Styrene-maleic anhydride copolymers: Synthesis,characterization, and thermal properties

Radical copolymerization of styrene and maleic anhydride have been carried out in N, N-dimethylformamide at 60°C using 2,2′-azobisisobutyronitrile as initiator. The copolymer compositions were determined using an aqueous conductometric direct titration method. Monomer reactivity ratios were calculated by Fineman-Ross, Kelen-Tudos, and conversion-based Kelen-Tudos methods. Gel permeation chromatography was used to determine molecular weights and polydispersity indexes. The thermal degradation and energy of activation of the degradation process were determined by several thermogravimetric analysis and differential scanning calorimetric models. The thermal degradation of the copolymer is a two-stage process, the major degradation being the second stage. The copolymer degrades at a lower temperature than polystyrene. © 1996 John Wiley & Sons, Inc.     

Synthesis,characterization, and kinetic study on the thermal decomposition of polyamidoethers

Some new polyamidoethers have been synthesized by condensation reaction of N,N'-dichloroacetyl-1,4-phenylene-diamine with bisphenols (4,4'-isopropylidenediphenol, 4,4'-dihydroxydiphenyl sulfone, 4,4'-dihydroxydiphenyl sulfide, and 4,4'-dihydroxybiphenyl) in N-methylpyrrolidone medium using DB-24-Crown-8 as a phase-transfer catalyst. The structure of these polymers has been characterized by infrared (i.r.) and ¹H nuclear magnetic resonance (NMR) spectroscopy. Kinetic method of thermal decomposition of these polymers and their 2% mixture with polyvinylchloride (PVC) has been studied.     

Synthesis,characterization and thermal decomposition behaviour of triphenylphosphine-linked multiwalled carbon nanotubes

Triphenylphosphine-linked multiwalled carbon nanotubes (Tpp-MWCNT) were prepared in aprotic media and under anhydrous conditions by treating bromo-arylated-MWCNT with potassium diphenylphosphine (Tpp-MWCNT (1)), or with chlorodiphenylphosphine and butyllithium (Tpp-MWCNT (2)). Tpp-MWCNT were characterised by various techniques, including transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS). The presence of the expected elements (C and P) is evident in the XPS spectra. Furthermore XPS results showed the presence of phosphorus with average concentrations of 0.7% and 2.6% in Tpp-MWCNT (1) and Tpp-MWCNT (2), respectively. TGA results revealed the following thermal decomposition order: Tpp-MWCNT (2) < Tpp-MWCNT (1) < purified MWCNT, thus suggesting that the thermal stability of the MWCNT decreases with increasing amount of triphenylphosphine moieties attached to their surface. Moreover TGA results demonstrate that Tpp-MWCNTs have improved flame retardant behaviour since they produce 4–5 times more char than purified MWCNT.     

A new Schiff base epoxy oligomer resin: Synthesis,characterization, and thermal decomposition kinetics

Oligo{2,2′‐{1,4‐phenylenebis[nitrilomethylylidene]}bis(6‐methoxyphenol)} (OPNMMP) was synthesized from o‐vanillin and p‐phenylene diamine by oxidative polycondensation with NaOCl in an aqueous alkaline. Then, a new Schiff Base epoxy oligomer resin, OPNMMP–epichlorohydrine (EPC), was produced with EPC. The structures of the resulting compounds were confirmed by Fourier transform infrared spectroscopy, ultraviolet–visible spectroscopy, ¹H‐NMR, and ¹³C‐NMR. Further characterization processes were preformed by thermogravimetry (TG)–differential thermal analysis, gel permeation chromatography, and solubility testing. Also, the kinetics of the thermal decomposition of OPNMMP–EPC were investigated by thermogravimetric analysis. The TG curves showed that the thermal decomposition of OPNMMP–EPC occurred in one stage. The kinetic parameters related to the decomposition kinetics of OPNMMP–EPC were obtained from TG curves with the following methods: Friedman, Flynn–Wall–Ozawa, Kissinger, invariant kinetic parameter, and Coats–Redfern (CR), under an N₂ dynamic atmosphere and different heating rates (5, 10, 15, and 20°C/min). The mechanism function and pre‐exponential factor were also determined by a master plots method. The apparent activation energies of the thermal decomposition were calculated from these methods for OPNMMP–EPC. The analysis of the results obtained by the CR and master plots methods showed that the decomposition mechanism of OPNMMP–EPC in N₂ was a deceleration‐type mechanism. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

