Optimization of preparation conditions of epoxy-containing nanocapsules

2017 ◽  
Vol 24 (1) ◽  
pp. 155-161 ◽  
Author(s):  
Xiulan Cai ◽  
Datian Fu ◽  
Ailan Qu

AbstractNanocapsules using epoxy and urea formaldehyde as core and shell materials, respectively, were prepared by in situ polymerization. The effects of processing conditions on the properties of epoxy nanocapsules were systematically investigated based on w(core) and average diameter of nanocapsules through the method of orthographic factorial design, and the optimum processing conditions were concluded. The results indicated that the key influencing factors on w(core) was agitation rate; on average, diameter of nanocapsules was emulsifier. The analysis of mechanical properties and thermal stability indicated that nanocapsules prepared in the optimum conditions are suitable for storage and the optimum content of nanocapsules was 10%. Scanning electron microscopy indicated that nanocapsules were well encapsuled and presented uniform spheres with rough surface. The broken nanocapsule indicated that the shell of the nanocapsule was thin and could coat more epoxy resin. The analysis of finite element method proved that nanocapsules prepared in the optimum conditions with an average of 110 nm shell thickness were suitable for self-healing materials.

2010 ◽  
Vol 143-144 ◽  
pp. 353-357
Author(s):  
Ting Ting Li ◽  
Xing Liu ◽  
Rui Wang

Healing agents significantly affect the efficiency of healing microcracks, which produced from life-time service in composites. And microencapsulating 5-ethylidene-2-norbornene (ENB) with Melamine-Urea-Formaldehyde (MUF) shell possessing higher self-healing efficiency is sensitive to the manufacture temperature profile which is difficult to control but crucial to the microcapsule performance and thus the reproducibility. In this paper, we studied the relationship between heating curve (rate, steps and time) and microcapsule performance (surface morphology, thermal stability and shell thickness). It shows that fast-slower heating stage produces the best quality of microcapsule with proper outer and inner surface which can endure 285°C, and the particle size is about 100m with 400-700nm shell thickness.


2010 ◽  
Vol 148-149 ◽  
pp. 1031-1035
Author(s):  
Yang Zhao ◽  
Wei Zhang ◽  
Le Ping Liao ◽  
Wu Jun Li ◽  
Yi Xin

With the development of the embedded microcapsule concept for self-healing material, the preparation of microcapsule has been paid more attentions. A new series of microcapsules were prepared by in situ polymerization technology in an oil-in-water emulsion with polyoxymethylene urea (PMU) as shell material and a mixture of epoxy resins as core material. The PMU microcapsules were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electronic microscopy (SEM), particle size analyzer and thermo gravimetric analyzer (TGA) to investigate their chemical structure, surface morphology, size distribution and thermal stability, respectively. The results indicate that PMU microcapsules containing epoxy resins can be synthesized successfully. The optimized reaction parameters were obtained as follow: agitation rate 600 rpm, 60°C water bath, pH=3.5, core material 20ml and hot water dilution by in-situ polymerization. The size is around 116 μm. The rough outer surface of microcapsule is composed of agglomerated PMU nanoparticles. The microcapsules basically exhibit good storage stability at room temperature, and they are chemically stable before the heating temperature is up to approximately 200°C.


Polymers ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 1918 ◽  
Author(s):  
Hyeong-Jun Jeoung ◽  
Kun Won Kim ◽  
Yong Jun Chang ◽  
Yong Chae Jung ◽  
Hyunchul Ku ◽  
...  

The mechanically-enhanced urea-formaldehyde (UF) microcapsules are developed through a multi-step in situ polymerization method. Optical microscope (OM) and field emission scanning electron microscope (FE-SEM) prove that the microcapsules, 147.4 μm in diameter with a shell thickness of 600 nm, are well-formed. From 1H-nuclear magnetic resonance (1H-NMR) analysis, we found that dicyclopentadiene (DCPD), a self-healing agent encapsulated by the microcapsules, occupies ca. 40.3 %(v/v) of the internal volume of a single capsule. These microcapsules are mixed with EPDM (ethylene-propylene-diene-monomer) and Grubbs’ catalyst via a solution mixing method, and universal testing machine (UTM) tests show that the composites with mechanically-enhanced microcapsules has ca. 47% higher toughness than the composites with conventionally prepared UF microcapsules, which is attributed to the improved mechanical stability of the microcapsule. When the EPDM/microcapsule rubber composites are notched, Fourier-transform infrared (FT-IR) spectroscopy shows that DCPD leaks from the broken microcapsule to the damaged site and flows to fill the notched valley, and self-heals as it is cured by Grubbs’ catalyst. The self-healing efficiency depends on the capsule concentration in the EPDM matrix. However, the self-healed EPDM/microcapsule rubber composite with over 15 wt% microcapsule shows an almost full recovery of the mechanical strength and 100% healing efficiency.


