Curing Reaction Of Epoxy Resin Research Articles

Glycine-Ti3C2Tx Hybrid Material Improves the Electrochemical Corrosion Resistance of a Water-Borne Epoxy Coating.

Improving the dispersibility and compatibility of nanomaterials in water-borne epoxy resins is an important means to improve the protection ability and corrosion resistance of coatings. In this study, glycine-functionalized Ti3C2Tx (GT) was used to prepare an epoxy composite coating. The results of Fourier transform infrared spectroscopy and X-ray diffraction showed that glycine was successfully modified. The scanning electron microscopy and transmission electron microscopy results showed that the aggregation of Ti3C2Tx was alleviated. Electrochemical impedance spectroscopy test results show that, after 60 days of immersion, GT coating still shows the best protection performance, and the composite coating |Z|f = 0.01 Hz is 3 orders of magnitude higher than that of the pure epoxy coating. This is mainly because, after adding glycine, the -COOH group on the surface of glycine binds to the -OH group on the surface of Ti3C2Tx, improving the aggregation of Ti3C2Tx itself. At the same time, the -NH group of glycine can also participate in the curing reaction of epoxy resin to strengthen the bonding strength between the coating and the metal. The good dispersion of GT in epoxy resin makes it fill the pores and holes left by epoxy resin curing and strengthen the corrosion resistance. The easy availability and green properties of glycine provide a simple and environmentally friendly method for the modification of Ti3C2Tx.

Improving flame retardancy in BADGE epoxy via novel phosphorus‐functionalized epoxy integration

AbstractA novel epoxy resin, DPHP, was synthesized from diphenolic acid, which contains biobased levulinic acid, with triethylphosphite, to improve the flame retardancy of bisphenol‐A diglycidyl ether (BADGE) epoxy. Curing experiments were conducted using isophorone diamine as a curing agent for BADGE and DPHP mixtures. Variations in cure kinetics, mechanical properties, and flame retardancy were evaluated across different DPHP contents. The introduction of phosphorus functional groups into DPHP affected the polarization of epoxide CO bonds, resulting in reduced apparent activation energy for epoxy curing reactions. However, the higher epoxy equivalent weight of DPHP compared with that of BADGE led to a decrease in the tensile strength and the glass transition temperature of the cured material with increasing DPHP content. A significant increase in char yield for combustion of the epoxy blend was observed, ranging from 8.3% at 0 wt% DPHP to 20.1% at 50 wt% DPHP. Additionally, cone calorimeter measurements showed significant reductions in heat release rate and total heat release, leading to a decrease in fire spread from 1.07 MJm−2 s−1 at 0 wt% DPHP to 0.43 MJm−2 s−1 at 50 wt% DPHP. These results show that the flame retardancy of the cured material improved significantly as the DPHP content increased.

Evaluation of the curing reaction of epoxy resins by electrochemical measurement and molecular orbital method

Epoxy resin is a thermosetting resin with excellent mechanical properties. It has been pointed out that there are problems on its mechanical properties due to poor polymerization of the epoxy ring caused by water and chlorine impurities during resin production. In this study, we focused on the electrochemical behavior during curing reaction of epoxy resin. To investigate the electrochemical reaction, galvanostat meter was used to measure the voltage behavior during chemical reaction. Molecular Orbital (MO) method was used to understand the mechanisms of voltage behavior during curing reaction. Furthermore, the effect of water existence during curing reaction was investigated by experimentally and analytically. As a result of experimental electrochemical reaction, we successfully measured the voltage behavior associated with the curing reaction. In the case of MO analysis, the epoxy and curing agent models were prepared. Before the reaction, each molecule had zero charge, but after the reaction, it was confirmed that the epoxy had a positive charged and the amine had a negative charged. It is thought that the voltage could be observed due to the movement of this charge during curing reaction. It has been also demonstrated through experimentation and analysis that water accelerates the curing reaction. It was observed that the accelerating effect amplifies as the quantity of water increases. Building upon these results, it was confirmed that the factor leading to the increase in voltage is due to the amount of water. To examine the presence of chlorine impurities during the production of epoxy resin, MO analysis was conducted on the production reaction of epoxy prepolymers. The findings indicated that as the water content increases, the reaction that results in the production of by-products is amplified. This outcome suggested that by-products were already incorporated during the formation of the epoxy. In conclusion, this study provides significant insights into the electrochemical behavior during the curing reaction of epoxy resin, the role of water in accelerating the reaction, and the impact of chlorine impurities during resin production. The findings pave the way for further research to optimize the production process and enhance the mechanical properties of epoxy resin.