DGEBA‐grafted polyaniline: Synthesis,characterization and thermal properties

The utilization of conducting emeraldine salt (PANI‐ES) and intrinsic leucoemeraldine polyaniline (PANI‐LEB) in the synthesis of DGEBA‐grafted PANI via anionic copolymerization is described. The structures of copolymers obtained were characterized by FTIR, ¹³C and ¹H NMR. The extent of grafting was verified by THF Soxhlet (solvent extraction). The thermal properties of these new copolymers were described and their conductivities were reported. Results obtained indicated that the graft copolymer exhibited higher electrical and thermal conductivities than that of the blend counterpart. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis,characterization, and kinetics study of thermal decomposition of epoxidized soybean oil acrylate

The synthesis of epoxidized soybean oil acrylate (ESOA) from epoxidized soybean oil (ESO) had been carried out by reacting acrylic acid with the oxirane group in ESO. The acrylated ESO products were characterized using a variety of analytical techniques. The oxygen value, iodine value, and acid value were obtained to know the amount of unsaturation in the synthesized product. Infrared and proton NMR spectra were carried out to confirm the participation of oxirane group in the acrylation reaction. Free‐radical initiators, benzoyl peroxide and tertiary butyl peroxy benzoate, were used for the curing of ESOA resin. Thermal decomposition kinetics of ESOA was studied by the methods of Ozawa, Kissinger, and Horowitz‐Metzger, and the kinetic parameters were compared. The thermal decomposition data of the cured ESOA resin was analyzed by thermogravimetric analysis (TGA) at different heating rates. TG curves showed that the thermal decomposition of the ESOA system occurred in one stage. The apparent activation energies determined by the Ozawa, Kissinger, and Horowitz‐Metzger methods are 122.69, 95.347, and 126.20 kJ/mol, respectively. The results show that there was a reasonably good agreement between the calculated activation energies for stage one in the above methods. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis,characterization, thermal and flame-retardant properties of silicon-based epoxy resins

A new silicon-containing oxirane triglycidyl phenyl silane oxide (TGPSO) and its corresponding silicon-containing epoxy resins are synthesized and characterized. The activation energies of TGPSO curing reaction with various curing agents, including 4,4-diaminodiphenylmethane, 4,4-diaminodiphenylsulfone, and dicyanodiaminde, are found to be 180, 196.5, and 154 kJ/mol. The curing reaction of TGPSO with diamines is determined to be a first-order reaction through means of Arrhenius plots. The introduction of the silicon-containing group results in higher curing reactivity. This silicon-containing resin possesses higher char yield as well as higher limiting oxygen index (LOI = 35) than the commercial epoxy resins, confirming the usefulness of these silicon-containing epoxy resins as flame retardants. Char yields and LOI measurements demonstrate that incorporating silicon into epoxy resins is able to improve their flame retardancy. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 1231–1238, 1999     

Synthesis,characterization and assessment thermal properties of clay based nanopigments

Nano-clay based pigments (NCP) are new type of pigments composed of organic dyes and layered silicate-clay nano-particles, and have already been used in polymeric coatings to improve mechanical thermal and stability properties. In this paper, the basic blue 41(BB41) was intercalated into Na⁺- montmorillonite in an aqueous medium. The dye-intercalated montmorillonite was centrifuged, dried, and milled to prepare the nanopigment particles. X-ray diffraction showed an increase in the basal spacing, thus confirming intercalation of the BB41 molecules within the nanostructures of the interlayer spaces. Fourier transform infrared spectroscopy was used for identifying the functional groups and chemical bounding of Na⁺-montmorillonite, BB41 and montmorillonite-BB41. The morphology of NCP was also studied by transmission electron microscopy. Finally, thermo-gravimetric analysis and differential thermograms suggested the thermal stability of the intercalated dye was improved.     

Cellulose hydrogels physically crosslinked by glycine: Synthesis,characterization, thermal and mechanical properties

Biopolymers are very efficient for significant applications ranging from tissue engineering, biological devices to water purification. There is a tremendous potential value of cellulose because of its being the most abundant biopolymer on earth, swellability, and functional groups to be modified. A novel, highly efficient route for the fabrication of mechanically stable and natural hydrogels is described in which cellulose and glycine are dissolved in an alkaline solution of NaOH and neutralized in an acidic solution. The dissolving temperature and the glycine amount are essential parameters for the self-assembly of cellulose chains and for tuning the morphology and the aggregate structures of the resulting hydrogels. Glycine plays the role of a physical crosslinker based on the information obtained from FTIR and Raman spectra. Among the prepared set of hydrogels, CL5Gly30 hydrogels have the highest capacity to absorb water. The prepared CL5Gly30 gels can absorb up to seven times their dry weight due to its porous 3-D network structure. CL5Gly10 hydrogel exhibits 80% deformation under 21 N force executed. The method developed in this article can contribute to the application of heavy metal adsorption in aqueous solutions for water purification and waste management. © 2019 The Authors. 137 published by Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48380.     

