Latent Heat Enhancement of Paraffin Wax in Poly(divinylbenzene-co-methyl methacrylate) Microcapsule

The preparation of divinylbenzene (DVB)-methyl methacrylate (MMA) copolymer microcapsule encapsulated Rubitherm27 (RT27) P(DVB-co-MMA)/RT27 used as heat storage material by the microsuspension polymerization was studied to improve the latent heats of the encapsulated RT27 with sufficient polymer shell strength. Percent loading of RT27 and DVB:MMA ratio were optimized. The optimal condition was 30% loading of RT27 and 30:70 (% w/w) of DVB:MMA ratio. The nonspherical microcapsules with a dent having core-shell morphology were obtained. The thermal properties of the encapsulated RT27 in the P(DVB-co-MMA)/RT27 capsules were measured by thermogravimetric analyzer and differential scanning calorimeter. The heats of melting (ΔH_m; 153 J/g-RT27) and crystallization (ΔH_c; 164 J/g-RT27) of the encapsulated RT27 in the prepared copolymer capsules were higher than those in PDVB and closed to those of bulk RT27 (162 and 168 J/g-RT27 for ΔH_m and ΔH_c, respectively).     

Preparation of high performance copolymer microcapsule encapsulated heat storage material without supercooling

ABSTRACT

The methyl methacrylate (MMA)-based copolymer microcapsules encapsulating Rubitherm®27 (RT27) used as a phase change material were successfully prepared by microsuspension polymerization. The influence of three types of crosslinked comonomers such as ethylene glycol dimethacrylate), trimethylolpropane trimethacrylate, and divinylbenzene (DVB) on the microcapsule formation was studied at various ratios of MMA:crosslinked comonomer. It was found that using MMA:DVB at 70:30 wt% was the optimum ratio. The obtained microcapsules were nonspherical in shape with a dent and high shell strength. In addition, the latent heats of melting and crystallization of the encapsulated RT27 were about 140 J/g-RT27 which were close to those of the original RT27. However, the crystallization temperatures (T_c) of the encapsulated RT27 (14°C) were lower than that of the original RT27 (25°C) which was called supercooling. To prevent supercooling, the effect of nucleating agents (emulgen 150, 1-octadecanol, and RT58) on decreasing supercooling of the encapsulated RT27 was investigated. The results clearly presented that the addition of at least 5 wt% of RT58 significantly increased T_c (25°C) of the encapsulated RT27, whereas the observed latent heats were pretty close to original RT27.     

Preparation,characterization, and prominent thermal stability of phase‐change microcapsules with phenolic resin shell and n‐hexadecane core

Microcapsules with phenolic resin (PFR) shell and n‐hexadecane (HD) core were prepared by controlled precipitation of the polymer from droplets of oil‐in‐water emulsion, followed by a heat‐curing process. The droplets of the oil phase are composed of a polymer (PFR), a good solvent (ethyl acetate), and a poor solvent (HD) for the polymer. Removal of the good solvent from the droplets leads to the formation of microcapsules with the poor solvent encapsulated by the polymer. The microstructure, morphology, and phase‐change property as well as thermal stability of the microcapsules were systematically characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimety (DSC), and thermogravimetric analysis (TGA). The phase‐change microcapsules exhibit smooth and perfect structure, and the shell thickness is a constant fraction of the capsule radius. The initial weight loss temperature of the microcapsules was determined to be 330°C in N₂ and 255°C in air, respectively, while that of the bulk HD is only about 120°C both in air and N₂ atmospheres. The weight loss mechanism of the microcapsules in different atmosphere is not the same, changing from the pyrolysis temperature of the core material in N₂ to the evaporation of core material caused by the fracture of shell material in air. The melting point of HD in microcapsules is slightly lower than that of bulk HD, and a supercooling was observed upon crystallization. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

DSC and synchrotron-radiation X-ray diffraction studies on crystallization and polymorphic behavior of palm stearin in bulk and oil-in-water emulsion states

