scholarly journals Synthesis of Benzene Tetracarboxamide Polyamine and Its Effect on Epoxy Resin Properties

Polymers ◽  
2018 ◽  
Vol 10 (7) ◽  
pp. 782 ◽  
Author(s):  
Seoyoon Yu ◽  
Wonjoo Lee ◽  
Bongkuk Seo ◽  
Chung-Sun Lim
Keyword(s):  
Epoxy Resin ◽  
Epoxy Resins ◽  
High Performance ◽  
Protective Coatings ◽  
Industrial Applications ◽  
Thermomechanical Properties ◽  
Scanning Calorimetry ◽  
Adhesive Properties ◽  
Cross Sectional ◽  
Value Determination

Epoxy resins have found various industrial applications in high-performance thermosetting resins, high-performance composites, electronic-packaging materials, adhesives, protective coatings, etc., due to their outstanding performance, including high toughness, high-temperature performance, chemical and environmental resistance, versatile processability and adhesive properties. However, cured epoxy resins are very brittle, which limits their applications. In this work, we attempted to enhance the toughness of cured epoxy resins by introducing benzene tetracarboxamide polyamine (BTCP), synthesized from pyromellitic dianhydride (PMDA) and diamines in N-methyl-2-pyrrolidone (NMP) solvent. During this reaction, increased viscosity and formation of amic acid could be confirmed. The chemical reactions were monitored and evidenced using 1H-NMR spectroscopy, FT-IR spectroscopy, water gel-phase chromatography (GPC) analysis, amine value determination and acid value determination. We also studied the effect of additives on thermomechanical properties using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamical mechanical analysis (DMA), thermomechanical analysis (TMA) and by measuring mechanical properties. The BTCP-containing epoxy resin exhibited high mechanical strength and adhesion strength proportional to the amount of BTCP. Furthermore, field-emission scanning electron microscopy images were obtained for examining the cross-sectional morphology changes of the epoxy resin specimens with varying amounts of BTCP.

Studies of the Physical Properties of Cycloaliphatic Epoxy Resin Reacted with Anhydride Curing Agents

2017 ◽  
Vol 737 ◽  
pp. 248-255 ◽  
Author(s):  
Tae Hee Kim ◽  
Dae Yeon Kim ◽  
Choong Sun Lim ◽  
Bong Kuk Seo
Keyword(s):  
Physical Properties ◽  
Reaction Kinetics ◽  
Epoxy Resin ◽  
High Performance ◽  
Industrial Applications ◽  
Scanning Calorimetry ◽  
Low Viscosity ◽  
High Performance Polymer ◽  
Curing Agents ◽  
The Impact

The preparation of high performance epoxy composites for industrial applications has been extensively researched. In this report, we study the change in physical properties and reaction kinetics between epoxy resin and curing agents of similar geometry. For the experiments, celloxide 2021P, an epoxy resin having low viscosity, was blended with three different curing agents: methylhexahydropthalic acid, methyltetrahydropthalic acid, and 5-norbornene-2, 3-dicarboxylic anhydride. The amount of 1, 2-dimethylimidazole catalyst was controlled, and the highest heat flow temperature (Tpeak) was observed at around 145 °C. The impact on reaction kinetics relative to the change in heating rate was studied with differential scanning calorimetry (DSC) for each of the curing agents. The glass transition temperature (Tg) of each composition was measured with a second DSC cycle. The prepared epoxy compositions were thermally cured in a metallic mold to provide pure epoxy resins without fillers. Finally, the flexural strengths of these resins were compared to each other. The authors believe that insights into choosing an appropriate epoxy binder are useful when it comes to the overall preparation of high performance polymer composites.