Modification mechanism of modified diatomite with flexible amine‐based structure as a filler of epoxy resin and mechanical properties and curing kinetic of composites

AbstractIn this study, the binding of amine‐based hyperbranched macromolecular polyethyleneimine (PEI) to diatomite (DE) was carried out by using the silane coupling agent KH560 (PEI‐KH560‐DE). Fourier infrared spectroscopy, scanning electron microscopy were used to characterize the structure of the modified DE. Then, the composites were prepared using PEI‐KH560‐DE as the filler in the epoxy resin matrix and then cured with dimethylimidazole. The cured composites were tested for impact resistance, flexural properties, and tensile properties, and then subjected to DSC. The experimental results showed that when different proportions of diatomite or modified diatomite were added to the epoxy resin matrix, the strength and toughness of the composites could be significantly enhanced. When the content of PEI‐KH560‐DE was 15 wt%, the impact strength of the composites reached the maximum value of 5.39 kJ/m2, which was 156.67% higher than that of the pure epoxy resin (2.10 kJ/m2). The tensile strength was also improved from 16.38 MPa of the pure epoxy resin to 26.55 MPa, corresponding to an increase of 62.09%. With the addition of modified diatomite, the Tdmax and char yield of the composites were significantly enhanced, indicating that the addition of diatomite can enhance the heat resistance and thermal stability of the composites. The curing kinetics study showed that the addition of PEI‐KH560‐DE can significantly reduce the apparent activation energy required for the curing reaction of epoxy resin probably due to the presence of amine group in PEI, which plays a role in promoting the curing behavior.Highlights Amine groups and flexible chain segments were introduced into diatomite. Mechanism of polyethyleneimine‐modified diatomite was investigated. Improved mechanical and thermal properties of PEI‐KH560‐DE/EP composites. Curing kinetics showed that amine groups reduce apparent activation energy.

Adhesion properties of the hybrid system made of laser-structured aluminium EN AW 6082 and CFRP by co-bonding-pressing process

ABSTRACT A parameter investigation for manufacturing a hybrid system through the prepreg pressing process was carried out within the scope of this work to achieve optimal adhesion properties. The hybrid specimen comprises an aluminium sheet of alloy EN AW 6082 in T6 condition and a thermoset Carbon Fibre Reinforced Plastics prepreg. The prepreg pressing process allows the curing reaction of epoxy resin and the joining process to occur simultaneously to avoid an additional bonding process step. The surface of the aluminium sheet was pretreated in advance using a pulsed Nd:YAG laser to enhance the bonding properties. In the first step, the shear edge tests investigated the adhesion properties achieved with different consolidation (temperature, time and pressure) and laser parameters. Then, 3-point bending tests were carried out to investigate the influence of the consolidation parameters on the mechanical properties of the Carbon Fibre Reinforced Plastics-laminate. In this way, the optimal parameter sets for manufacturing hybrid structures were determined.

A Parametric Model for the Analysis of the Impedance Spectra of Dielectric Sensors in Curing Epoxy Resins.

