Synthesis of ortho-methyltetrahydrophthalimide functional benzoxazine containing phthalonitrile group: Thermally activated polymerization behaviors and properties of its polymer

2020 ◽  
pp. 095400832095451
Author(s):  
Rui Yang ◽  
Yuting Wang ◽  
Boran Hao ◽  
Kan Zhang
Keyword(s):  
Scanning Calorimetry ◽  
Thermally Activated ◽  
Chemical Structures ◽  
Yield Value ◽  
Release Capacity ◽  
Mannich Condensation ◽  
Ft Ir ◽  
Lower Temperature ◽  
Heat Release Capacity

Two novel benzoxazine monomers, oHMTI-a and oHMTI-pn, have been obtained via the modified Mannich condensation from ortho-4-methyltetrahydrophalimide functional phenol, paraformaldehyde, and aniline/4-aminophthalonitrile, respectively. The chemical structures of both benzoxazine monomers have been studied by Fourier transform infrared (FT-IR) and 1H and 13C nuclear magnetic resonance (NMR) spectra. Their polymerization processes are investigated using in-situ FT-IR and different scanning calorimetry (DSC). Specifically, the phthalonitrile group in oHMTI-pn can react at a relatively lower temperature without adding any catalysts, which suggests the presence of the thermal synergistic polymerization effect in this benzoxazine monomer. In addition, the thermal and fire related properties of the resulting polybenzoxazines are evaluated by thermogravimetric analysis (TGA) and micro-scale combustion calorimetry (MCC). The polybenzoxazine derived from oHMTI-pn shows both high thermal stability and outstanding flame retardancy, with a T g of 350°C, a T d10 value of 417°C, a high char yield value of 65%, and a very low heat release capacity value of 35.2 J/(g·K).

scholarly journals Preparation, Thermal, and Thermo-Mechanical Characterization of Polymeric Blends Based on Di(meth)acrylate Monomers

Polymers ◽  
2021 ◽  
Vol 13 (6) ◽  
pp. 878
Author(s):  
Krystyna Wnuczek ◽  
Andrzej Puszka ◽  
Łukasz Klapiszewski ◽  
Beata Podkościelna
Keyword(s):  
Mechanical Analysis ◽  
Attenuated Total Reflection ◽  
Scanning Calorimetry ◽  
Force Microscopy ◽  
Chemical Structures ◽  
Atomic Force ◽  
Polymeric Blends ◽  
Ft Ir ◽  
Acrylate Monomers ◽  
Synthesized Materials

This study presents the preparation and the thermo-mechanical characteristics of polymeric blends based on di(meth)acrylates monomers. Bisphenol A glycerolate diacrylate (BPA.GDA) or ethylene glycol dimethacrylate (EGDMA) were used as crosslinking monomers. Methyl methacrylate (MMA) was used as an active solvent in both copolymerization approaches. Commercial polycarbonate (PC) was used as a modifying soluble additive. The preparation of blends and method of polymerization by using UV initiator (Irqacure® 651) was proposed. Two parallel sets of MMA-based materials were obtained. The first included more harmless linear hydrocarbons (EGDMA + MMA), whereas the second included the usually used aromatic copolymers (BPA.GDA + MMA). The influence of different amounts of PC on the physicochemical properties was discussed in detail. Chemical structures of the copolymers were confirmed by attenuated total reflection–Fourier transform infrared (ATR/FT-IR) spectroscopy. Thermo-mechanical properties of the synthesized materials were investigated by means of differential scanning calorimetry (DSC), thermogravimetric (TG/DTG) analyses, and dynamic mechanical analysis (DMA). The hardness of the obtained materials was also tested. In order to evaluate the surface of the materials, their images were obtained with the use of atomic force microscopy (AFM).

scholarly journals Design of High-Performance Polybenzoxazines with Tunable Extended Networks Based on Resveratrol and Allyl Functional Benzoxazine

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 2794
Author(s):  
Yunliang Xing ◽  
Xianru He ◽  
Rui Yang ◽  
Kan Zhang ◽  
Shengfu Yang
Keyword(s):  
High Performance ◽  
Condensation Reaction ◽  
Good Thermal Stability ◽  
Chemical Structures ◽  
Dsc Measurements ◽  
Mannich Condensation ◽  
Polymerization Behavior ◽  
Oxazine Ring ◽  
Nmr Techniques ◽  
Ft Ir