2013 ◽  
Vol 800 ◽  
pp. 471-475
Author(s):  
Wang Rui ◽  
Qian Jin Mao ◽  
Qi Dong Liu ◽  
Xiao Yu Ma ◽  
Su Ping Cui ◽  
...  

The self-healing polymer material which was embedded microcapsules possesses the ability to heal cracks automatically. The microcapsules were synthesized by in-situ polymerization in an oil-in-water emulsion with urea and formaldehyde as the raw shell material,and epoxy resin (E-51)/ xylene as the core material. The impact of stirring speed on the morphology and particle size of synthetic microcapsules were discussed by optical microscopy (OM), scanning electron microscopy (SEM), and Fourier-transform infrared spectrometer (FTIR).Microcapsules of 400~1500 um in diameter were produced by appropriate selection of agitation rate in the range of 300~600 r/min.


2014 ◽  
Vol 654 ◽  
pp. 11-15
Author(s):  
Xiu Lan Cai ◽  
Da Tian Fu ◽  
Ai Lan Qu

A series of microcapsules were prepared by interfacial polymerization method using epoxy and urea formaldehyde resin as core material and shell material, individually. The effects of processing conditions on the properties of epoxy microcapsules were systematically investigated based on w(Core), average diameter and decomposition temperature of microcapsules through the method of orthographic factorial design and the most optimum processing conditions were included. The results indicated that core/shell mass ratio was the most important factor on w(Core), average diameter and decomposition temperature of microcapsules. The optimum processing conditions were concluded: 1:1 for the core/shell mass ratio, 300 rpm for agitation rate and 0.8% DBS as emulsifier. The microcapsules prepare in the optimum processing conditions were well encapsuled and presented thin shell and smooth surface. Moreover, the addition of 10% microcapsules can improve the mechanical properties of epoxy matrix greatly.


2018 ◽  
Vol 7 (2) ◽  
pp. 147-159 ◽  
Author(s):  
Uday D. Bagale ◽  
Shirish H. Sonawane ◽  
Bharat A. Bhanvase ◽  
Ravindra D. Kulkarni ◽  
Parag R. Gogate

Abstract The present work deals with the production of nanocapsules containing a natural corrosion inhibition component. Azadirachta indica was encapsulated in urea-formaldehyde polymeric shell using ultrasound-assisted and conventional approaches of in situ polymerization. Subsequently nanocapsules were incorporated into clear epoxy polyamide to develop the green self-healing corrosion inhibition coating. The actual performance of the coating was evaluated based on the studies involving the repair of the crack of high solid surface coating. Corrosion inhibition of the healed area has been evaluated using the electrochemical impedance spectroscopy and immersion test based on the use of standard epoxy coating. The obtained results confirmed better corrosion protection in terms of the electrochemical impendence spectroscopy data and Tafel plot. It was found that current density decreases from 0.0011 A/cm2 (for standard epoxy coating) to 5.22 E−7 A/cm2 as 4 wt% nanocapsules incorporated in coating.