Observing the curing reaction of epoxy resins is a key to quality assurance in fibre composite production. The evaluation of electrical impedance spectra is an established monitoring method. Such impedance spectra contain the physical effects of dipole relaxation, ionic conduction and electrode polarisation, which shift to lower frequencies as curing progresses. In the early stage of the curing reaction, ionic conductivity and electrode polarisation dominate, and in the later stage of the curing reaction, dipole relaxation dominates. Due to the shift of the effects over several frequency decades, it makes sense to evaluate electrical impedance spectra not exclusively at one frequency but over an entire available frequency spectrum. The measured spectral raw data cannot be easily interpreted by a control algorithm and have to be mapped to simpler key indicators. For this purpose, a frequency-dependent model is proposed to address the aforementioned physical effects. With only five free parameters, measured spectra can be described with a relative error of only 2.3%. The shift of the occurring effects to lower frequencies necessitates switching the key indicator used in the progression of the cure reaction.

Improving the Heat Resistance and Flame Retardancy of Epoxy Resin Composites by Novel Multifunctional Cyclophosphazene Derivatives.

A novel multiple-ring molecule containing P and N, called HCCP-SA, was successfully prepared by the nucleophilic substitution reaction of salicylamide (SA) and hexachlorocyclotriphosphazene (HCCP). Particularly, HCCP-SA possessed the dual functions of heat resistance and flame retardancy. The molecular structure of HCCP-SA was identified by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy. HCCP-SA was bonded into the molecular chain of epoxy resin by the ring-opening curing reaction of epoxy resin, aiming to form a heat-resistant and flame-retardant composite (E-HS-x). In particular, the best-prepared E-HS-x composite with a 20 phr content of HCCP-SA (E-HS-20) presented excellent thermal stability, with an initial decomposition temperature of 267.94 °C and a max weight loss speed of only 0.95 mg·min-1. Moreover, E-HS-20 exhibited remarkable flame retardancy with a limiting oxygen index value of 27.1% and a V-2 rating in the UL94 flame retardancy test. The best-prepared E-HS-20 composite would be a suitable and potential candidate for heat-resistant and flame-retardant polymer materials.

Hydroxyl-functionalized block co-polyimide enables simultaneously improved toughness and strength of tetrafunctional epoxy resin

Tetrafunctional epoxy resins are widely used as matrix of advanced composite materials due to their excellent high temperature performance. However, the highly crosslinking density of tetrafunctional epoxy resins results in an inherent brittleness, which limits its further application. In this work, hydroxyl-functionalized block co-polyimide (BPADA-ODA/HAB) is first synthesized by the condensation of 3,3′-Dihydroxybenzidine and 4,4′-Diaminodiphenyl ether with 4,4'-(4,4′-isopropylidenediphenoxy) di-phthalic anhydride, and used to toughen tetrafunctional epoxy resins. The co-polyimide molecules provide reactive blocks that participate in the curing reaction of epoxy resin and decrease the crosslinking density of epoxy resin; the co-polyimide can form nano-sized separated phase via self-assembly, which could activate additional energy dissipative mechanisms to enhance the resistance of failure for the epoxy resins. With 5% BPADA-ODA/HAB, the resultant epoxy resins exhibit simultaneous enhancements in impact strength and tensile strength, 184% and 150% higher than those of neat epoxy resin. This study provides an efficient method for preparing tough and strong tetrafunctional epoxy resins, which are expected to be applied more broadly in industries.

Comparison of Different Cure Monitoring Techniques.

The ability to measure the degree of cure of epoxy resins is an important prerequisite for making manufacturing processes for fibre-reinforced plastics controllable. Since a number of physical properties change during the curing reaction of epoxy resins, a wide variety of measurement methods exist. In this article, different methods for cure monitoring of epoxy resins are applied to a room-temperature curing epoxy resin and then directly compared. The methods investigated include a structure-borne sound acoustic, a dielectric, an optical and a strain-based observation method, which for the first time are measured simultaneously on one and the same resin sample. In addition, the degree of cure is determined using a kinetic resin model based on temperature measurement data. The comparison shows that the methods have considerable but well-explainable differences in their sensitivity, interference immunity and repeatability. Some measurement methods are only sensitive before and around the gel point, while the strain-based measurement method only reacts to the curing from the gel point onwards. These differences have to be taken into account when implementing a cure monitoring system. For this reason, a multi-sensor node is suitable for component-integrated curing monitoring, measuring several physical properties of the epoxy resin simultaneously.