A novel resveratrol-based bio-benzoxazine monomer (RES-al) containing an allyl group has been synthesized using resveratrol, allylamine, and paraformaldehyde via Mannich condensation reaction, and its chemical structures have been characterized by FT-IR spectroscopy and NMR techniques. The polymerization behavior of this benzoxazine resin has been investigated using in situ FT-IR and differential scanning calorimeter (DSC) measurements, and the thermal-mechanical properties of its corresponding polybenzoxazines are evaluated by DMA and TGA. We show that by controlling the curing process of the oxazine ring, the C=C bond in resveratrol, and the allyl group in RES-al, the cross-linking network of the polybenzoxazine can be manipulated, giving rise to tunable performance of thermosets. As all curable functionalities in RES-al are polymerized, the resulted polybenzoxazine exhibits a good thermal stability with a Tg temperature of 313 °C, a Td5 value of 352 °C, and char yield of 53% at 800 °C under N2.

Bioenveloping Inorganic Filler-Based Eggshell Wastes for Enhancing the Properties of Natural Rubber Biocomposites

2020 ◽  
Author(s):  
Hesham Moustafa ◽  
Soma El-Mogy ◽  
Saber A. Ibrahim ◽  
Anhar Awad ◽  
Nabila A. Darwish
Keyword(s):  
Mechanical Properties ◽  
Natural Rubber ◽  
Infrared Imaging ◽  
Morphological Data ◽  
Inorganic Filler ◽  
Scanning Calorimetry ◽  
Potential Alternative ◽  
Fourier Transform Infrared Imaging ◽  
Ft Ir ◽  
Lower Temperature

ABSTRACT In this study, eggshell (ES) wastes were used as a renewable reinforcing material in natural rubber (NR) composite to limit carbon production. Long bio-alkyd resin (LAR) was also used to envelope the inorganic ES particles and to aid in dispersing the filler in the NR matrix. The effect of the coated ES filler (ESR) in the rubber mix on the morphology, mechanical properties, and swelling was investigated. The ES filler and its biocomposites were characterized by X-ray fluorescence, scanning electron microscopy, Fourier transform infrared imaging microscope (FT-IR-IM), differential scanning calorimetry (DSC), and thermogravimetric analysis. The morphological data reveal that the resin enhances the dispersion of the ES filler in the NR matrix. These data were confirmed by the results obtained from FT-IR-IM. The swelling and mechanical properties were significantly improved when the coated filler was used in NR matrix, especially at 20 wt.% ESR. DSC thermograms revealed that the increase in the resin caused the glass transition temperature (Tg) to be shifted to a lower temperature. The obtained results show that the bioenveloping ESR can be used as potential alternative for green tire and vehicle applications rather than conventional petroleum-based filler.

Preparation and Thermal Stability of Pyrrole and m-Toluidine Copolymer/Montmorillonite Composites

2014 ◽  
Vol 915-916 ◽  
pp. 780-783
Author(s):  
Hong Wang ◽  
Ming Tian Li ◽  
Yue Lu ◽  
Di Liu
Keyword(s):  
Thermal Stability ◽  
Interfacial Interaction ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Chemical Polymerization ◽  
X Ray ◽  
Ft Ir ◽  
Clay Layers ◽  
Thermal Stability Of

Pyrrole and m-toluidine copolymer (P(PY/MT)) / montmorillonite (MMT) Composites were prepared by in situ chemical polymerization of pyrrole with m-toluidine monomer in the presence of montmorillonite. The structural, morphological and thermal properties of these composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and differential scanning calorimetry (DSC). X-ray diffraction result for P(PY/MT)-MMT illuminated the intercalation of P(PY/MT) copolymer between the clay layers. The FT-IR result showed the successful incorporation of montmorillonite clay in the prepared P(PY/MT)/MMT composite. The higher thermal stability of high MMT content rate might be attributed to its higher chain compactness due to the interfacial interaction between the P(PY/MT) and the clay.

