized by FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA).</p>

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