Synthesis,structure and thermal decomposition of alinite

Alinite was synthesized from CaCl₂ fluxes containing MgO. Mg is essential and cannot be omitted. In contrast to the formula given by Ilyukhin et al. EPMA measurements revealed the composition Ca_9.9Mg_0.8□_0.3[Si_3.4Al_0.6O₁₆]O_1.9Cl_1.0 Spectroscopic and X-ray structure investigations favour the CaO₆ octahedra for substitution by Mg. No phase transformations were detected by DTA and X-ray diffraction. The thermal decomposition begins at 1000°C, its rate depends strongly on the crystal size.     

新型溴代长波长BODIPY类荧光染料的合成及表征

通过吡咯和乙酰氯经一步法合成了含吡咯取代基的长波长BODIPY染料,溴化后得到一溴和二溴染料,染料通过质谱、二维核磁等手段进行了结构表征.测试了这些染料的吸收光谱和发射光谱,研究了不同极性的溶剂对染料光谱性能的溶剂化效应以及Br原子对染料光谱的重原子效应.结果表明:随着溶剂极性的增大所合成的染料吸收波长均发生了蓝移,发射波长变化不大,摩尔消光系数逐渐增大,荧光量子产率逐渐减小,表现出明显的溶剂化效应;在同一溶剂中,随着染料结构中Br原子取代基数目的增加,发射波长发生红移,吸收波长变化不大,摩尔消光系数逐渐增大,荧光量子产率逐渐减小,表现出明显的重原子效应.     

Synthesis,properties and thermal decomposition of the Ta4AlC3 MAX phase

The present work describes a synthesis route for bulk Ta₄AlC₃ MAX phase ceramics with high phase purity. Pressure-assisted densification was achieved by both hot pressing and spark plasma sintering of Ta₂H, Al and C powder mixtures in the 1200–1650 °C range. The phases present and microstructures were characterized as a function of the sintering temperature by X-ray diffraction and scanning electron microscopy. High-purity α-Ta₄AlC₃ was obtained by hot pressing at 1500 °C for 30 min at 30 MPa. The β-Ta₄AlC₃ allotrope was observed in the samples produced by SPS. The Young’s modulus, Vickers hardness, flexural strength and single-edge V-notch beam fracture toughness of the high-purity bulk sample were determined. The thermal decomposition of Ta₄AlC₃ into TaC_x and Al vapour in high (˜10⁻⁵ mbar) vacuum at 1200 °C and 1250 °C was also investigated, as a possible processing route to produce porous TaC_x components.     

Synthesis, characterization, and thermal properties of poly(siloxane-carborane)s

Three exactly alternating carborane-siloxane polymers P1, P2, and P3, have been synthesized by the polycondensation of 1,7-bis(dimethylhydroxylsilyl)-m-carborane and cyclotrisilazanes in the presence of (NH₄)₂SO₄. The reaction shows a new and convenient synthesis of poly(carborane-siloxane)s, and the first example of stoichiometric polycondensation of cyclosilazanes with diols. The new polymers P2 and P3 could be converted into thermosets at elevated temperature through the cross-linking of pendant vinyl groups. The structures of the polymers were fully characterized. Thermogravimetric analysis (TGA) showed the superior thermal stability of the polymers and thermosets, with their char yields of over 83% both in air (800 °C) and nitrogen (1000 °C). The microstructure of the chars was studied by scanning electron microscopy (SEM). It was found that the cross-linking of vinyl groups helped in enhancing the thermal stabilities of the polymers and keeping the integrity of the chars. The results suggest their potential utility under severe thermal and/or thermo-oxidative conditions.     

Synthesis,characterization, and thermal properties of cyanate esters with azo linkages

A series of azo functionalized diols were synthesized through diazotization which involves the reaction of amine with phenol and 2,6‐dimethyl phenol. Four different amines have been used to prepare five bisphenols. These bisphenols were converted to their corresponding cyanate esters by treatment with cyanogen bromide (BrCN) in the presence of triethylamine (Et₃N). The chemical structures of the prepared compounds were characterized with Fourier Transform Infrared, ¹H‐NMR, ¹³C‐NMR spectroscopy, and elemental analysis. Dynamic curing behavior was investigated using differential scanning calorimetry. The maximum curing temperature of these cyanate esters are in the range of (186–208°C). T_g values of the polycyanurate networks are in the range of 245–276°C. The thermal properties of cured cyanate ester were studied at a heating rate of 10°C min^?1 in N₂ atmosphere. The polymers showed excellent thermal stability (T₁₀ was found to be in the range 405–438°C) and the percentage of char yield at 800°C were found to be 30–49. The flame retardancy of the cyanate ester resins have been studied using limited oxygen index value which is in the range of 29.5–37.1 at 800°C. POLYM. ENG. SCI., 55:47–53, 2015. © 2014 Society of Plastics Engineers     