Synthesis of a phosphorus–nitrogen-containing flame retardant and its application in epoxy resin

2018 ◽  
Vol 31 (2) ◽  
pp. 186-196 ◽  
Author(s):  
Shuang Yang ◽  
Yefa Hu ◽  
Qiaoxin Zhang
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Epoxy Resins ◽  
Proton Nuclear Magnetic Resonance ◽  
Scanning Calorimetry ◽  
Cone Calorimeter Test

In this article, a phosphorus–nitrogen-containing flame retardant (DOPO-T) was successfully synthesized by nucleophilic substitution reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and cyanuric chloride. The chemical structure of DOPO-T was characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance (NMR) and phosphorous-31 NMR, and elemental analysis. DOPO-T was then blended with diglycidyl ether of bisphenol-A to prepare flame-retardant epoxy resins. Thermal properties, flame retardancy, and combustion behavior of the cured epoxy resins were evaluated by differential scanning calorimetry, thermogravimetric analysis, limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The results indicated that the glass transition temperature ( Tg) and temperature at 5% weight loss of epoxy resin (EP)/DOPO-T thermosets were gradually decreased with the increasing content of DOPO-T. DOPO-T catalyzed the decomposition of EP matrix in advance. The flame-retardant performance of EP thermosets was significantly enhanced with the addition of DOPO-T. EP/DOPO-T-0.9 sample had an LOI value of 36.2% and achieved UL94 V-1 rating. In addition, the average of heat release rate, peak of heat release rate, average of effective heat of combustion, and total heat release (THR) of EP/DOPO-T-0.9 sample were decreased by 32%, 48%, 23%, and 31%, respectively, compared with the neat EP sample. Impressively, EP/DOPO-T thermosets acquired excellent flame retardancy under low loading of flame retardant.

scholarly journals Fully Biobased Epoxy Resins from Fatty Acids and Lignin

Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1158 ◽  
Author(s):  
Pablo Ortiz ◽  
Richard Vendamme ◽  
Walter Eevers
Keyword(s):  
Epoxy Resin ◽  
Renewable Resources ◽  
Epoxy Resins ◽  
Linseed Oil ◽  
Tensile Tests ◽  
Present System ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Commodity Chemicals ◽  
Epoxidized Linseed Oil

The use of renewable resources for plastic production is an imperious need for the reduction of the carbon footprint and the transition towards a circular economy. With that goal in mind, fully biobased epoxy resins have been designed and prepared by combining epoxidized linseed oil, lignin, and a biobased diamine derived from fatty acid dimers. The aromatic structures in lignin provide hardness and strength to an otherwise flexible and breakable epoxy resin. The curing of the system was investigated by infrared spectroscopy and differential scanning calorimetry (DSC). The influence of the different components on the thermo-mechanical properties of the epoxy resins was analyzed by DSC, thermal gravimetric analysis (TGA), and tensile tests. As the content of lignin in the resin increases, so does the glass transition, the Young’s modulus, and the onset of thermal degradation. This correlation is non-linear, and the higher the percentage of lignin, the more pronounced the effect. All the components of the epoxy resin being commodity chemicals, the present system provides a realistic opportunity for the preparation of fully biorenewable resins at an industrial scale.

Synthesis of Carboxymethyl Starch-Bio-Based Epoxy Resin and their Impact on Mechanical Properties

2020 ◽  
Vol 234 (11-12) ◽  
pp. 1759-1769 ◽  
Author(s):  
Tariq Aziz ◽  
Hong Fan ◽  
Farman Ullah Khan ◽  
Roh Ullah ◽  
Fazal Haq ◽  
...  
Keyword(s):  
Epoxy Resin ◽  
Interfacial Adhesion ◽  
Diglycidyl Ether ◽  
Scanning Calorimetry ◽  
Adhesive Properties ◽  
Toxic Side Effect ◽  
Dimethyl Siloxane ◽  
Naturally Occurring ◽  
Lower Viscosity ◽  
Chain Lengths