In-Situ Characterisation of Precipitation in AI-Cu thin films

1999 ◽  
Vol 562 ◽  
Author(s):  
J. P. Lokker ◽  
A. J. Bottger ◽  
G. C. A. M. Janssen ◽  
S. Radelaar
Keyword(s):  
Thin Films ◽  
Differential Scanning Calorimetry ◽  
Bulk Material ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Enthalpy Changes ◽  
Thin Foils ◽  
Lower Temperature

ABSTRACTThe precipitate formation occurring in Al-Cu thin foils with copper concentrations of either 1.15 at.% or 0.3 at.%, has been studied. In-situ X-ray diffraction analysis and differential scanning calorimetry are applied to determine the phases formed and the enthalpy changes in the same samples. Both X-ray diffraction and differential scanning calorimetry indicate that the precipitation behaviour of thin films (about 500 nm thickness) differs significantly from that of bulk material. In the films studied the precipitation of Al2Cu occurs at a much lower temperature than expected on the basis of the (bulk) phase diagram. Moreover, no intermediate phases are observed prior to Al2Cu precipitation. Also the amount of Cu in solid solution (0.20 at%Cu) observed by electron-probe micro-analysis after slowly cooling from 500°C to room temperature, exceeds the solubility of bulk Al-Cu.

scholarly journals Synthesis and characterization of linear and crosslinked polymers with the addition of DMSPS

2019 ◽  
Vol 73 (1) ◽  
pp. 1
Author(s):  
Karolina Fila ◽  
Beata Podkościelna
Keyword(s):  
Spectroscopic Analysis ◽  
Bulk Polymerization ◽  
Synthesis And Characterization ◽  
Scanning Calorimetry ◽  
Chemical Structures ◽  
Hardness Tests ◽  
Ft Ir ◽  
The Impact ◽  
Sulfur Containing

<p>The aim of this research was the synthesis of polymers with the addition of S,S'-thiodi-4,1-phenylene bis(thiomethacrylate) (DMSPS) by bulk polymerization. Styrene (St), divinylbenzene (DVB) and ethylene glycol dimethacrylate (EGDMA) were used for the copolymerization as main monomers. The chemical structures of sulfur-containing polymers were confirmed by the spectroscopic analysis (ATR/FT-IR). In order to determine the impact of the sulfur derivative (DMSPS) addition on thermal properties of the obtained copolymers, differential scanning calorimetry (DSC) was performed. The hardness tests of the obtained copolymers were also applied using a Shore durometer.</p>

scholarly journals Preparation and Performance of Nano-hybrids Synthesized from Polyimide and Silica

2009 ◽  
Vol 2 (1) ◽  
pp. 99-107 ◽  
Author(s):  
S. M. M. Alam
Keyword(s):  
Sol Gel ◽  
Tensile Modulus ◽  
Mechanical Analysis ◽  
Hybrid Films ◽  
Scanning Calorimetry ◽  
Chemical Structures ◽  
Sol Gel Process ◽  
Biphenyltetracarboxylic Dianhydride ◽  
Silica Hybrid

Polyimide (PI)-inorganic like silica hybrid films were successfully prepared to combine the good performances of silica like tensile modulus, thermal stability etc. into organic PI. Polyamic acid (PAA), precursor of PI, was prepared from 3, 3′, 4, 4′-biphenyltetracarboxylic dianhydride (BPDA), p-phenylediamine (PDA) and in-situ formed silica was formed into PAA from tetraethoxysilane (TEOS) through in-situ sol-gel process. The films were transparent and became translucent in presence of up to 10% inorganic contents. The chemical structures were characterized by Fourier transform infrared spectroscopy (FTIR). The morphology of the films was investigated by scanning electronic microscopy (SEM). Differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), stress-strain tests and dynamic mechanical analysis (DMA) were used to evaluate the performances of the films. The results indicated that the glass-transition temperatures (Tg) and decomposition temperatures of the PI-silica hybrid films were higher than those of pristine PI. Tensile modulus, tensile strength of PI increased prominently in presence of small amount (1%) of silica in PI-silica hybrid. Keywords: Polyimide; Hybrid; Sol-gel process. © 2010 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved. DOI: 10.3329/jsr.v2i1.2733                 J. Sci. Res. 2 (1), 99-107 (2010)  

scholarly journals Synthesis of Eugenol-Based Silicon-Containing Benzoxazines and Their Applications as Bio-Based Organic Coatings