Simultaneously reinforcing and toughening of shape-memory epoxy resin with carboxylated lignosulfonate: Facile preparation and effect mechanism

To improve the compatibility and reactivity of lignosulfonate (LS) with epoxy oligomers, the LS was firstly functionalized with anhydride via the carboxylation reaction. The carboxylated lignosulfonate (CLS) reinforced epoxy resin with excellent mechanical and shape memory performance was prepared facilely via distributing the CLS into the combined epoxy monomers of DGEBA and PEGDGE with the aid of water, rather than using the normal organic solvents. The incorporated CLS promoted the curing reaction of epoxy resin. A typical sea-island structure was formed in the cured sample at the CLS content of 5 phr, exhibiting the highest increases in tensile strength, modulus, elongation at break and toughness by 23.8 %, 18.2 %, 217 % and 113 %, respectively, relative to neat epoxy. Interestingly, the incorporation of CLS at a proper amount led to the simultaneous strengthening and toughing effects on cured epoxy resin, which could be attributed to the rigid structure of CLS covalently introduced in the epoxy resin network and the heterogeneous structure formed in the epoxy matrix. The rigid CLS component also restrained the movement of chain segments, consequently, the mechanical stability was enhanced and the fast shape recovery rate of epoxy resin network was slowed down to some extent.

Laboratory development and evaluation of an oleylamine curing Epoxy Asphalt

ABSTRACT There are still some deficiencies in the development and applications of epoxy asphalt materials, and the chemistry and curing mechanism of epoxy asphalt materials remain unknown. Based on the curing mechanism of commercial epoxy asphalt, an oleylamine curing epoxy asphalt (OCEA) material was prepared, and it was systematically described from the perspective of engineering application and reaction mechanism. The viscosity properties of OCEA were mainly used to predict its reserved time range and temperature during construction. The tensile properties of OCEA and commercial epoxy asphalt are evaluated to show the mechanical properties. The fluorescence microscopy and infrared spectroscopy of the OCEA were analyzed to understand its micromorphology and curing mechanism, and its current advantages are further explained in combination with the tensile properties of OCEA. The results show that the OCEA has the advantage of high strength and toughness. The asphalt phase can participate in the curing reaction of epoxy resin, enhancing the miscibility between constituents, which further enhances the miscibility of the asphalt binder and epoxy resin. This study can provide new materials for engineering epoxy asphalt and implications for further research on epoxy asphalt materials.

Cure Kinetics of Samarium-Doped Fe3O4/Epoxy Nanocomposites

To answer the question “How does lanthanide doping in iron oxide affect cure kinetics of epoxy-based nanocomposites?”, we synthesized samarium (Sm)-doped Fe3O4 nanoparticles electrochemically and characterized it using Fourier-transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-Ray analysis (EDX), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy analyses (XPS). The magnetic particles were uniformly dispersed in epoxy resin to increase the curability of the epoxy/amine system. The effect of the lanthanide dopant on the curing reaction of epoxy with amine was explored by analyzing differential scanning calorimetry (DSC) experimental data based on a model-free methodology. It was found that Sm3+ in the structure of Fe3O4 crystal participates in cross-linking epoxy by catalyzing the reaction between epoxide rings and amine groups of curing agents. In addition, the etherification reaction of active OH groups on the surface of nanoparticles reacts with epoxy rings, which prolong the reaction time at the late stage of reaction where diffusion is the dominant mechanism.

