Preparation and characterization of microcapsules containing capsaicin

With urea‐formaldehyde (UF) resin as walls and capsaicin as core substances, microcapsules were prepared based on in situ polymerization process. The morphology and size distribution of the microcapsules were analyzed by Fourier transform infrared spectroscopy, laser particle size analyzer, and scanning electron microscopy. The microcapsulated capsaicin (MC) agents had a mean diameter of about 30–50 μm. Moreover, the thermal properties of the MC agents were measured by differential scanning calorimetry and thermogravimetric analysis. It was demonstrated that the melting point and thermal stability of the MC agents were greatly improved compared with that of the uncovered capsaicin, which were caused by the encapsulating crosslinked UF resin over the surface. The shell formation mechanism and the effects of the process conditions such as U/F ratio, shearing force, and acidification time on the particle size of the MC agents were discussed. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Evaluation of melamine‐modified urea‐formaldehyde resins as particleboard binders

Particleboards bonded with 6 and 12% melamine‐modified urea‐formaldehyde (UMF) resins were manufactured using two different press temperatures and press times and the mechanical properties, water resistance, and formaldehyde emission (FE) values of boards were measured in comparison to a typical urea‐formaldehyde (UF) resin as control. The formaldehyde/(urea + melamine) (F/(U + M)) mole ratio of UMF resins and F/U mole ratio of UF resins were 1.05, 1.15, and 1.25 that encompass the current industrial values near 1.15. UMF resins exhibited better physical properties, higher water resistance, and lower FE values of boards than UF resin control for all F/(U + M) mole ratios tested. Therefore, addition of melamine at these levels can provide lower FE and maintain the physical properties of boards. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synthesis of enhanced urea–formaldehyde resin microcapsules doped with nanotitania

Urea–formaldehyde (UF) resin microcapsules doped with TiO₂ nanoparticles were prepared by in situ polymerization, and the properties of the microcapsules, such as the surface morphologies, thermal properties, and chemical elemental composition, were measured by optical microscopy, scanning electron microscopy, thermogravimetric analysis, and energy‐dispersive X‐ray spectrometer analysis. The effects of the presence of ammonium chloride and its concentration and the concentrations of UF resin prepolymer and TiO₂ nanoparticles during the reaction and deposition of UF on the microcapsule surface on the properties of the microcapsules were investigated. Enhanced UF resin microcapsules with more stability and mechanical strength could be obtained under the optimal conditions. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis and characterization of phenol–formaldehyde microcapsules containing linseed oil and its use in epoxy for self‐healing and anticorrosive coating

Phenol–formaldehyde microcapsules with linseed oil as an active agent were produced by applying in situ polymerization method. The anticorrosion and self‐healing efficiency of the synthesized materials were studied. Characteristics of these synthesized capsules were studied by Fourier transform infrared spectroscopy, and surface morphology was analyzed by using scanning electron microscope. Controllable particle size was estimated at different rpm of stirrer and particle size was checked under microscope and also by using particle size analyzer. The anticorrosion performance of encapsulated microcapsules coated with epoxy resin was carried out in 5% NaCl aqueous solution. The effectiveness of linseed oil filled microcapsules was investigated for healing the cracks generated in paint films or coatings. It was found that the cracks were successfully healed when linseed oil was released from ruptured microcapsules. Further, linseed oil‐healed area was found to prevent effectively the corrosion of the substrate in immersion studies. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Uron and uron–urea‐formaldehyde resins

