Curing study and evaluation of epoxy resin with amine functional chloroaniline acetaldehyde condensate

2015 ◽  
Vol 44 (1) ◽  
pp. 19-25
Author(s):  
T. Maity ◽  
B.C. Samanta

Purpose – The purpose of this paper was to check effectiveness of amine functional chloroaniline acetaldehyde condensate (AFCAC) as a new curing agent for diglycidyl ether of bisphenol A (DGEBA) resin. For this purpose, first AFCAC was synthesised, characterised and then curing reaction was carried out. Design/methodology/approach – Equimolecular mixture of AFCAC and DGEBA was subjected to curing reaction, and the reaction was followed by differential scanning calorimetry (DSC) analysis. The kinetic studies of this curing reaction were also carried out from those DSC exotherms. The mechanical properties, dynamic mechanical analysis (DMA) and thermogravimetric analysis (TGA) of cured epoxy were also reported. Findings – DSC results reflected the effective first order curing reaction of AFCAC with epoxy resin. Mechanical properties reflected appreciable rigidity of AFCAC cured epoxy matrix and TGA showed that the cured epoxy networks were thermally stable up to around 297°C. Research limitations/implications – The curing agent AFCAC was synthesised by using chloroaniline and acetaldehyde in acid medium. There are some limitations for this procedure. The synthetic procedure is pH dependent. So reaction cannot be done at any pH value. The reaction must also be carried out at room temperature without any heating. To obtain low molecular weight curing agent, chloroaniline and acetaldehyde cannot be taken in equimolecular ratio because the equimolecular mixture of them produces high molecular weight condensate. This was shown in our previous publication. Some implications are also there. By changing amine and aldehyde other curing agents could be synthesised and the curing efficiency of those for epoxy resin could also be studied. Originality/value – Experimental results revealed the greater suitability of AFCAC as curing agent for DGEBA resin and novelty of AFCAC cured matrix in the field of protective coating, casting, adhesives, etc.

2015 ◽  
Vol 44 (6) ◽  
pp. 358-363 ◽  
Author(s):  
Lizhu Liu ◽  
Hong Zhang ◽  
Nan Zhang ◽  
Ling Weng

Purpose – The purpose of this study is to investigate the effects of two epoxy ratio and carboxyl-terminated butadiene solid rubber (CTBN) content on adhesive and flexible copper clad laminate (FCCL) performance. The epoxy adhesive used for FCCL was prepared with epoxy resin of 901 and 6128 as matrix and CTBN as toughener. Design/methodology/approach – The epoxy adhesive was prepared with epoxy resin as matrix, CTBN as toughener and 4,4′-diamino diphenyl sulfone as curing agent in solvent of butanone by mechanical agitation. The adhesives were cast on the polyimide film; subsequently, the polyimide film was dried at 160°C for 3 min to remove the solvent. Then, it was laminated with copper foil at 180°C with the pressure of 12 MPa for 3 min. The FCCL was obtained after heating for 3 h in a vacuum oven at 160°C. The structure and dielectric properties of cured adhesive, surface morphology of peeling FCCL and mechanical properties of FCCL were determined. Findings – CTBN was found to react with the epoxy resin during the curing process, with the rubber phase being precipitated and dispersed in the epoxy matrix. The relative dielectric constant and the dielectric loss tangent slightly increased with increasing CTBN content. The peeling strength of FCCL increased accompanied by a decrease of folding resistance with the increase of 901 content. Further, with the addition of XNBR, the peel strength of FCCL increased, as well as the folding resistance of FCCL, but at a higher XNBR level of 20 weight per cent, the folding resistance of FCCL tended to decrease. Research limitations/implications – In the study reported here, the effects of different epoxy resin molecular weight and CTBN content were investigated. Results of this research could benefit in-depth understanding of the influence of epoxy resin molecular weight and CTBN content on adhesive performance and could further promote the development of epoxy adhesive. Practical implications – The adhesion of epoxy adhesive prepared from epoxy resin with different molecular weight and CTBN increased, leading to the increase in peeling strength and folding resistance of FCCL. Social implications – The peeling strength of FCCL increased as the adhesion strength of epoxy adhesive increased by adding CTBN, making FCCL widely applicable. Originality/value – The mechanical properties of epoxy adhesive were increased by adding CTBN. The effects of CTBN on the microstructure and properties of FCCL were discussed in detail.


Processes ◽  
2020 ◽  
Vol 9 (1) ◽  
pp. 42
Author(s):  
Stefano Merighi ◽  
Laura Mazzocchetti ◽  
Tiziana Benelli ◽  
Loris Giorgini

In order to obtain an environmentally friendly epoxy system, L-tryptophan and guanine were investigated as novel green curing agents for the cross-link of diglycidyl ether of Bisphenol A (DGEBA) as a generic epoxy resin model of synthetic and analogous bio-based precursors. In particular, L-tryptophan, which displays high reaction temperature with DGEBA, was used in combination with various bio-based molecules such as urea, theobromine, theophylline, and melamine in order to increase the thermal properties of the epoxy resin and to reduce the crosslinking reaction temperature. Later, in order to obtain similar properties using a single product, guanine, a totally heterocyclic molecule displaying amine functional groups, was tested as hardener for DGEBA. The thermal behavior of the precursor mixtures was evaluated by dynamic differential scanning calorimetry (DSC) leading to a preliminary screening of different hardening systems which offered a number of interesting hints in terms of bio-based compounds able to provide high Tg resins. These encouraging results pave the way for a further study of a new class of renewable, low-toxic, and sustainable curing agent systems for the production of fully bio-based epoxy resins.


