The crystal structure and thermal decomposition kinetics of cis-hexanitrostilbene

2021 ◽  
Vol 77 (1) ◽  
pp. 150-157
Author(s):  
Yunzhang Liu ◽  
Lizhen Chen ◽  
Jianlong Wang ◽  
Jun Chen ◽  
Jingqi Wang ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Energetic Material ◽  
Decomposition Temperature ◽  
Raw Material ◽  
Separation And Purification ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Light Yellow ◽  
Methyl Pyrrolidone

Hexanitrostilbene (HNS) is an energetic material with wide application and excellent comprehensive performance. cis-HNS is successfully prepared using crude HNS with a purity of 95% as the raw material and N-methyl pyrrolidone (NMP) as the solvent. After separation and purification, acetone is used as a solvent to obtain light-yellow crystals at room temperature. The molecular structure of cis-HNS is determined through analysis of Fourier transform infrared, 13C NMR and 1H NMR spectroscopy and single-crystal X-ray diffraction data. The thermal decomposition properties of cis and trans-HNS are studied using differential scanning calorimetry (DSC). When the heating rate is low, cis-HNS will undergo a crystal transformation after melting, from liquid cis-HNS to liquid trans-HNS, and then it will solidify and release heat. According to the results of DSC data, the apparent kinetic parameters of thermal decomposition of cis- and trans-HNS were obtained by Kissinger method [Kissinger (1957). Anal. Chem. 29, 1702–1706] and Ozawa method [Ozawa (1965). Bull. Chem. Soc. Jpn. 38, 1881–1886], respectively. The spontaneous combustion temperature and self-accelerating decomposition temperature of cis and trans-HNS are calculated by the Zhang-Hu-Xie-Li method [Zhang et al. (1994). Thermochim. Acta, 244, 171–176].

Liquid crystalline hyperbranched polyesters with phosphorus functional groups

2020 ◽  
pp. 095400832096053
Author(s):  
Diana Serbezeanu ◽  
Ana-Maria Macsim ◽  
Ionela-Daniela Carja ◽  
Corneliu Hamciuc ◽  
Marius Pislaru ◽  
...  
Keyword(s):  
Liquid Crystalline ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Initial Decomposition Temperature ◽  
Molar Ratios ◽  
H Nmr ◽  
Hyperbranched Polyesters ◽  
Hyperbranched Poly ◽  
C Nmr

Liquid crystalline hyperbranched poly(aryl ester)s (A2B3) were prepared by polycondensation reaction of 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)1,4-naphthalene diol with 1,3,5-benzenetricarbonyl trichloride, taken in two different molar ratios. The chemical structure of the newly synthesized hyperbranched polymers was confirmed by FTIR, 1H NMR, 13C NMR spectroscopy. The polymers exhibited high thermal stability with initial decomposition temperature above 410–435°C and char yield at 700°C higher than 40%. Combined differential scanning calorimetry, polarized optical microscopy and wide-angle X-ray diffraction measurements were carried out to closely examine their thermal behavior and phase transitions.

scholarly journals Synthesis and Characterization of N-Substituted Polyether-Block-Amide Copolymers

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 773
Author(s):  
Jyun-Yan Ye ◽  
Kuo-Fu Peng ◽  
Yu-Ning Zhang ◽  
Szu-Yuan Huang ◽  
Mong Liang
Keyword(s):  
Titanium Isopropoxide ◽  
Decomposition Temperature ◽  
Phenyl Isocyanate ◽  
Cross Linking ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Degradation Temperature ◽  
Melt Polycondensation ◽  
Structural Regularity

A series of N-substituted polyether-block-amide (PEBA-X%) copolymers were prepared by melt polycondensation of nylon-6 prepolymer and polytetramethylene ether glycol at an elevated temperature using titanium isopropoxide as a catalyst. The structure, thermal properties, and crystallinity of PEBA-X% were investigated using nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectroscopy, differential scanning calorimetry, wide angle X-ray diffraction, and thermogravimetric analysis. In general, the crystallinity, melting point, and thermal degradation temperature of PEBA-X% decreased as the incorporation of N-methyl functionalized groups increased, owing to the disruption caused to the structural regularity of the copolymer. However, in N-acetyl functionalized analogues, the crystallinity first dropped and then increased because of a new γ form arrangement that developed in the microstructure. After the cross-linking reaction of the N-methyl-substituted derivative, which has electron-donating characteristics, with poly(4,4′-methylenebis(phenyl isocyanate), the decomposition temperature of the resulting polymer significantly increased, whereas no such improvements could be observed in the case of the electro-withdrawing N-acetyl-substituted derivative, because of the incompleteness of its cross-linking reaction.

Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi
Keyword(s):  
Liquid Crystalline ◽  
Spectroscopic Method ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
Scanning Calorimetry ◽  
Polar Solvents ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.

scholarly journals A Facile Method to Construct MXene/CuO Nanocomposite with Enhanced Catalytic Activity of CuO on Thermal Decomposition of Ammonium Perchlorate

Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2457 ◽  
Author(s):  
Haifeng Zhao ◽  
Jing Lv ◽  
Junshan Sang ◽  
Li Zhu ◽  
Peng Zheng ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Catalytic Activity ◽  
Ammonium Perchlorate ◽  
Photoelectron Spectra ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Improved Performance ◽  
Calcination Method

In this work, a mixing-calcination method was developed to facilely construct MXene/CuO nanocomposite. CuO and MXene were first dispersed in ethanol with sufficient mixing. After solvent evaporation, the dried mixture was calcinated under argon to produce a MXene/CuO nanocomposite. As characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectra (XPS), CuO nanoparticles (60–100 nm) were uniformly distributed on the surface and edge of MXene nanosheets. Furthermore, as evaluated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the high-temperature decomposition (HTD) temperature decrease of ammonium perchlorate (AP) upon addition of 1 wt% CuO (hybridized with 1 wt% MXene) was comparable with that of 2 wt% CuO alone, suggesting an enhanced catalytic activity of CuO on thermal decomposition of AP upon hybridization with MXene nanosheets. This strategy could be further applied to construct other MXene/transition metal oxide (MXene/TMO) composites with improved performance for various applications.

scholarly journals Hydrothermal Synthesis of Hematite Nanoparticles Decorated on Carbon Mesospheres and Their Synergetic Action on the Thermal Decomposition of Nitrocellulose

Nanomaterials ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 968 ◽  
Author(s):  
Abdenacer Benhammada ◽  
Djalal Trache ◽  
Mohamed Kesraoui ◽  
Salim Chelouche
Keyword(s):  
Activation Energy ◽  
Thermal Decomposition ◽  
Analytical Techniques ◽  
Decomposition Reaction ◽  
Decomposition Temperature ◽  
Heating Rates ◽  
Scanning Calorimetry ◽  
Nano Catalyst ◽  
Average Size ◽  
A Minor

In this study, carbon mesospheres (CMS) and iron oxide nanoparticles decorated on carbon mesospheres (Fe2O3-CMS) were effectively synthesized by a direct and simple hydrothermal approach. α-Fe2O3 nanoparticles have been successfully dispersed in situ on a CMS surface. The nanoparticles obtained have been characterized by employing different analytical techniques encompassing Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The produced carbon mesospheres, mostly spherical in shape, exhibited an average size of 334.5 nm, whereas that of Fe2O3 supported on CMS is at around 80 nm. The catalytic effect of the nanocatalyst on the thermal behavior of cellulose nitrate (NC) was investigated by utilizing differential scanning calorimetry (DSC). The determination of kinetic parameters has been carried out using four isoconversional kinetic methods based on DSC data obtained at various heating rates. It is demonstrated that Fe2O3-CMS have a minor influence on the decomposition temperature of NC, while a noticeable diminution of the activation energy is acquired. In contrast, pure CMS have a slight stabilizing effect with an increase of apparent activation energy. Furthermore, the decomposition reaction mechanism of NC is affected by the introduction of the nano-catalyst. Lastly, we can infer that Fe2O3-CMS may be securely employed as an effective catalyst for the thermal decomposition of NC.

Preparation, characterization, and properties of polystyrene/Na-montmorillonite composites

2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik
Keyword(s):  
Electron Microscopy ◽  
Interlayer Spacing ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Sem Images ◽  
Specific Pore Volume ◽  
Transmission Electron ◽  
Thermal Stability Of

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.

scholarly journals Lipase mediated synthesis of polycaprolactone and its silica nanohybrid

2019 ◽  
Vol 91 (6) ◽  
pp. 957-965
Author(s):  
Meltem Akkulak ◽  
Yasemin Kaptan ◽  
Yasar Andelib Aydin ◽  
Yuksel Avcibasi Guvenilir
Keyword(s):  
Average Molecular Weight ◽  
Proton Nuclear Magnetic Resonance ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Structural Investigations ◽  
Crystallinity Degree ◽  
Molecular Weights ◽  
H Nmr

Abstract In this study, rice husk ash (RHA) silanized with 3-glycidyloxypropyl trimethoxysilane was used as support material to immobilize Candida antarctica lipase B. The developed biocatalyst was then utilized in the ring opening polymerization (ROP) of ε-caprolactone and in situ development of PCL/Silica nanohybrid. The silanization degree of RHA was determined as 4 % (w) by thermal gravimetric analysis (TGA). Structural investigations and calculation of molecular weights of nanohybrids were realized by proton nuclear magnetic resonance (1H NMR). Crystallinity was determined by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Scanning Electron Microscopy (SEM) was used for morphological observations. Accordingly, the PCL composition in the nanohybrid was determined as 4 %, approximately. Short chained amorphous PCL was synthesized with a number average molecular weight of 4400 g/mol and crystallinity degree of 23 %. In regards to these properties, synthesized PCL/RHA composite can find use biomedical applications.