The favored pH ranges for the formation of urons in urea‐formaldehyde (UF) resins preparation were determined, these being at pH's higher than 6 and lower than 4 at which the equilibrium urons ↔ N,N′‐dimethylol ureas are shifted in favor of the cyclic uron species. Shifting the pH slowly during the preparation from one favorable range to the other causes shift in the equilibrium and formation of a majority of methylol ureas species, whereas a rapid change in pH does not cause this to any great extent. UF resins in which uron constituted as much as 60% of the resin were prepared and the procedure to maximize the proportion of uron present at the end of the reaction is described. Uron was found to be present in these resins also as linked by methylene bridges to urea and other urons and also as methylol urons, the reactivity of the methylol group of this latter having been shown to be much lower than that of the same group in methylol ureas. Thermomechanical analysis (TMA) tests and tests on wood particleboard prepared with uron resins to which relatively small proportions of urea were added at the end of the reaction were capable of gelling and yielding bonds of considerable strength. Equally, mixing a uron‐rich resin with a low F/U molar ratio UF resin yielded resins of greater strength than a simple UF of corresponding molar ratio indicating that UF resins of lower formaldehyde emission with still acceptable strength could be prepared with these resins. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 277–289, 1999     

Production of melamine fortified urea‐formaldehyde resins with low formaldehyde emission

Melamine can be incorporated in the synthesis of urea‐formaldehyde (UF) resins to improve performance in particleboards (PB), mostly in terms of hydrolysis resistance and formaldehyde emission. In this work, melamine‐fortified UF resins were synthesized using a strong acid process. The best step for melamine addition and the effect of the reaction pH on the resin characteristics and performance were evaluated. Results showed that melamine incorporation is more effective when added on the initial acidic stage. The condensation reaction pH has a significant effect on the synthesis process. A pH below 3.0 results on a very fast reaction that is difficult to control. On the other hand, with pH values above 5.0, the condensation reaction becomes excessively slow. PBs panels produced with resins synthesized with a condensation pH between 4.5 and 4.7 showed good overall performance, both in terms of internal bond strength and formaldehyde emissions. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Granular urea‐formaldehyde slow‐release fertilizer with superabsorbent and moisture preservation

To improve the utilization of fertilizer and water resource at the same time, a new type of slow‐release fertilizer with superabsorbent and moisture preservation was developed, with the combination of slow‐release technique and superabsorbent polymers. The coatings were formed by the inverse phase polymerization technique. The element analysis results showed that the product contained 22.58% nitrogen element, and the water absorbency of the product was 94 times its own weight if it was allowed to swell in tap water at room temperature for 2 h. The results of the slow‐release behavior of N and the water absorbency and retention properties in soil showed that the product not only had good slow‐release property but also had excellent water absorbency and water retention capacity, which was a significant advantage over the normal slow‐release or controlled‐release fertilizers. The effects of the amount of initiator, crosslinker, reaction time, and the degree of neutralization of acrylic acid on water absorbency were investigated and optimized. At the same, a rather new and simple method was used to make homogeneous urea‐formaldehyde granules. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3230–3235, 2006     

Mechanical properties of blends of HDPE and recycled urea‐formaldehyde resin

The mechanical properties of blends of high‐density polyethylene (HDPE) with a recycled thermosetting filler, urea‐formaldehyde grit (UFG), were evaluated in the range of 0–23% of filler by volume. Ethylene‐acrylic acid (EAA) copolymers and an ionomer based on EAA were evaluated as compatibilizers. The observed tensile modulus of the ionomer‐treated blends was raised to three times the modulus of virgin polyethylene, whereas the modulus of the untreated blends reached double that of polyethylene. The ionomer‐treated blends also showed a higher tensile strength than the blends without filler treatment. The improvement in the properties was assigned to an increased interaction between the filler and the polymer matrix. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 3220–3227, 2000     

Optimal preparation and characterization of poly(urea–formaldehyde) microcapsules

Microcapsules with epoxy curing agent were successfully prepared by an in‐situ polymerization route with epoxy resin and poly‐(urea–formaldehyde) as core and shell materials, respectively. The synthetic conditions were optimized by a comprehensive investigation on raw materials consumption, size distribution, and surface morphology. Preparation of microcapsules with high wrap ratio was also demonstrated. The as‐synthesized microcapsules were studied using various characterizations techniques, including optical microscope, fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry, and contact angle meter. Spherical microcapsules (size: ～ 60 μm) with smooth surface were obtained when the stirring rate was 400 rpm and the amount of core materials is 76 wt %. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Effects of surface modification of self‐healing poly(melamine‐urea‐formaldehyde) microcapsules on the properties of unsaturated polyester composites