2012 ◽  
Vol 24 (8) ◽  
pp. 730-737 ◽  
Author(s):  
Wang Fang ◽  
Xiao Jun ◽  
Wang Jing-wen ◽  
Li Shu-qin

A modified imidazole curing agent, EMI-g-BGE, was encapsulated for one-package of diglycidyl ether of bisphenol A (DGEBA) epoxy resin system. Polyetherimide (PEI) was used as the wall material, and the emulsion solvent evaporation method was used to form the microcapsules. The morphology and particle size distribution of microcapsules were evaluated by scanning electron microscopy (SEM), mastersizer analyzer. Microcapsules exhibited spherical shapes and the mean particle size was about 745 nm. The curing kinetic of DGEBA/microcapsules curing agent was studied by nonisothermal differential scanning calorimetry (DSC) technique at different heating rates. Dynamic DSC scans indicated the microcapsule was an effective curing agent of epoxy resin. The apparent activation energy Ea was 88.03 kJ/mol calculated through Kissinger method, more than DGEBA/EMI-g-BGE system. This microcapsule of EMI-g-BGE exhibited a long shelf life, and the curing did not occur in this epoxy-microcapsule resin system for more than 3months at room temperature. The kinetic parameters were determined by Málek method and a two-parameter ( m, n) autocatalytic model (Šesták–Berggren equation) was found to be the most adequate selected kinetic model, which showed the encapsulation of the curing agent EMI-g-BGE did not change the cure reaction mechanism of the epoxy resin system. From the experimental data, the nonisothermal DSC curves show the results being in accordant with those theoretically calculated.


2013 ◽  
Vol 634-638 ◽  
pp. 3008-3016
Author(s):  
Yan Li ◽  
Zhi Nan Zhou ◽  
Xiao Yan Xu ◽  
Long Xie

Two Novolac Resins Were Synthesized by the Reaction between Bisphenol A and Benzaldehyde (bis-BENR) or Bisphenol A and P-hydroxybenzaldehyde (bis-PHNR). Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR) Were Applied to Characterize the Molecular Structure of Bis-BENR (or Bis-PHNR). then the Two Novolac Resins Were Used as Curing Agent for Bisphenol A Type Epoxy Resin (DGEBA). the Curing Reaction and Curing Kinetics Were Studied by Dynamic FTIR and Differential Scanning Calorimetry (DSC). Dynamic FTIR Showed that the Two Novolac Resins Reacted with Epoxy Resins and Formed a Crosslinking Network Structure. DSC Results Show that the Optimum Mass Ratio between DGEBA and Bis-BENR (or Bis-PHNR) Was 7:3, under which the Curing Reaction Processed Completely. the Mechanical Properties and Sulfide Resistance of DGEBA/bis-BENR (or Bis-PHNR) System Were Also Investigated. the Results Showed that when the Mass Ratio between DGEBA and Bis-BENR (or Bis-PHNR) Was 7:3, the Curing Coatings Had Optimum Mechanical Properties and Sulfide Resistance.


2011 ◽  
Vol 109 ◽  
pp. 170-173
Author(s):  
Li Huo ◽  
Yong Gang Du ◽  
Yong Mei Wang

The cure kinetics for bisphenol A epoxy resin (BPAER) modified by liquid crystalline Sulfonyl bis(4,1-phenylene)bis[4-(2,3-epoxypropyloxy)benzoate](p-SBPEPB), with3-methyl-tetrahy drophthalic anhydride (MeTHPA) as a curing agent, were investigated by nonisothermal differential scanning calorimetry (DSC) method. The effect of the different liquid crystalline contents and activation energy (Ea) on curing reaction were discussed. The glass transition temperature (Tg) and mechanical property were charactered, The results show that the better content is about 10wt%.


Materials ◽  
2019 ◽  
Vol 12 (9) ◽  
pp. 1489 ◽  
Author(s):  
José William de Lima Souza ◽  
Nichollas Guimarães Jaques ◽  
Matthias Popp ◽  
Jana Kolbe ◽  
Marcus Vinícius Lia Fook ◽  
...  