AbstractIn the current research, we observed numerous suggestions are promoting the use of bio-based epoxy resins, replacing the petroleum-based products like Diglycidyl ether of bisphenol A type epoxy resin DGEBA. With the passage of time, the impending challenges include preparation of environmentally-friendly epoxy with minimum toxic side effect and improved properties. Therefore, we describe a very useful method for preparing new silicone-bridged dimethyl siloxane monomers in high quantity, derived from naturally occurring eugenol. By putting the methyl siloxane, computed with different chain lengths into their molecular backbone. Such epoxy monomers have different molecular structure with high purity. This dimethyl siloxane epoxy, with lower viscosity than commercial DGEBA epoxy, has superior thermal properties, which were evaluated using differential scanning calorimetry DSC. Modification of CMS increases the hydrophilicity. Bio-based epoxy (self-prepared) resin improved adhesive properties, with the help of modified CMS. This study presents a very easy and effective chemical modification to enhance interfacial adhesion composites with superior properties.

scholarly journals Optimization of the Curing and Post-Curing Conditions for the Manufacturing of Partially Bio-Based Epoxy Resins with Improved Toughness

Polymers ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1354 ◽  
Author(s):  
Diego Lascano ◽  
Luis Quiles-Carrillo ◽  
Sergio Torres-Giner ◽  
Teodomiro Boronat ◽  
Nestor Montanes
Keyword(s):  
Epoxy Resin ◽  
Epoxy Resins ◽  
Polymer Network ◽  
Thermomechanical Properties ◽  
Diglycidyl Ether ◽  
Polymer Chains ◽  
Cross Linking ◽  
Reactive Diluent ◽  
Gel Time ◽  
Curing Conditions

This research deals with the influence of different curing and post-curing temperatures on the mechanical and thermomechanical properties as well as the gel time of an epoxy resin prepared by the reaction of diglycidyl ether of bisphenol A (DGEBA) with an amine hardener and a reactive diluent derived from plants at 31 wt %. The highest performance was obtained for the resins cured at moderate-to-high temperatures, that is, 80 ° C and 90 ° C , which additionally showed a significant reduction in the gel time. This effect was ascribed to the formation of a stronger polymer network by an extended cross-linking process of the polymer chains during the resin manufacturing. Furthermore, post-curing at either 125 ° C   or 150 ° C yielded thermosets with higher mechanical strength and, more interestingly, improved toughness, particularly for the samples previously cured at moderate temperatures. In particular, the partially bio-based epoxy resin cured at 80 ° C and post-cured at 150 ° C for 1 h and 30 min, respectively, showed the most balanced performance due to the formation of a more homogeneous cross-linked structure.

scholarly journals New Biosourced Flame Retardant Agents Based on Gallic and Ellagic Acids for Epoxy Resins

Molecules ◽  
2019 ◽  
Vol 24 (23) ◽  
pp. 4305 ◽  
Author(s):  
Valeriia Karaseva ◽  
Anne Bergeret ◽  
Clément Lacoste ◽  
Hélène Fulcrand ◽  
Laurent Ferry
Keyword(s):  
Phenolic Compounds ◽  
Epoxy Resin ◽  
Epoxy Resins ◽  
Flame Retardants ◽  
Fire Behavior ◽  
Diglycidyl Ether ◽  
Scanning Calorimetry ◽  
Burning Behavior ◽  
Borate Ester ◽  
Thermal Stability Of

The aim of this work was an investigation of the ability of gallic (GA) and ellagic (EA) acids, which are phenolic compounds encountered in various plants, to act as flame retardants (FRs) for epoxy resins. In order to improve their fireproofing properties, GA and EA were treated with boric acid (to obtain gallic acid derivatives (GAD) and ellagic acid derivatives (EAD)) to introduce borate ester moieties. Thermogravimetric analysis (TGA) highlighted the good charring ability of GA and EA, which was enhanced by boration. The grafting of borate groups was also shown to increase the thermal stability of GA and EA that goes up respectively from 269 to 528 °C and from 496 to 628 °C. The phenolic-based components were then incorporated into an epoxy resin formulated from diglycidyl ether of bisphenol A (DGEBA) and isophorone diamine (IPDA) (72, 18, and 10 wt.% of DGEBA, IPDA, and GA or EA, respectively). According to differential scanning calorimetry (DSC), the glass transition temperature (Tg) of the thermosets was decreased. Its values ranged from 137 up to 108 °C after adding the phenolic-based components. A cone calorimeter was used to evaluate the burning behavior of the formulated thermosets. A significant reduction of the peak of heat release rate (pHRR) for combustion was detected. Indeed, with 10 wt.% of GA and EA, pHRR was reduced by 12 and 44%, respectively, compared to that for neat epoxy resin. GAD and EAD also induced the decrease of pHRR values by 65 and 33%, respectively. In addition, a barrier effect was observed for the resin containing GAD. These results show the important influence of the biobased phenolic compounds and their boron derivatives on the fire behavior of a partially biobased epoxy resin.