Poly(melamine‐urea‐formaldehyde) (MUF) microcapsules used as self‐healing component of composites were prepared by in situ polymerization. The surface of MUF microcapsules was modified by 3‐aminopropyltriethoxy silane‐coupling agent (KH550). The interfacial interactions between MUF microcapsules and KH550 were studied by Fourier transform infrared spectra (FTIR). FTIR results show that the silane‐coupling agent molecule binds strongly to the MUF microcapsules surface. A chemical bond (Si? O? C) is formed by the reaction between the Si? OH and the hydroxyl group of MUF microcapsule. This modification improves the thermal properties of microcapsules. Optical microscope (OM) and scanning electron microscope (SEM) show that a thin layer is formed on the surface of MUF microcapsules. The interfacial adhesion effect between MUF microcapsules and unsaturated polyester matrix was investigated. MUF microcapsules disperse evenly in the composites. When crack propagated, the microcapsules were broken and the repair agent flowed from the microcapsules to react with the curing agent. Then the crosslinking structure was formed and the composite was repaired. The tensile properties, impact properties, and dynamic mechanical properties of composites have been evaluated. The results indicate that the silane‐coupling agent plays an important role in improving the interfacial performance between the microcapsules and the matrix, as well as the mechanical properties of the composites. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

13C‐NMR study on the structure of phenol‐urea‐formaldehyde resins prepared by methylolureas and phenol

Phenol‐urea‐formaldehyde (PUF) resins were synthesized by reacting mixture of methylolureas (MMU), phenol, and formaldehyde. The structure of PUF cocondensed resins at different stages of reaction were analyzed by liquid ¹³C nuclear magnetic resonance (NMR) spectroscopy. The liquid ¹³C‐NMR analysis indicated that methylolureas had the dominant content in MMU with the reaction between urea and formaldehyde under the alkaline condition. The PUF cocondensed resins had no free formaldehyde. methylolureas were well incorporated into the cocondensed resins by reacting with phenolic units to form cocondensed methylene bridges. The second formaldehyde influenced the further reaction and the structure of the PUF resins. The resins with the prepared method of PUFB possessed relatively high degree of polymerization and low proportion of unreacted methylol groups. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Correlating viscosity in urea–formaldehyde polymerization

The objective of this study was to find a correlation for the viscosity changes during step polymerization of urea and formaldehyde. For this reason, a kinetic model for the condensation reactions was proposed, and using this model, a correlation for the kinematic viscosity changes of the solution during polymerization was obtained. Viscosity measurements of the samples during condensation reactions were carried out using Ubbelohde viscometers at intervals. The experimental data were curve fitted using our model, which was found to correspond very well. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 631–636, 1998     

A study on the colloidal nature of urea‐formaldehyde resins and its relation with adhesive performance

Urea‐formaldehyde (UF) resins present a swollen colloidal phase dispersed within a continuous water phase containing soluble oligomers. The main goal of the present investigation is to clarify the physical and chemical nature of those two phases and elucidate their impact on the bonding process. Optical and electronic microscopy has provided information on the morphology of the colloidal phase, showing primary particles and particle agglomerates. Mechanisms are suggested for the colloidal stabilization and dilution‐induced flocculation. Three commercial UF resins with different F/U molar ratios were studied using particle size distribution (PSD) analysis. The results showed the influence of the resin's degree of condensation and the aging status on the size of the colloidal structures. Gel permeation chromatography analysis was performed on samples of different resins and of the respective continuous and dispersed phases, separated by centrifugation. The quantified fraction of insoluble molecular aggregates present in the chromatograms was related to the resins synthesis conditions and age. Differential scanning calorimetry and tensile shear strength tests were performed to evaluate the reactivity and adhesive performance of each phase. It is suggested that the colloidal phase acts as a reactive filler at the wood joint interfaces, contributing for the resins bonding performance. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Intercalation structure and toughening mechanism of graphene/urea‐formaldehyde nanocomposites prepared via in situ polymerization