Coatings ◽  
2018 ◽  
Vol 8 (3) ◽  
pp. 88 ◽  
Author(s):  
Jinyue Dai ◽  
Shimin Yang ◽  
Na Teng ◽  
Yuan Liu ◽  
Xiaoqing Liu ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Moisture Absorption ◽  
High Hardness ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Good Thermal Stability ◽  
Chemical Structures ◽  
Ring Opening Reaction ◽  
Ft Ir ◽  
Excellent Adhesion

In this work, several bio-based main-chain type benzoxazine oligomers (MCBO) were synthesized from eugenol derivatives via polycondensation reaction with paraformaldehyde and different diamine. Afterwards, their chemical structures were confirmed by Fourier Transform Infrared Spectroscopy (FT-IR) and Nuclear Magnetic Resonance Spectroscopy (1H-NMR). The curing reaction was monitored by Differential Scanning Calorimetry (DSC) and FT-IR. The polybenzoxazine films were prepared via thermal ring-opening reaction of benzoxazine groups without solvent, and their thermodynamic properties, thermal stability, and coating properties were investigated in detail. Results indicated that the cured films exhibited good thermal stability and mechanical properties, showing 10% thermal weight loss (Td10%) temperature as high as 408 °C and modulus at a room temperature of 2100 MPa as well as the glass transition temperature of 123 °C. In addition, the related coatings exhibited high hardness, excellent adhesion, good flexibility, low moisture absorption, and outstanding solvent resistance.

scholarly journals Study of ZnO-CNT Nanocomposites in High-Pressure Conditions

Materials ◽  
2021 ◽  
Vol 14 (18) ◽  
pp. 5330
Author(s):  
Laura-Madalina Cursaru ◽  
Sorina Nicoleta Valsan ◽  
Maria-Eliza Puscasu ◽  
Ioan Albert Tudor ◽  
Nicoleta Zarnescu-Ivan ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
High Pressure ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Transmission Electron ◽  
Specific Morphology ◽  
Ft Ir ◽  
Nanocomposite Powders

Recently, carbon nanotubes (CNTs) have been used extensively to develop new materials and devices due to their specific morphology and properties. The reinforcement of different metal oxides such as zinc oxide (ZnO) with CNT develops advanced multifunctional materials with improved properties. Our aim is to obtain ZnO-CNT nanocomposites by in situ hydrothermal method in high-pressure conditions. Various compositions were tested. The structure and morphology of ZnO-CNT nanocomposites were analyzed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry—thermogravimetry (DSC-TG), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). These analyses showed the formation of complex ZnO-CNT structures. FT-IR spectra suggest possible interactions between CNT and ZnO. DSC-TG analysis also reveals the formation of some physical bonds between ZnO and CNT, through the appearance of endothermic peaks which could be assigned to the decomposition of functional groups of the CNT chain and breaking of the ZnO-CNT bonds. XRD characterization demonstrated the existence of ZnO nanocrystallites with size around 60 nm. The best ZnO:CNT composition was further selected for preliminary investigations of the potential of these nanocomposite powders to be processed as pastes for extrusion-based 3D printing.

scholarly journals Synthesis and Characterization of Encapsulated 1-Tetradecanol for Thermal Energy Storage

2020 ◽  
Vol 8 (4S4) ◽  
pp. 264-268
Keyword(s):  
Air Conditioning ◽  
In Situ Polymerization ◽  
Cooling System ◽  
Core Material ◽  
Scanning Calorimetry ◽  
Air Conditioning System ◽  
Thermo Gravimetric Analyzer ◽  
Ft Ir ◽  
Average Size

Microencapsulated phase change material (PCM) is used for industrial and house hold air conditioning system for longer term usage. In this study 1-Tetradecanol (C14H30O) is used as a core material. Urea (CH4N2O)-Formaldehyde (CH2O) is used as shell material. Micro capsulation is made using in-situ polymerization technique. Prepared microcapsules were tested for feasibility to use cooling system. The average size was verified using Scanning Electron microscope (SEM) and result was found 3µm and shape was observed as spherical and surface morphology was smooth. The presence of chemicals of core and shell materials was verified by Fourier Transform Infra-Red spectroscopy (FT-IR). The peak temperature of microcapsules was found as 150°C from Thermo Gravimetric Analyzer (TGA). Thermal cyclic stability was verified by Differential Scanning Calorimetry (DSC). The cyclic temperature was observed as 45.9°C and 39.78°C. These prepared microcapsules can used to control the temperature of 37°C. This prepared microcapsule can be used for room air conditioning system

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