scholarly journals Microstructural Features and Mechanical Properties after Industrial Scale ECAP of an Al 6060 Alloy

2010 ◽  
Vol 667-669 ◽  
pp. 1153-1158 ◽  
Author(s):  
Philipp Frint ◽  
Matthias Hockauf ◽  
T. Halle ◽  
G. Strehl ◽  
Thomas Lampke ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Shear Zone ◽  
High Performance ◽  
Large Scale ◽  
Low Voltage ◽  
Tensile Tests ◽  
Industrial Applications ◽  
Industrial Scale ◽  
Opening Angle ◽  
Cross Sectional

Future applications of ultrafine-grained, high performance materials produced by equal-channel angular pressing (ECAP) will most likely require processing on an industrial scale. There is a need for detailed microstructural and mechanical characterisation of large-scale, ECAP-processed billets. In the present study, we examine the microstructure and mechanical properties as a function of location and orientation within large (50 x 50 x 300 mm³) billets of an Al 6060 alloy produced by ECAP (90° channel angle) with different magnitudes of backpressure. The internal deformation is analysed using a grid-line method on split billets. Hardness is recorded in longitudinal and cross-sectional planes. In order to further characterise the local, post-ECAP mechanical properties, tensile tests in different layers are performed. Moreover, low voltage scanning transmission electron microscopy observations highlight relevant microstructural features. We find that the homogeneity and anisotropy of mechanical properties within the billets depend significantly on the geometry of the shear zone. We demonstrate that deformation gradients can be reduced considerably by increasing the backpressure: The opening-angle of the fan-shaped shear zone is reduced from ψ ≈ 20 ° to ψ ≈ 7 ° when the backpressure is increased from 0 to 150 MPa. Backpressures of 150 MPa result in excellent homogeneity, with a relative variation of tensile mechanical properties of less than 7 %. Our investigation demonstrates that ECAP is suitable for processing homogenous, high performance materials on a large scale, paving the way for advanced industrial applications.

An improved simplified approach for curing kinetics of epoxy resins by nonisothermal differential scanning calorimetry

2017 ◽  
Vol 30 (3) ◽  
pp. 303-311 ◽  
Author(s):  
Chao Chen ◽  
Yanxia Li ◽  
Yizhuo Gu ◽  
Min Li ◽  
Zuoguang Zhang
Keyword(s):  
Differential Scanning Calorimetry ◽  
Epoxy Resin ◽  
Kinetic Parameters ◽  
Epoxy Resins ◽  
Curing Kinetics ◽  
Scanning Calorimetry ◽  
Simplified Approach ◽  
Curing Kinetic ◽  
Autocatalytic Curing ◽  
Kinetics Of

The curing kinetics of two different types of commercial epoxy resins were investigated by means of nonisothermal differential scanning calorimetry (DSC) in this work. The complex curve of measured heat flow of CYCOM 970 epoxy resin was simplified with the method of resolution of peak. Two typical autocatalytic curing reaction curves were gained and the kinetic parameters of the curing process were demonstrated by combination of those two reactions. The Kissinger method was adopted to obtain the values of the activation energy. The parameters of curing kinetic model were acquired according to the fitting of Kamal model. Isothermal DSC curve of CYCOM 970 epoxy resin obtained using the experimental data shows a good agreement with that theoretically calculated. Then, 603 epoxy resin was investigated by the simplified method and the kinetic parameters were received through the same procedure. The nonisothermal DSC curve tested according to the recommended cure cycle of 603 epoxy resin is also consistent with the calculated results. This improved simplified approach provides an effective method to analyze the curing kinetics of the epoxy resins with complex DSC curves as similar to this study.

