scholarly journals Preparation and Characterization of Microencapsulated Ethylenediamine with Epoxy Resin for Self-healing Composites

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Liye Yuan ◽  
Tongqing Sun ◽  
Honglin Hu ◽  
Shuxia Yuan ◽  
Yu Yang ◽  
...  
Keyword(s):  
Epoxy Resin ◽  
Interfacial Polymerization ◽  
Silicone Oil ◽  
Optical Microscope ◽  
Self Healing ◽  
Scanning Calorimetry ◽  
Oil Emulsion ◽  
Factors Affecting ◽  
Healing Agent ◽  
Water In Oil Emulsion

AbstractHealing agent microcapsules have been used to realize self-healing for polymeric composites. In this work a novel kind of microcapsules encapsulating ethylenediamine (EDA) with epoxy resin as shell material were prepared by interfacial polymerization technology. The oil phase was epoxy resin prepolymer and carbon tetrachloride, and the water phase was EDA and deionized water. Under the action of emulsifier, a stable water-in-oil emulsion was formed. Then the emulsion was added to dimethyl silicone oil, stirred and dispersed, to prepare microcapsules. In addition, the factors affecting the preparation of microcapsules were studied. In this study, Fourier transform infrared(FTIR) was carried out to demonstrate the chemical structure of ethylenediamine microcapsules. Optical microscope(OM) and scanning electron microscope(SEM) were used to observe the morphology of microcapsules. Thermogravimetric analysis and differential scanning calorimetry were done to investigate the thermal properties of microcapsules. Permeability experiment and isothermal aging test were executed to verify the environment resistance of microcapsules. Results showed that EDA was successfully coated in epoxy resin and the microcapsule size was in the range of 50~630 μm. The synthesized microcapsules were thermally stable below 75 °C and perfect permeability resistance to ethanol solvent.

Synthesis and Self-Healing Mechanism of Self-Healing Epoxy Microcapsule Materials

2020 ◽  
Vol 842 ◽  
pp. 3-9
Author(s):  
Zhuo Ni ◽  
Zhen Guo ◽  
Yu Hao Lin
Keyword(s):  
Epoxy Resin ◽  
Interfacial Polymerization ◽  
Curing Temperature ◽  
Future Research ◽  
Self Healing ◽  
Practical Applications ◽  
The Core ◽  
Good Surface ◽  
Core Content ◽  
Wall Materials

Self-healing epoxy resin microcapsules are prepared by interfacial polymerization, in which the core materials are epoxy resin, the wall materials are constructed with triethylenetetramine and the epoxy resin. The orthogonal experimental L9(34) are designed to investigate the influence of emulsifier dosage, hardener dosage, curing temperature and hardener adding rate on the core content and storage life of epoxy resin microcapsule. Scanning electron microscope is used to characterize surface topography and distribution. Fourier transform infrared spectroscopy is used to study reaction mechanism of the microcapsule wall materials, respectively. The results indicate that when the dosage of emulsifier is 1.2%, the dosage of hardener is 1.2%, the hardener droplets adding rate is 1.2 g/h and the curing temperature is 50°C, the prepared microcapsules with a high level of core content are spherical in shape with good surface compactness and dispersibility. Future research may focus on improving microcapsule storage stability and the obstacles encountered in practical applications.

Melamine Resin-Walled Microcapsules Containing Styrene: Preparation and Characterization

2008 ◽  
Vol 47-50 ◽  
pp. 286-289 ◽  
Author(s):  
Hai Ping Wang ◽  
Yan Chao Yuan ◽  
Min Zhi Rong ◽  
Ming Qiu Zhang
Keyword(s):  
In Situ Polymerization ◽  
Weight Ratio ◽  
Processing Parameters ◽  
Optical Microscope ◽  
Resonance Spectroscopy ◽  
Self Healing ◽  
Melamine Formaldehyde ◽  
Scanning Calorimetry ◽  
Water Emulsion ◽  
Core Content

For purposes of developing a novel self-healing chemistry for polymer composites, melamine-formaldehyde (MF) resin-walled microcapsules containing styrene were prepared by in-situ polymerization in an oil-in-water emulsion. Chemical structure of the microcapsules was identified by Fourier-transform infrared spectroscopy (FTIR) and proton magnetic resonance spectroscopy (1H NMR), respectively. In addition, scanning electron microscope (SEM) and optical microscope (OM) were used to investigate morphology and geometry of the product. The effects of dispersion rate, weight ratio of core to shell and emulsifier concentration were carefully analyzed. It was found that poly(melamine-formaldehyde) (PMF) microcapsules containing styrene were successfully synthesized through the proposed technical route, and their mean diameters fall in the range of 20~71 µm. The rough surface of the microcapsules is composed of agglomerated PMF nanoparticles. Both core content and size of the microcapsule can be adjusted by selecting different processing parameters. The highest loading of styrene in the capsules is about 60% and the emulsifier with lower molecular weight used to result in higher core content. In terms of differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), thermal behavior and storage stability of the capsules were studied. The results indicated that the microcapsules can be handled up to 72 oC.

scholarly journals Robust synthesis of epoxy resin-filled microcapsules for application to self-healing materials

