Synthesis and characterization of novel polyamides based on tridecanedioic acid: Nylons 3 13, 5 13, 6 13, 7 13, 9 13, 10 13, 11 13

e-Polymers ◽  
2004 ◽  
Vol 4 (1) ◽  
Author(s):  
Xiaowen Cui ◽  
Deyue Yan ◽  
Dan Xiao
Keyword(s):  
Mechanical Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Melt Polycondensation ◽  
Step Heating ◽  
Melting And Crystallization Temperatures ◽  
Melting And Crystallization

Abstract Linear polyamides with high aliphatic content were prepared through step-heating melt polycondensation of tridecanedioic acid with various diamines. The synthesized polyamides were characterized comprehensively by means of IR, NMR and Raman spectroscopy. In addition, thermogravimetry, differential scanning calorimetry and dynamic mechanical analysis were used to investigate thermal properties of the obtained polyamides. It was found that melting and crystallization temperatures decrease as the aliphatic content increases. X-ray diffraction was applied to determine the crystal structures of the polyamides.

scholarly journals Stacking Control by Molecular Symmetry of Sterically Protected Phthalocyanines

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5552
Author(s):  
Ryota Kudo ◽  
Masahiro Sonobe ◽  
Yoshiaki Chino ◽  
Yu Kitazawa ◽  
Mutsumi Kimura
Keyword(s):  
Lamellar Structure ◽  
Synthesis And Characterization ◽  
Molecular Symmetry ◽  
X Ray Diffraction ◽  
Melting Points ◽  
Scanning Calorimetry ◽  
Structural Isomers ◽  
X Ray ◽  
Temperature Controlled

The synthesis and characterization of two phthalocyanine (Pc) structural isomers, 1 and 2, in which four 2,6-di(hexyloxy)phenyl units were attached directly to the 1,8,15,22- or 1,4,15,18-positions of the Pc rings, are described. Both Pcs 1 and 2 exhibited low melting points, i.e., 120 and 130 °C respectively, due to the reduction in intermolecular π-π interaction among the Pc rings caused by the steric hindrance of 2,6-dihexyloxybenzene units. The thermal behaviors were investigated with temperature-controlled polarizing optical microscopy, differential scanning calorimetry, powder X-ray diffraction, and absorption spectral analyses. Pc 1, having C4h molecular symmetry, organized into a lamellar structure containing lateral assemblies of Pc rings. In contrast, the other Pc 2 revealed the formation of metastable crystalline phases, including disordered stacks of Pcs due to rapid cooling from a melted liquid.

scholarly journals Synthesis and characterization of allyl- and vinyl-substituted 1,2-bis(tetrazolo)ethanes as polymeric precursors

2016 ◽  
Vol 71 (12) ◽  
pp. 1199-1209
Author(s):  
Vera A. Hartdegen ◽  
Maximilian S. Hofmayer ◽  
Konstantin Karaghiosoff ◽  
Thomas M. Klapötke
Keyword(s):  
Allyl Bromide ◽  
2D Nmr ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
2D Nmr Spectroscopy ◽  
X Ray ◽  
Physical Stimuli ◽  
Thermal Stability Of

AbstractOn the basis of 1,2-bis(5-tetrazolo)ethane (BTE) the corresponding twofold vinyl and allyl N-substituted derivatives were synthesized using 1,2-dibromoethane and allyl bromide, respectively. The compounds were obtained as two different constitutional isomers. Both species were analyzed using NMR and IR spectroscopy, elemental analysis, as well as mass spectrometry. In the case of the diallyl bistetrazoles, the two isomers were characterized using 2D NMR spectroscopy. The synthesis of the divinyl compounds gave crystals of the 2,2′-N-substituted isomer, which were analyzed by single-crystal X-ray diffraction. The thermal stability of the compounds was determined using differential scanning calorimetry (DSC) and gave decomposition temperatures around 190°C and 230°C. For the investigation of the inherent energetic potential, sensitivities toward physical stimuli and detonation parameters were determined. The compounds turned out to be insensitive toward friction and impact and possess moderate energetic properties.

Chemical synthesis and characterization of polyaniline-molybdenum trisulfide composite

1999 ◽  
Vol 14 (5) ◽  
pp. 1805-1813 ◽  
Author(s):  
Florence Fusalba ◽  
Daniel Bélanger
Keyword(s):  
Aqueous Solution ◽  
Photoelectron Spectroscopy ◽  
Synthesis And Characterization ◽  
Scanning Electron Micrographs ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Chemical Polymerization ◽  
X Ray ◽  
Scanning Electron

A novel polyaniline-molybdenum trisulfide composite has been prepared by chemical polymerization from an acidic (1 M HCl) aqueous solution containing aniline and ammonium tetrathiomolybdate. The presence of molybdenum trisulfide in the polyaniline matrix induces morphological change to the polymer as evidenced by scanning electron micrographs. X-ray diffraction and differential scanning calorimetry indicate that polyaniline-molybdenum trisulfide is slightly less crystalline than polyaniline-HCl. X-ray photoelectron spectroscopy (XPS) and elemental analysis have been used to confirm the presence of molybdenum trisulfide in the polymer matrix. The XPS data also confirm that molybdenum trisulfide and tetrathiomolybdate anions are present with polyaniline to form a new inorganic-organic composite.