Based on the industrialized graphene (GN) product, a series of graphene/urea‐formaldehyde nanocomposites were synthesized via in situ polymerization by incorporation of silicon coupling agent with terminal amino groups (SA) as the compatibilizer. The results showed that addition of SA coupling agent led to much more efficient grafting of UF molecules on the GN surface with high layer thickness by formation of hydrogen bonding, and thus complete exfoliation and uniform dispersion of GN were achieved for the composites. Compared with neat UF, the addition of 1.0 wt% GN resulted in a roughly 25% increase in tensile strength and 12% increase in impact strength; meanwhile the impact fracture surfaces of the composite showed obvious ductile fracture characteristics, indicating the reinforcing and toughening effect of GN on the UF matrix. With increasing GN content, the storage modulus, glass transition temperature and crosslinking density of UF increased, while the tan δ_max decreased, suggesting that a double crosslinking network structure with GN centered crosslinking point and chemical crosslinking point of UF molecular chains formed, leading to improvement in the stiffness of the composites. The present work showed promising potential for developing high performance UF resin on an industrial scale. © 2017 Society of Chemical Industry     

Curing of low level melamine‐modified urea‐formaldehyde particleboard binder resins studied with dynamic mechanical analysis (DMA)

Effects of resin formulation, catalyst, and curing temperature were studied for particleboard binder‐type urea‐formaldehyde (UF) and 6 ～ 12% melamine‐modified urea‐melamine‐formaldehyde (UMF) resins using the dynamic mechanical analysis method at 125 ～ 160°C. In general, the UF and UMF resins gelled and, after a relatively long low modulus period, rapidly vitrified. The gel times shortened as the catalyst level and resin mix time increased. The cure slope of the vitrification stage decreased as the catalyst mix time increased, perhaps because of the deleterious effects of polymer advancements incurred before curing. For UMF resins, the higher extent of polymerization effected for UF base resin in resin synthesis increased the cure slope of vitrification. The cure times taken to reach the vitrification were longer for UMF resins than UF resins and increased with increased melamine levels. The thermal stability and rigidity of cured UMF resins were higher than those of UF resins and also higher for resins with higher melamine levels, to indicate the possibility of bonding particleboard with improved bond strength and lower formaldehyde emission. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 377–389, 2005     

Syntheses and properties of carboxymethyl chitosan/urea–formaldehyde snake‐cage resins

A series of novel snake‐cage resins were synthesized using carboxymethyl chitosan (CM‐CTS) as the snake resin and urea–formaldehyde resin (UF) as the cage resin. Such factors as the optimal synthesis conditions, content of the crosslinking agent, and sorption capacities for metal ions of the above‐mentioned resins were investigated. The experimental results show that these resins have appropriate swelling properties and good mechanical stability. They do not run off in water, HCl, and NaOH aqueous solutions. To form a stable network system, NH₄Cl was used as a crosslinking agent to crosslink urea and formaldehyde in synthesis. The sorption experiment showed that the sorption properties of the resins in the presence of the crosslinking agent NH₄Cl are better than those without a crosslinking agent. The investigation of the FTIR spectra indicated that the chelate groups, such as —OH, —CO and NHCH₂CO, in snake‐resin molecules participated in the coordination with the metal ions, but the —C?O bonds in the cage resin UF did not. The snake resin CM‐CTS in the snake‐cage resins was the major contributor of sorption. The sorption dynamics showed that the sorption was controlled by liquid film diffusion. The isotherms can be described by Freundlich and Langmuir equations. The saturated sorption capacities of the resins for Cu²⁺, Ni²⁺, Zn²⁺, and Pb²⁺ were 1.48, 0.78, 0.13, and 0.02 mmol g^?1, respectively. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 310–317, 2002; DOI 10.1002/app.10331     