Real-Time Monitoring Polymerization Reactions Using Dipolar Echoes in 1H Time Domain NMR at a Low Magnetic Field.

1H time domain nuclear magnetic resonance (1H TD-NMR) at a low magnetic field becomes a powerful technique for the structure and dynamics characterization of soft organic materials. This relies mostly on the method sensitivity to the 1H-1H magnetic dipolar couplings, which depend on the molecular orientation with respect to the applied magnetic field. On the other hand, the good sensitivity of the 1H detection makes it possible to monitor real time processes that modify the dipolar coupling as a result of changes in the molecular mobility. In this regard, the so-called dipolar echoes technique can increase the sensitivity and accuracy of the real-time monitoring. In this article we evaluate the performance of commonly used 1H TD-NMR dipolar echo methods for probing polymerization reactions. As a proof of principle, we monitor the cure of a commercial epoxy resin, using techniques such as mixed-Magic Sandwich Echo (MSE), Rhim Kessemeier—Radiofrequency Optimized Solid Echo (RK-ROSE) and Dipolar Filtered Magic Sandwich Echo (DF-MSE). Applying a reaction kinetic model that supposes simultaneous autocatalytic and noncatalytic reaction pathways, we show the analysis to obtain the rate and activation energy for the epoxy curing reaction using the NMR data. The results obtained using the different NMR methods are in good agreement among them and also results reported in the literature for similar samples. This demonstrates that any of these dipolar echo pulse sequences can be efficiently used for monitoring and characterizing this type of reaction. Nonetheless, the DF-MSE method showed intrinsic advantages, such as easier data handling and processing, and seems to be the method of choice for monitoring this type of reaction. In general, the procedure is suitable for characterizing reactions involving the formation of solid products from liquid reagents, with some adaptations concerning the reaction model.

Dynamic Mechanical and Chemorheology Analysis for the Blended Epoxy System with Polyurethane Modified Resin

As the important matrix material, epoxy resin has been widely used in the composites for various fields. On account of the poor toughness of epoxy resin limiting their suitability for advanced applications, considerable interests have been conducted to modify the epoxy resin to meet the engineering requirements. In this study, the bio-based polyurethane (PU) modified resin was adopted to modify the pure bisphenol-A epoxy by blending method with various proportions. Aiming to illuminate the curing behavior, mechanical and thermal properties, the blended epoxy systems were characterized by viscosity-time analysis, dynamic mechanical analysis (DMA) at different frequencies and temperatures, mechanical tensile test, thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopy. The results indicated that the introduction of PU modified epoxy was found to significantly inhibit the viscosity growth rates especially when the content of PU modified epoxy resin is higher than 60%. Notwithstanding the dynamic modulus and Tg reduced with the increment of PU modified epoxy, remarkable increment on the elongation at break was found and the flexibility was greatly promoted with the introduction of PU modified epoxy. The proportion of PU modified epoxy in the blends should be put balance considerations to obtain optimal mechanical properties. TGA results and FTIR spectrum demonstrated that the addition of PU modified epoxy did not change the thermal decomposition mechanism and chemical reaction mechanism, but the addition of PU modified epoxy inhibits the curing reaction of epoxy resin by measured and calculated the damping temperature domain ΔT from 35.7°C to 48.9°C.

Enhanced thermal conductivity of epoxy composites via bridged Al2O3 network with in situ formed silver nanoparticles