2018 ◽  
Vol 47 (3) ◽  
pp. 272-278 ◽  
Author(s):  
Amir Khalaj Asadi ◽  
Morteza Ebrahimi ◽  
Mohsen Mohseni

Purpose The purpose of this investigation is to develop a facile method to encapsulate a sunlight-curable silicone-based resin into a melamine–urea–formaldehyde (MUF) shell in the presence of polyvinylpyrrolidone (PVP) as an emulsifier. These microcapsules can be used in self-healing coating formulations. Design/methodology/approach MUF microcapsules containing a sunlight-curable core (methacryloxypropyl-terminated polydimethylsiloxane, MAT-PDMS) have been fabricated by means of in situ polymerisation of an oil-in-water emulsion using PVP as an efficient and environmentally advantageous stabiliser. The effects of agitation rate and PVP concentration on the microencapsulation process have been investigated using optical microscopy (OM) and scanning electron microscopy (SEM). The chemical structure and thermal stability of the microcapsules have been studied using Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). The solvent resistance of the microcapsules has been determined as well. Findings It has been revealed that the pH of the reaction mixture remained almost constant during the reaction, which simplified the process. It has also been observed that the microencapsulation yield improved and the microcapsules’ surface morphology became smoother when a high PVP content was used. With an increase in stirring rate from 600 to 1,200 rpm, the surface roughness and the average particle size decreased. The mean diameter of the prepared microcapsules ranged from 32.1 to 327.1 µm depending on the synthesis conditions. It was demonstrated that the microcapsules had a high capacity for MAT-PDMS encapsulation (more than 88 Wt.%). The solvent stability of the microcapsules against different polar, semi-polar and non-polar solvents was also evaluated. Research limitations/implications This research is limited to the encapsulation of a hydrophobic and sunlight curable liquid (such as MAT-PDMS) by means of in situ polymerisation of amino resins. Practical implications The results can be used by researchers working on the fabrication of microcapsules for applications such as drugs, electrophoretic inks, electrophoretic displays, intumescent fire-retardant coatings and self-healing materials. Social implications In self-healing coatings, healing agents which can be cured by UV irradiation or sunlight are envisaged attractive because they are catalyst-free, environmentally friendly and relatively inexpensive. PVP is an environmentally friendly emulsifier. The prepared microcapsules can be used in self-healing coatings to help in reducing maintenance costs for buildings and steel structures. Originality/value The novel aspect of this work is the development of a sunlight-curable silicone-based resin that was encapsulated in a MUF shell in the presence of PVP. A simple method was used to fabricate MUF microcapsules containing MAT-PDMS without the need to control pH during the reaction. Conventional methods for the preparation of amino resin microcapsules require an intensive and precise pH control to obtain favourable microcapsules. MAT-PDMS can be cured by sunlight and is catalyst-free, environmentally friendly and relatively inexpensive.


2018 ◽  
Vol 913 ◽  
pp. 1090-1096 ◽  
Author(s):  
Peng Liang ◽  
Qian Jin Mao ◽  
Zi Ming Wang ◽  
Su Ping Cui

In this paper, several urea–formaldehyde/epoxy microcapsules with different particle sizes were synthesized by in-situ polymerization. The chemical structure and compressive rupture load of microcapsule were characterized. The effect of microcapsule dosage, particle size and preload pressure on compressive strength of cementitious materials was studied. The result shows: when the particle size of microcapsule is 2 mm~2.5 mm, the rupture load of microcapsule is highest, more than 3N; When the microcapsule dosage is less than 2.5%, the strength loss of the matrix is relatively small; With the increase of the particle size of the capsule, the strength of the matrix decrease greatly; When the dosage of microcapsule is 2.5%, the particle size is 1.5 mm and the preload pressure is 30%~45%fmax, the compressive strength of the self-healing specimen is 8% higher than that of the non-preloaded specimens, which shows a certain self-healing performance.


2015 ◽  
Vol 766-767 ◽  
pp. 3-7 ◽  
Author(s):  
J. Lilly Mercy ◽  
S. Prakash ◽  
Katta Sai Sandeep ◽  
Dasari Sai Praveen

Self-healing composite materials possess healing agent which fills up the crack when ruptured and heals the crack by becoming a tough polymer when stimulated by a catalyst. Dicyclopentadiene (DCPD) in its monomer form is microencapsulated in the shell of Urea Formaldehyde (UF) under different agitation rates to acquire microcapsules of different diameters. The distribution of particle size, surface morphology and the presence of various chemical constituents in the microcapsules were analysed using optical microscopy, SEM and EDAX respectively. An agitation rate of 300 rpm, yielded capsules of diameters ranging from 800μm to 1700μm and at 900rpm the diameters were less than 300μm. Spherical shaped free flowing microcapsules were obtained through insitu polymerisation of dicyclopentadiene in Urea Formaldehyde.


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