Epoxy resin based on bisphenol A diglycidyl ether/anhydride methyl tetrahydrophthalic/2,4,6-tris(dimethylaminomethyl)phenol (DGEBA/MTHPA/DEH 35) was produced by magnetic stirring; chicken eggshell (ES) was added as cure improver. Thermal stability, cure parameters, mechanical properties, and fracture surface were investigated by thermogravimetry (TGA), differential scanning calorimetry (DSC), tensile experiments, and scanning electron microscopy (SEM). In general, the addition of ES slightly decreased the thermal stability, being T0.05 5% lower than that of the reference sample. The cure rate increased with the heating rates, while best results were obtained upon addition of neat membrane (M) from ES. Surprisingly, the mechanical properties were significantly improved with ES as well as with M, being the Young’s modulus 18% higher, the tensile strength 50% higher, and the deformation 35% higher than those of epoxy resin. SEM images showed that the synthetic compounds presented a smooth fracture surface, while the compounds with ES and M had a rougher surface with multiplane fractures, suggesting a fracture with higher energy absorption. In conclusion, epoxy/ES composites with better performance were produced, and effective tools are provided to control and attain in the future even better properties with ecological features.


2011 ◽  
Vol 146 ◽  
pp. 160-169 ◽  
Author(s):  
A. Stan ◽  
I. Dinca ◽  
C. Ban ◽  
S. Ilina ◽  
Dan Donescu ◽  
...  

The paper deals with the rheological properties of epoxy resin additivated with organically modified montmorillonites, carbon nanotubes and nanocarbon. The paper also presents the influence of nanoadditives over composites mechanical properties. The epoxy polymer is diglycidyl ether of bisphenol A (DGEBA) and the curing agent is an aliphatic tetraamine. Organically modified montmorillonites Cloisite 30B and Cloisite 93A, MWCNTs and laser synthesized nanocarbon were used to synthesize nanocomposites by dispersing each in an epoxy resin. The dispersion was achieved through mechanical and sonic methods. The epoxy resin additivated with nanosized fillers was rheologically tested to study the dispersion influence. The sonic dispersion of nanoadditives is observed to drastically influence the rheological behavior of the suspensions. Newtonian fluid behavior disappears as the additive loading increases. The work mentions the influence of nanoadditives on the manufacturing process of epoxy /glass fibre and epoxy/ carbon fibre laminated composites.


2014 ◽  
Vol 775-776 ◽  
pp. 588-592
Author(s):  
Camila Rodrigues Amaral ◽  
Ruben Jesus Sanchez Rodriguez ◽  
Magno Luiz Tavares Bessa ◽  
Verônica Scarpini Cândido ◽  
Sergio Neves Monteiro

The correlation between the structural network of a diglycidyl ether of the bisphenol-A (DGEBA) epoxy resin, modified by two distinct aliphatic amines (tetraethylenepentamine TEPA and jeffamine D230), and its mechanical properties, was investigated as possible matrix for abrasive composites applications. Both flexural tests, to determine the yield stress and the elastic modulus, as well as impact tests to determine the notch toughness, were performed. The DGEBA/D230 presented the highest stiffness and toughness but lowest yield stress. This epoxy network also displayed a greater plastic deformation during fracture.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Ali Kuliaei ◽  
Iraj Amiri Amraei ◽  
Seyed Rasoul Mousavi

Abstract The purpose behind this research was to determine the optimum formulation and investigate the cure kinetics of a diglycidyl ether of bisphenol-A (DGEBA)-based epoxy resin cured by dicyandiamide and diuron for use in prepregs. First, all formulations were examined by the tensile test, and then, the specimens with higher mechanical properties were further investigated by viscometry and tack tests. The cure kinetics of the best formulation (based on tack test) in nonisothermal mode was investigated using differential scanning calorimetry at different heating rates. Kissinger and Ozawa method was used for determining the kinetic parameters of the curing process. The activation energy obtained by this method was 71.43 kJ/mol. The heating rate had no significant effect on the reaction order and the total reaction order was approximately constant ( m + n ≅ 2.1 $m+n\cong 2.1$ ). By comparing the experimental data and the theoretical data obtained by Kissinger and Ozawa method, a good agreement was seen between them. By increasing the degree of conversion, the viscosity decreased; as the degree of conversion increased, so did the slope of viscosity. The results of the tack test also indicated that the highest tack could be obtained with 25% progress of curing.


Author(s):  
Abbas Hassan Faris

In this work, appropriate alternative for diglycidyl ether bisphenol A (DGEBA) was found to avoid the destructive effects of bisphenol A. Lignin, an aromatic compound from palm tree leaves, was used as a renewable material to synthesize a bio-based epoxy resin. Lignin extracted using Kraft pulping process. Kraft Lignin was epoxidized with epichlorohydrin in alkaline medium. Nano-titanium dioxide was used as filler with ratio of 10% to prepare the green epoxy composite. The structure of the Kraft lignin and lignin-based epoxy resin was proven via Infrared spectra (FT-IR) were recorded using solid KBr disk by testing Shimadzu (FT-IR-8300) spectrophotometer. The thermal properties of the curing process of lignin-based epoxy resin and composite were investigate using Differential scanning calorimetry (DSC) analysis. Potentiodynamic measurements data revealed that the anti-corrosion performance of the lignin based epoxy resin. The study demonstrates successful of epoxidation of Kraft lignin. In addition, lignin based eopxy resin showed effective inhibitor for carbon steel in 3.5 wt. % NaCl electrolyte solutions


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