scholarly journals Synthesis, Characterization andIn VitroAnticancer Evaluation of Itaconic Acid Based Random Copolyester

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
J. Gowsika ◽  
R. Nanthini
Keyword(s):  
Itaconic Acid ◽  
Hydrolytic Degradation ◽  
Gel Permeation Chromatography ◽  
Xrd Analysis ◽  
Titanium Tetraisopropoxide ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Melt Polycondensation

The present study deals with the synthesis and characterization of an aliphatic copolyester, poly [butylene fumarate-co-butylene itaconate] (PIFB) copolymer was obtained from itaconic acid, fumaric acid, and 1,4-butanediol using titanium tetraisopropoxide (TTiPO) through a two step process of transesterification and melt polycondensation. The synthesized aliphatic random copolyester was characterized with the help of FT-IR,1H-NMR,13C-NMR, viscosity measurements, Gel Permeation Chromatography (GPC) and X-ray diffraction (XRD) analysis. Thermal properties have been analyzed using thermogravimetric analysis (TGA) and Differential Scanning Calorimetry (DSC). Hydrolytic degradation studies were carried out in acid and alkaline regions of various pH values. The synthesized copolymer was subjected toin vitroanticancer activity studies against human breast cancer (MCF-7) cell line.

scholarly journals Use of sweet sorghum bagasse (Sorghum bicolor (L.) Moench) for cellulose acetate synthesis

BioResources ◽  
2019 ◽  
Vol 14 (2) ◽  
pp. 3534-3553
Author(s):  
José M. da Silva Neto ◽  
Líbia de S. C. Oliveira ◽  
Flávio L. H. da Silva ◽  
José N. Tabosa ◽  
José G. A. Pacheco ◽  
...  
Keyword(s):  
Cellulose Acetate ◽  
Cellulose Triacetate ◽  
Point Of View ◽  
Raw Material ◽  
Sodium Chlorite ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Sorghum Bagasse ◽  
Chemical Inputs ◽  
Sorghum Bicolor L

The objective of this work was to synthesize cellulose acetate from sorghum bagasse, a promising raw material for the production of chemical inputs, both from a photosynthetic point of view and the maturation speed compared with that of sugarcane. The bagasse was treated with hydrogen peroxide, and then cellulose was isolated using sodium chlorite, acetic acid, and sodium hydroxide. The cellulose was subjected to an acetylation reaction, from which cellulose triacetate was obtained. By means of statistical analysis, it was observed that the conditions that generated the highest solubilization of lignin (62%) and higher yield from cellulose extraction (39.5%) were 60 °C, a 6% peroxide concentration, and 4 h. Cellulose acetate was obtained with a degree of substitution of 3.66 at 25 °C and 24 h. Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetry, differential thermogravimetry, and differential scanning calorimetry analyses confirmed that the obtained cellulose presented specific characteristics of this material. Also, the reaction of acetylation was confirmed through these techniques.

scholarly journals Preparation and Properties of Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) and Polypropylene Grafting Maleic Anhydride Two-Component Materials

2018 ◽  
Vol 26 (3(129)) ◽  
pp. 17-22 ◽  
Author(s):  
Xichao Sun ◽  
Yeqian Ge
Keyword(s):  
Maleic Anhydride ◽  
High Sensitivity ◽  
Crystal Form ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Melt Mixing ◽  
Two Component ◽  
Thermal Analyser ◽  
Thermal Stability Of

In order to provide a theoretical basis for the preparation and spinnability of two-component materials, poly(3-hydroxybutyrate-co-3-hydroxyvalerate)(PHBV) and polypropylene grafting maleic anhydride (PP-g-MAH) blends were prepared by melt mixing with different ratios (100/0, 75/25, 50/50, 25/75, 0/100). Properties of the blends system were investigated by means of a mixed rheometer, scanning electron microscope, simultaneous thermal analyser, differential scanning calorimetry and X-ray diffraction. The results demonstrate that PHBV/PP-g-MAH blends exhibit different morphology of the sea-island with a change in the mix ratio. The initial thermal decomposition temperature of PHBV in the blending system is over 250 °C, which means the thermal stability of PHBV is markedly improved. The crystallisation of PHBV varied according to the blending process parameter. When the cooling velocity increases, the crystallisation peak becomes wide, the temperature of crystallisation decreases, and the crystallisation temperature of PHBV increases significantly. PHBV has a high sensitivity to variation in the shear rate, and PHBV/PP-g-MAH blends have the mixing characteristic of shear thinned liquid. There is no diffraction peak at 2θ = 22.8°, and this result certifies that PP-g-MAH changes the crystal form of PHBV. and that PP-g-MAH addition is beneficial to the spinnability of PHBV. Results show that the interplay between PHBV and PP-g-MAH is of great significance and universal for both plastics and fibres.

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