Properties of poly(urea‐formaldheyde) microcapsules containing an epoxy resin

Physical properties of urea‐formaldehyde microcapsules containing an epoxy resin are presented and discussed. Microcapsules were prepared by in situ polymerization of monomers in an oil‐in‐water emulsion. Differential scanning calorimetry, thermogravimetric analysis, and scanning electronic microscopy were applied to investigate thermal and morphological microcapsule properties. Microencapsulation was detected by means of FTIR and Raman techniques. It was found that the amount of encapsulated epoxy resin as well as the extent of urea‐formaldehyde polymerization depends on the reaction temperature and the stirring speed. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Effect of addition of glycolysis products of poly(ethyleneterephthalate) wastes to urea‐formaldehyde resin on its adhesion performance to wood substrates and formaldehyde emission

Recycling of poly(ethyleneterephthalate) waste was achieved through glycolysis using diethyleneglycol (DEG) and poly(ethyleneglycol) (PEG 400), which yielded different fractions that exhibited hydroxyl numbers of 174.41 and 54.86 mg of KOH/g, respectively, whereas GPC profiles revealed bimodality in both cases corresponding to M_n values equivalent to 534 and 1648. The products of glycolysis from both cases were individually incorporated as modifiers during the synthesis of urea‐formaldehyde resins from both the basic as well as acidic stages, respectively. It was found that the free formaldehyde level was remarkably decreased for the modified resins while the gel time was slightly affected indicating some activation of the resins. In addition, the adhesion strength of wood joints bonded with the modified resins improved markedly in the dry state while the moisture resistance was significantly fortified with respect to the comparable joints formulated from unmodified resins where instant failure took place within few hours after immersion in water. The shelf life of the resins did not prolong and lasted maximum for about 2 months which was ascribed to the presence of reasonable amount of carboxyl terminal groups at the ends of a minor portion of the glycolyzed products that could actively act to self‐catalyze the polycondensation and crosslinking reactions during storage leading eventually to vitrification of the resin and shortening of shelf life. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis and characterization of grafting β‐cyclodextrin with chitosan

Two new adsorbents [β‐cyclodextrin–chitosan (β‐CD–CTS) and β‐cyclodextrin‐6–chitosan (β‐CD‐6‐CTS)] were synthesized by the reaction of β‐cyclodextrin (β‐CD) with epoxy‐activated chitosan (CTS) and the sulfonation of the C‐6 hydroxyl group of β‐cyclodextrin with CTS, respectively. Their structures were confirmed by IR spectral analysis and X‐ray diffraction analysis, and their apparent amount of grafting was determined by ultraviolet spectroscopy. The adsorption properties of β‐CD‐CTS and β‐CD‐6‐CTS for p‐dihydroxybenzene were studied. The experimental results showed that the two new adsorbents exerted adsorption on the carefully chosen target. The highest saturated capacity of p‐dihydroxybenzene of β‐CD‐CTS and β‐CD‐6‐CTS were 51.68 and 46.41 mg/g, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 860–864, 2004     

Storage stability and solubility of poly(urea‐formaldehyde) microcapsules containing A‐olefin drag reducing polymer

Microcapsules containing α‐olefin drag reducing polymer were prepared by in situ and interfacial polymerization with urea, formaldehyde, and styrene as shell materials, respectively. IR spectrums of prepared shells indicated the formations of poly(urea‐formaldehyde) and polystyrene in the microencapsulating process. The morphologies of uncoated particles and microcapsules were observed by scanning electron microscopy (SEM) which proved that the α‐olefin drag reducing polymer particles were effectively coated. For the purpose of determining the stability of microcapsules in transportation and storage, the static pressure experiment was carried out and lasted for 6 months. In this process, microcapsules with polystyrene as shell material stuck together after 3 months; however, those with poly(urea‐formaldehyde) kept the state of particles. The thermal characteristics of uncoated particles (core), poly(urea‐formaldehyde) (shell), and microcapsules with that as shell material were characterized by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) which proved that thermal stable temperature of microcapsules containing α‐olefin drag reducing polymer with poly(urea‐formaldehyde) as shell material was below 225°C, and the mean heat absorbed by microcapsules in the temperature increasing process was 1.5–2.0 W/g higher than that by cores. The evaluation of drag reducing rate of microcapsules showed that the microencapsulating process had no influence on the drag reduction of α‐olefin drag reducing polymer. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011