2016 ◽  
Vol 374 (2061) ◽  
pp. 20150083 ◽  
Author(s):  
Patryk A. Bolimowski ◽  
Ian P. Bond ◽  
Duncan F. Wass
Keyword(s):  
Epoxy Resin ◽  
Size Distribution ◽  
Fibre Composite ◽  
Diglycidyl Ether ◽  
High Yield ◽  
Self Healing ◽  
Carbon Fibre Composite ◽  
Scanning Calorimetry ◽  
Water Emulsion ◽  
Oil In Water Emulsion

Mechanically and thermally robust microcapsules containing diglycidyl ether bisphenol A-based epoxy resin and a high-boiling-point organic solvent were synthesized in high yield using in situ polymerization of urea and formaldehyde in an oil-in-water emulsion. Microcapsules were characterized in terms of their size and size distribution, shell surface morphology and thermal resistance to the curing cycles of commercially used epoxy polymers. The size distribution of the capsules and characteristics such as shell thickness can be controlled by the specific parameters of microencapsulation, including concentrations of reagents, stirrer speed and sonication. Selected microcapsules, and separated core and shell materials, were analysed using thermogravimetric analysis and differential scanning calorimetry. It is demonstrated that capsules lose minimal 2.5 wt% at temperatures no higher than 120°C. These microcapsules can be applied to self-healing carbon fibre composite structural materials, with preliminary results showing promising performance.

scholarly journals Experimental Investigation of a Novel Formulation of a Cyanoacrylate-Based Adhesive for Self-Healing Concrete Technologies

2021 ◽  
Vol 7 ◽  
Author(s):  
Cristina De Nardi ◽  
Diane Gardner ◽  
Giulia Cazzador ◽  
Davide Cristofori ◽  
Lucio Ronchin ◽  
...  
Keyword(s):  
Bond Strength ◽  
Shelf Life ◽  
Sessile Drop ◽  
Cement Mortar ◽  
Self Healing ◽  
Vascular Networks ◽  
Concrete Technology ◽  
Scanning Calorimetry ◽  
Liquid Form ◽  
Healing Agent

The selection of an appropriate healing agent is critical to the success of vascular and mini-vascular networks. In self-healing concrete technology, commercially available cyanoacrylate (CA) adhesives have been shown to produce good strength recoveries; however, their rapid curing rate and short shelf-life make them unsuitable for site application. The aim of this study was to develop a modified cyanoacrylate (n-CA) with an extended shelf-life suitable for incorporation in a self-healing system. A series of n-CAs were formed from a commercial Ethyl Cyanoacrylate adhesive mixed with acrylic acid (AA) and nitro-anthraquinone (nAq) in varying ratios. When encapsulated within 3D printed mini-vascular networks (MVNs), the n-CAs remained dormant in liquid form for up to 5 days. The contact angle between the n-CAs and the cement mortar substrate, as measured via the sessile drop technique, decreased significantly with increasing AA content. The mechanical properties (bond strength) and the polymerization hardening of the n-CAs were evaluated over a curing period of 7–21 days, via a series of pull-off tests using cement mortar cubes. The 4:1:02 (CA:AA:nAq) n-CA formulation showed a significant increase in bond strength from 14 to 21 days, with a ceiling value of 2.6 MPa, while the 2:1 (CA:AA) n-CA formulation exhibited a good bond strength after 21 days (1 MPa). Nuclear Magnetic Resonance (NMR) conducted on the n-CAs suggested the formation of several new polymeric species, whilst differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) on the pre- and post-printed MVN material confirmed no significant changes in chemistry with no evidence of polymer degradation. Considered together, the experimental results show the potential for different n-CA formulations to act efficiently as a healing agent.

scholarly journals Preparation and Characterization of Nano-CaCO3/Ceresine Wax Composite Shell Microcapsules Containing E-44 Epoxy Resin for Self-Healing of Cement-Based Materials

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 197
Author(s):  
Wei Du ◽  
Erwang Li ◽  
Runsheng Lin
Keyword(s):  
Epoxy Resin ◽  
Recovery Rate ◽  
Composite Shell ◽  
Chloride Ion ◽  
Self Healing ◽  
The Core ◽  
Core Content ◽  
Cement Based Materials ◽  
Healing Agent ◽  
Melt Condensation

As an intelligent material, microcapsules can efficiently self-heal internal microcracks and microdefects formed in cement-based materials during service and improve their durability. In this paper, microcapsules of nano-CaCO3/ceresine wax composite shell encapsulated with E-44 epoxy resin were prepared via the melt condensation method. The core content, compactness, particle size distribution, morphologies, chemical structure and micromechanical properties of microcapsules were characterized. The results showed that the encapsulation ability, mechanical properties and compactness of microcapsules were further improved by adding nano-CaCO3 to ceresine wax. The core content, elastic modulus, hardness and weight loss rate (60 days) of nano-CaCO3/ceresine wax composite shell microcapsules (WM2) were 80.6%, 2.02 GPA, 72.54 MPa and 1.6%, respectively. SEM showed that WM2 was regularly spherical with a rough surface and sufficient space inside the microcapsules to store the healing agent. The incorporation of WM2 to mortar can greatly improve the self-healing ability of mortar after pre-damage. After 14 days of self-healing, the compressive strength recovery rate, proportion of harmful pores and chloride ion diffusion coefficient recovery rate increased to 90.1%, 45.54% and 79.8%, respectively. In addition, WM2 also has good self-healing ability for mortar surface cracks, and cracks with initial width of less than 0.35 mm on the mortar surface can completely self-heal within 3 days.