Synthesis,characterization, and thermal properties of alkyl‐functional naphthoxazines

A series of alkyl‐functional naphthoxazine resins having various alkyl chain lengths from C1 to C18 are synthesized with a high yield and high purity by the reactions of 1,5‐dihydroxynaphthalene, formaldehyde, and aliphatic amines. The proposed chemical structures of the naphthoxazines are confirmed by high‐resolution mass spectrometry, ¹H nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy, and pyrolysis mass spectrometry studies. The alkyl‐functional naphthoxazines have shown low polymerization temperature characteristics where polymerization of these monomers is achieved in the range of 150–170°C yielding cross‐linked polynaphthoxazines. The low‐temperature polymerization characteristics and the associated thermal degradation behaviors are studied. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Ketimine substituted polyphenol: Synthesis,characterization and investigation of its thermal and electrochemical properties

Oxidative polycondensation of 3‐(1‐(2‐phenylhydrazono)ethyl)phenol (3‐PHEP) was studied using oxidants such as sodium hypochlorite, air (O₂) and hydrogen peroxide in an aqueous alkaline medium under various polymerization conditions. The polymerization yield, molecular weight, solubility, and thermostability of the polymer were investigated. The macromolecular structure of the resulting polymer was characterized by elemental analysis, ultraviolet–visible, Fourier transform infrared, and nuclear magnetic resonance techniques. Thermogravimetric analysis showed poly(3‐PHEP) to be highly stable against thermo‐oxidative decomposition. Mass loss of the polymer was found to be only 16.3% at 1000°C. In addition, the highest occupied molecular orbital–lowest unoccupied molecular orbital energy levels, electrochemical (E_g′) band gaps and optical (E_g) band gaps were calculated from cyclic voltammetry and ultraviolet–visible measurements, respectively. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

TATB thermal decomposition: An improved kinetic model for explosive safety analysis

We investigate and model the cook-off behavior of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) to understand the response of explosive systems in abnormal thermal environments. Decomposition has been explored via conventional ODTX (one-dimensional time-to-explosion), PODTX (ODTX with pressure-measurement), PyGC-MS (pyrolysis gas chromatography mass spectrometry), TGA (thermo-gravimetric analysis), DSC (differential scanning calorimetry), and IR (infrared spectroscopy) experiments under isothermal and ramped temperature profiles. The data were used to fit rate parameters for proposed reaction schemes in a MATLAB thermo-chemical computational model. These parameterizations were carried out utilizing a genetic algorithm optimization method on LLNL's high-performance computing clusters, which enabled significant parallelization. These results include a multi-step reaction decomposition model, identification of likely autocatalytic gas-phase species, accurate high-temperature sensitization, and prediction of confined system pressurization. This model will be scalable to several applications involving TATB-based explosives, like LX-17, including thermal safety models of full-scale systems.     

Synthesis, structural investigation, thermal decomposition, and properties of a cocrystal energetic perchlorate amine salt

The molecular and crystal structure of a cocrystal energetic material (ethylenediamine triethylenediamine tetraperchlorate) is determined by means of the x-ray diffraction analysis. The compound crystallizes in the orthorhombic system of the Cmc21 space group with cell dimensions a = 8.1030±0.0016 ?, b = 24.725±0.005 ?, and c = 10.195±0.002 ?. The thermal decomposition mechanism of the title compound is studied by applying the Kissinger’s and Ozawa’s methods. Sensitivity tests reveal that the title compound has a sensitive nature.     

Synthesis, structures and magnetic properties of carbon-encapsulated nanoparticles via thermal decomposition of metal acetylide

A new low-temperature synthetic method for carbon-encapsulated metal and metal carbide nanoparticles was developed, where the metal cation M²⁺ is reduced by . In this method, metal cations form clusters at the beginning, followed by neutralization and segregation. Formations of metallic tin and cobalt, and metastable carbides of cobalt, palladium and nickel are evidenced by powder X-ray diffractions. TEM observation reveals that the nanoparticles are encapsulated in carbon shells despite the low temperature treatment. The formation of the metastable carbides and carbon shells can be explained by the carbon-rich precursor, acetylide clusters. Surplus carbon atoms tend to be excluded from the metal-carbon cores even at low temperature, automatically forming carbon shells.