AbstractIt is of great significance to achieve excellent thermal conduction for polymer composites in electrical insulation application. However, traditional polymer composites exhibit limited thermal conduction due to the absence of efficient heat transfer pathways. Herein, Al2O3 microspheres absorbed with silver acetate (AgAc) and 2‐ethyl‐4‐methylimidazole (2E4MI) complex were prepared as fillers for constructing heat transfer paths in epoxy composites. At a suitable temperature, 2E4MI was released from Ag(2E4MI)2Ac complex and initiated the curing reaction of epoxy. Simultaneously, nano silver ions were reduced, sintered in situ and then bridged separate Al2O3 microspheres to 3D filler network, which acted as thermal transport pathways in matrix. The thermal conductivity increased from 1.38 W/mK for Al2O3/epoxy composites to 2.62 W/mK for Al2O3@Ag(2E4MI)2Ac/epoxy composites at 60 vol% Al2O3 loading. Thanks to the 3D filler network, the tensile strength of Al2O3@Ag(2E4MI)2Ac/epoxy composites was obviously improved. Both the electrical resistivity and dielectric strength of the composites were basically preserved. Al2O3@Ag(2E4MI)2Ac/epoxy composites exhibit promising application in thermal management materials for advanced electric machinery and electronic devices.

Effect of Cross-Linking Density on Horizontal and Vertical Shift Factors in Linear Viscoelastic Functions of Epoxy Resins

Epoxy resins are an important class of thermosetting resins, and their network structure, obtained by the curing reaction of epoxy and amine compounds, plays an important role in the material properties. We here revisited a time–temperature superposition (TTS) principle applied to the dynamic viscoelastic functions of epoxy resins, in which the network was well defined and systematically varied on the basis of the length of n-alkyl diamine. The superimposition of isothermal curves in the frequency domain required not only a horizontal shift but also a vertical shift, regardless of the length of n-alkyl diamine. The temperature dependence of the horizontal shift factor, aT, could be well expressed by the Williams–Landel–Ferry equation. The fitting parameter, called C2, increased with decreasing alkyl chain length of the diamine, meaning that the thermal expansion of the free volume was suppressed due to greater cross-linking density. This was qualitatively confirmed by a full-atomistic molecular dynamics (MD) simulation. Meanwhile, the vertical shift factor, bT, increased with increasing temperature, and the extent was smaller with increasing cross-linking density. This can be explained in terms of the entropic contribution to the modulus in the temperature region above the glass transition temperature. The entropy change estimated using the isobaric molar heat capacity from the MD simulation strongly supported this hypothesis. The knowledge here obtained should be useful for a better design of thermosetting polymers as well as for the prediction of long-term durability.

Effect of a novel green modification of alumina nanoparticles on the curing kinetics and electrical insulation properties of epoxy composites

AbstractA novel green surface modification was successfully implemented on alumina nanoparticles using chitosan (CS) to prevent nanoparticles' aggregation. To evaluate the surface changes of nanoparticles, FTIR, TGA, TEM, and SEM analyses were used. The cure kinetics of the uncured samples was analyzed by DSC. Different methods such as KAS, Friedman, Starink, and FWO were applied to measure the activation energy. The activation energy of epoxy reinforced with chitosan‐functionalized alumina (epoxy/[CS‐EPO‐alumina]) was less than that of epoxy reinforced with alumina (epoxy/alumina), which was a confirmation of the positive effect of CS on curing reaction kinetics. Using the Malek method, the Sestak‐Berggren autocatalytic equation was chosen to investigate the cure kinetics of the epoxy. It was found that the Sestak‐Berggren equation is well matched with the experimental data and the model was suitable to predict the epoxy curing reaction reliably. Moreover, the glass transition temperatures of all samples were approximately the same. The effect of surface modification of alumina on the electrical insulating behavior of epoxy was also studied. It was found that CS functionalized alumina (CS‐EPO‐alumina) increased volume resistivity of epoxy at a temperature range of 30 to 80°C more than that of alumina. Electric stability and breakdown strength of epoxy/alumina and epoxy/(CS‐EPO‐alumina) also enhanced, where epoxy/(CS‐EPO‐alumina) experienced a further increase compared to epoxy.

New Insights on Expandability of Pre-Cured Epoxy Using a Solid-State CO2-Foaming Technique.