Synthesis and Characterization of LiMn2O4 Nanoparticles Using Citric Acid as Chelating Agent

2009 ◽  
Vol 67 ◽  
pp. 227-232 ◽  
Author(s):  
Gurpreet Singh ◽  
Amrish Panwar ◽  
Anjan Sil ◽  
Sudipto Ghosh
Keyword(s):  
Citric Acid ◽  
Room Temperature ◽  
Sol Gel ◽  
Chelating Agent ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Powder Particles

Nanocrystalline LiMn2O4 powder was synthesized by sol-gel method using citric acid as a chelating agent. The powders were characterized by X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Differential scanning calorimetry (DSC), Differential thermal analysis (DTA), Impedance spectroscopy (IS) and Electrochemical measurements. The powder particles having slight agglomeration characteristics were found to have prismatic morphology and a wider size distribution from 50 nm to 200 nm, which provides good packing density of the material. The electrical conductivity of the powder at room temperature is in the order of ~10-5 S/cm. The structural stability of LiMn2O4 cubic spinel over the temperature range of battery operation was assessed. Electrochemical performance of the material shows a discharge capacity of ~130 mAh/gm.

Synthesis and characterization of 1,4-diazophenylenebridged Cu-phthalocyanine polymer

e-Polymers ◽  
2004 ◽  
Vol 4 (1) ◽  
Author(s):  
Cemil Alkan ◽  
Leyla Aras ◽  
Güngör Gündüz
Keyword(s):  
Electrical Conductivity ◽  
Diazonium Salt ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Uv Visible ◽  
Soluble Part

Abstract A novel type of phthalocyanine polymer, 1,4-diazophenylene-bridged Cuphthalocyanine, was prepared from the diazonium salt of diaminobenzene and Cu(II) 1,8,15,22-tetraaminophthalocyanine. The polymer is partially soluble in tetrahydrofuran, dichloromethane, and dimethylformamide. Characterization of the polymer was performed by IR and UV-visible spectroscopy, X-ray diffraction, ash analysis, viscometry, differential scanning calorimetry and thermogravimetric analysis. The molecular weight of the soluble part of the polymer was determined by ebullioscopy. Electrical conductivity of the polymer and its doped samples were determined by the 4-probe technique. It was found that the electrical conductivity increased up to 10-4 S/cm after doping. The redox behaviour of the polymer was investigated utilizing cyclic voltammetry.

Study of Cellulose-Dibutyl Sebacate Copolymer Synthesis and Characterization of Crosslinked Cellulose-Dibutyl Sebacate Copolymers for Oil Absorbency

2011 ◽  
Vol 311-313 ◽  
pp. 2075-2083
Author(s):  
Halidan Mamat
Keyword(s):  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Reaction Conditions ◽  
X Ray ◽  
Oil Absorbency ◽  
Dibutyl Sebacate ◽  
Oil Absorbent

A novel cellulose-based oil absorbent crosslinked cellulose-dibutyl sebacate copolymers was prepared by the graft crosslinking polymerization of in situ synthesized dibutyl sebacate and cotton cellulose using potassium persulfate as an initiator. The copolymers were characterized by infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetry, differential scanning calorimetry, etc. The effects of reaction conditions, such as, ratio of reaction regents, reaction temperature, reaction time, etc, on the efficiency of oil absorbency were examined. The optimized reaction conditions for the synthesis of crosslinked cellulose-dibutyl sebacate copolymers were: m(cotton pulp):m(K2S2O8 initiator):m(dibutyl sebacate) = 1 0.025 2.0(W/W)，75°C，and 5-6 h. The resulting crosslinked cellulose-dibutyl sebacate copolymers were floppy and exhibited excellent oil absorbency efficiency.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

Studies on the Preparation, Characterization and Solubility of -Cyclodextrin-Roxythromycin Inclusion Complexes

2009 ◽  
Vol 2 (2) ◽  
pp. 523-530
Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Inclusion Complexes ◽  
Phase Solubility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ir Studies ◽  
Poorly Soluble ◽  
Poorly Soluble Drug

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.

scholarly journals Synthesis and Characterization of Clay Polymer Nanocomposites of P(4VP-co-AAm) and Their Application for the Removal of Atrazine

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Nanocomposite Materials ◽  
Synthesis And Characterization ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
Numerous Species ◽  
X Ray ◽  
Different Types ◽  
Synthesized Materials

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.

scholarly journals High-pressure synthesis and characterization of the non-centrosymmetric scandium borate ScB6O9(OH)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Structure Solution ◽  
Temperature Experiment ◽  
Pressure Synthesis

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.

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