Thermo-mechanical characterization of discontinuous recycled/repurposed carbon fiber reinforced thermoplastic organosheet composites

2021 ◽  
pp. 002199832110157
Author(s):  
Philip R Barnett ◽  
Stephen A Young ◽  
Vivek Chawla ◽  
Darren M Foster ◽  
Dayakar Penumadu
Keyword(s):  
Mechanical Properties ◽  
Carbon Fiber ◽  
High Performance ◽  
Thermomechanical Properties ◽  
Polyphenylene Sulfide ◽  
Single Fiber ◽  
Thermoplastic Resin ◽  
Scanning Calorimetry ◽  
Post Process ◽  
Process Annealing

The integration of repurposed and recycled carbon fibers into high-performance composites is essential to the adoption of composites for automotive structures due to their low-cost, high formability, and reduced environmental impact. When high areal density nonwovens of these fibers are infused with a semi-crystalline thermoplastic resin, organosheets offering competitive mechanical properties can be produced. This study examined the optimization of such composites through multiscale material characterization and post-process annealing. Single fiber tensile tests were used to characterize repurposed and recycled fiber formats. The thermomechanical properties of the polyphenylene sulfide matrix and resulting composites subjected to different post-process annealing conditions were characterized using differential scanning calorimetry, dynamic mechanical analysis, and nano-indentation. Single fiber push-in testing was conducted to evaluate the fiber–matrix interface as a function of annealing. It was shown that statistical methods based on the bootstrap principle successfully identify the effects of post-process annealing, which are otherwise masked by material inhomogeneity. Post-process annealing was shown to be an effective method of improving the resulting mechanical properties of repurposed and recycled carbon fiber organosheet composites, thereby optimizing their properties for use as a high-performance automotive structural material.

Flame-retardant halogen-free polymers using phosphorylated hexaglycidyl epoxy resin

2017 ◽  
Vol 30 (2) ◽  
pp. 202-210 ◽  
Author(s):  
Rasool Kheyrabadi ◽  
Hossein Rahmani ◽  
S Heydar Mahmoudi Najafi
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Phosphine Oxide ◽  
Flame Retardancy ◽  
High Performance ◽  
Liquid Chromatography Mass Spectrometry ◽  
Scanning Calorimetry ◽  
Epoxy Monomer ◽  
Ul 94 ◽  
Halogen Free

Flame-retardant halogen-free epoxy resin, containing phosphorus and nitrogen atoms in the main chain, was synthesized through the curing of tris(3-(bis(oxiran-2-ylmethyl)amino)phenyl)phosphine oxide (HGE, hexaglycidyl epoxy monomer), starting from tris(3-aminophenyl) phosphine oxide (TAPO) and epichlorohydrin. The molecular structure of HGE with molecular weight 660 was confirmed using Fourier transform infrared, nuclear magnetic resonance, and liquid chromatography–mass spectrometry techniques. Epoxy equivalent weight determined by titration method was 120. The thermal curing behavior of the HGE/TAPO was investigated by differential scanning calorimetry. An intense exotherm due to curing reaction was observed in the temperature range from 123°C to 215°C. The HGE cured with TAPO, 4,4′-diaminodiphenylsulfone (DDS), and 1,5-diaminonaphthalene (DAN) and the thermal behaviors were studied by thermogravimetric analysis. The flame retardancy properties of the HGE/TAPO, DDS, and DAN were evaluated by vertical burning test (UL-94 V). The high performance cured epoxy resins showed high thermal stability and UL-94 V-0 flame retardancy rating.

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