Foaming an epoxy is challenging because the process involves the curing reaction of epoxy and hardener (from monomer to oligomer, to a gel and a final three-dimensional crosslinked network) and the loading of gas phase into the epoxy phase to develop the cellular structure. The latter process needs to be carried out at the optimum curing stage of epoxy to avoid cell coalescence and to allow expansion. The environmental concern regarding the usage of chemical blowing agent also limits the development of epoxy foams. To surmount these challenges, this study proposes a solid-state CO2 foaming of epoxy. Firstly, the resin mixture of diglycidylether of bisphenol-A (DGEBA) epoxy and polyamide hardener is pre-cured to achieve various solid-state sheets (preEs) of specific storage moduli. Secondly, these preEs undergo CO2 absorption using an autoclave. Thirdly, CO2 absorbed preEs are allowed to free-foam/expand in a conventional oven at various temperatures; lastly, the epoxy foams are post-cured. PreE has a distinctive behavior once being heated; the storage modulus is reduced and then increases due to further curing. Epoxy foams in a broad range of densities could be fabricated. PreE with a storage modulus of 4 × 104–1.5 × 105 Pa at 30 °C could be foamed to densities of 0.32–0.45 g/cm3. The cell morphologies were revealed to be star polygon shaped, spherical and irregularly shaped. The research proved that the solid-state CO2-foaming technique can be used to fabricate epoxy foams with controlled density.

Experimental Study of High Performance Synchronous Grouting Materials Prepared with Clay.

Shield construction discharges a large amount of soil and muck. The utilization of discharged soil of shield always has high energy consumption and a low utilization rate. Meanwhile, synchronous grouting is a key process for shield tunneling. The current studies show that the synchronous grouting materials applied now generally have the problem of mismatching among filling property, fluidity, and consolidation strength. In order to study the feasibility of using the excavated soil produced by shield construction in clay stratum as synchronous grouting material, high performance synchronous grouting material was studied by taking red clay as an example, modified by epoxy resin. The fluidity, stability, and strength were measured to evaluate performance of the grout. Material test results show that the addition of waterborne epoxy resin decreases density, improves the stability, the rate of stone, and the toughness of the grouting concretion. Finally, X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) were measured to analyze the cementitious mechanism of the grout, test results demonstrated that cement hydration and curing reaction of epoxy resin happened in the grout, the formed polymer film filled the voids in the mixture and effectively bound cement hydration gel and clay particles together.

Synthesis of a novel lignin‐based epoxy resin curing agent and study of cure kinetics, thermal, and mechanical properties

AbstractIn this contribution, first of all, the methoxy groups of organic solvent lignin (OSL) was converted to phenolic hydroxyl groups through demethylation reaction for the purpose of fabricating demethylated organic solvent lignin (DOSL). In addition, the resulting DOSL was utilized as a renewable material to synthesize a novel esterified lignin (EDOSL) by reacting with isobutyryl chloride for curing of epoxy resin. Finally, commercial liquid diglycidyl ether of bisphenol A was cured by EDOSL in the presence of 4‐dimethylaminopyridine (DMAP) used as a catalyst based on dual‐curing mechanism. Dual curing is a processing methodology based upon the alliance of two diverse and compatible polymerization reactions occurring sequentially or simultaneously. According to the FTIR spectra and 1H‐NMR analyses, the demethylation of OSL, esterification of DOSL, and the curing reaction of epoxy resin with EDOSL were successfully conducted. The value of the phenolic hydrogen in the DOSL was approximately 4.89 mmol/g, which increased by 12.64% after demethylation. The thermal and mechanical performances of these cured epoxy samples were measured by DSC, DMA, TGA, and tensile testing. The epoxy system cured by 10%wt esterified lignin with 1%wt DMAP possessed the tensile strength of 71.54 ± 7.50 MPa and the initial degradation temperature (T5%) of 370°C, which can compete fairly with commercial aromatic curing agents or other lignin‐based agents studied currently for the curing of epoxy systems.