scholarly journals Preparation and Characterization of Microcrystalline Wax/Epoxy Resin Microcapsules for Self-Healing of Cementitious Materials

Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1725
Author(s):  
Wei Du ◽  
Quantao Liu ◽  
Runsheng Lin ◽  
Xin Su
Keyword(s):  
Epoxy Resin ◽  
Size Distribution ◽  
Weight Ratio ◽  
Cementitious Materials ◽  
Self Healing ◽  
Surface Cracks ◽  
Preparation Temperature ◽  
Core Content ◽  
Healing Agent

Self-healing of cracks in cementitious materials using healing agents encapsulated in microcapsules is an intelligent and effective method. In this study, microcapsules were prepared by the melt–dispersion–condensation method using microcrystalline wax as the shell and E-51 epoxy resin as the healing agent. The effects of preparation process parameters and microcrystalline wax/E-51 epoxy resin weight ratio on the core content, particle size distribution, thermal properties, morphology, and chemical composition of microcapsules were investigated. The results indicated that the optimal parameters of the microcapsule were microcrystalline wax/E-51 epoxy resin weight ratio of 1:1.2, stirring speed of 900 rpm, and preparation temperature of 105 °C. The effects of microcapsules on pore size distribution, pore structure, mechanical properties, permeability, and ultrasonic amplitude of mortar were determined, and the self-healing ability of mortar with different contents of microcapsules was evaluated. The optimal content of microcapsules in mortars was 4% of the cement weight, and the surface cracks of mortar containing microcapsules with an initial width of 0.28 mm were self-healed within three days, indicating that microcapsules have excellent self-healing ability for cementitious materials.

Microencapsulation of Liquid Cyanoacrylate via In situ Polymerization for Self-healing Bone Cement Application

2012 ◽  
Vol 1417 ◽  
Author(s):  
Vineela D. Gandham ◽  
Alice B.W. Brochu ◽  
William M. Reichert
Keyword(s):  
Bone Cement ◽  
Interfacial Polymerization ◽  
In Situ Polymerization ◽  
Tissue Adhesive ◽  
Material System ◽  
Self Healing ◽  
Pmma Bone Cement ◽  
Polyethylene Glycol 200 ◽  
Healing Agent

ABSTRACTStructural polymers are susceptible to accumulated damage in the form of internal microcracks that propagate through the material, resulting in mechanical failure. Self- healing approaches offer a solution to repair these damages automatically. The first generation self-healing material system includes a microencapsulated healing agent within a catalyst-embedded matrix. Propagating microcracks rupture the microcapsules, releasing the liquid healing agent into the damaged region. Catalyst-triggered polymerization of the released healing agent repairs the damage. Our research focuses on a similar approach for addressing “damage accumulation failure” of poly(methyl methacrylate) (PMMA) bone cement caused by microcrack initiation and propagation. In this study, polyurethane (PU) microcapsules containing a tissue adhesive, 2-octylcyanoacrylate (OCA) were synthesized using in situ interfacial polymerization of toluene-2,4-diisocynate (TDI) and polyethylene glycol 200 (PEG 200) through an oil-in-oil-in-water microemulsion (o/o/w). The process was optimized by studying different combinations of organic solvents, surfactants, temperatures, agitation rates, pH, and reaction times and their effects on microencapsulation were observed. Microcapsule surface morphology, size, shell thickness, encapsulated OCA viability, thermal degradation, and chemical structure of the microcapsule shell were evaluated using a stereoscope, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and fourier transform infrared spectroscopy (FT-IR).

Self-Healing Mortar

2019 ◽  
pp. 135-148
Keyword(s):  
Epoxy Resin ◽  
Ultrasonic Pulse Velocity ◽  
Ultrasonic Pulse ◽  
Pulse Velocity ◽  
Experimental Program ◽  
Self Healing ◽  
Repair Materials ◽  
Healing Agent ◽  
The Cost ◽  
Initial Reading

The cost of repairing cracked concrete is expensive as it requires special repair materials and skilled labour. Thus, the developments of new materials, like self-healing materials, are highly needed to repair cracks automatically and to restore or even increase concretes' strength to prolong its service life. The aim of this chapter was to investigate the performance of epoxy resin without hardener as a self-healing agent in mortar. A detailed introduction of self-healing mortar is given followed by a problem statement. The epoxy resin as a self-healing material is also explained briefly. Self-healing concept is also discussed in detail followed by the experimental program. Results revealed that the epoxy resin without hardener as a healing agent performed effectively as the compressive strength and ultrasonic pulse velocity of 365 days old cracked mortar samples regained the initial reading with prolonged curing time.

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