The crystallization and polymorphic behavior of palm stearin (PS) in a bulk state and in oil-in-water (O/W) emulsion droplets (average diameter, 1.7±0.3 μm) was observed by using DSC, optical microscopy, and in situ X-ray diffraction with synchrotron radiation (SR-XRD). For the bulk sample the DSC measurements revealed three main exothermic peaks at approximately 31 (large), 21 (small) and 3°C (medium) on cooling, and broad endothermic peaks at approximate −3 (small), 8, 15 to 25 (medium), and 37 and 53°C upon heating. The SR-XRD patterns taken during cooling from 60 to −5°C clarified that the DSC exothermic peaks around 31 and 3°C corresponded to crystallization of the α form of high-melting and low-melting fractions, respectively, and that the occurrence of β′ corresponded to the small exothermic peak around 21°C. The XR-XRD patterns taken during heating from −5 to 60°C demonstrated that the DSC endothermic peaks corresponded to the following transformation processes: melting of α of the low-melting fraction (−3°C), melt-mediated transformation from α to ∇′ (15–25°C), melting of β′ (36°C), and melting of β (53°C) of the high-melting fraction. As for the O/W emulsion sample, the DSC and SR-XRD measurements during the cooling and heating processes exhibited basically the same behavior as that of PS in the bulk state, except that β′ did not crystallize during the cooling process, and the temperatures of crystallization of α, melt-mediated α→β′→β transformation, and melting of β were lower in the emulsion droplets than in the bulk state.     

种子微悬浮聚合法制备微胶囊相变材料

以苯乙烯(St)和二乙烯基苯(DVB)为壁材聚合单体,偶氮二异丁腈(AIBN)为引发剂,羟丙基纤维素(HPC)和碳酸钙(Ca CO3)为复合分散剂,用种子微悬浮聚合法制备交联聚苯乙烯(PS)包覆硬脂酸丁酯微胶囊。用扫描电子显微镜(SEM)、差示扫描热量仪(DSC)、粒度分析仪和热重分析仪(TG)表征了微胶囊的形貌和性能,考察了聚合方法、交联剂和分散剂对微胶囊形貌结构和性能的影响。结果表明,种子微悬浮聚合法制备的微胶囊呈粒径分布均匀、规整的球形结构,与常规悬浮聚合法制备的微胶囊相比,相变潜热提高了41.6%,包覆率提高15.1%;随着DVB用量的增加,壁材的交联度增大,微胶囊密封性和热稳定性提高;采用复合分散剂且m(HPC)∶m(CaCO_3)=2.2∶1时,微胶囊相变潜热提高了26.8%。     

Preparation and characterization of flame retardant phase change materials by microencapsulated paraffin and diethyl ethylphosphonate with poly(methacrylic acid‐co‐ethyl methacrylate) shell

Microcapsules containing paraffin and diethyl ethylphosphonate (DEEP) flame retardant with uncrosslinked and crosslinked poly (methacrylic acid‐co‐ethyl methacrylate) (P(MAA‐co‐EMA)) shell were fabricated by suspension‐like polymerization. The surface morphologies of the microencapsulated phase change materials (microPCMs) were studied by scanning electron microscopy. The thermal properties and thermal stabilities of the microPCMs were investigated by differential scanning calorimetry (DSC), and thermal gravimetric analysis (TGA). The flame retarding performances of the microcapsule‐treated foams were calculated by using an oxygen index instrument. The DSC results showed that the crosslinking of the polymer shell led to an increase in the melting enthalpies of the microcapsule by more than 15%. The crosslinked P(MAA‐co‐EMA) microcapsules with DEEP and without DEEP have melting enthalpies of 67.2 and 102.9 J/g, respectively. The TGA results indicated that the thermal resistant temperature of the crosslinked microcapsules with DEEP was up to 171°C, which was higher than that of its uncrosslinked counterpart by ～20°C. The incorporation of DEEP into the microPCM increased the limiting oxygen index value of the microcapsule‐treated foams by over 5%. Thermal images showed that both microcapsule‐treated foams with and without DEEP possessed favorably temperature‐regulated properties. As a result, the microPCMs with paraffin and DEEP as core and P(MAA‐co‐EMA) as shell have good thermal energy storage and thermal regulation potentials, such as thermal‐regulated foams heat insulation materials. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41880.     

Facile synthesis of silica/polymer hybrid microspheres and hollow polymer microspheres

Monodisperse silica/polydivinylbenzene (SiO₂/PDVB) and silica/poly(ethyleneglycol dimethacrylate) (SiO₂/PEGDMA) core-shell hybrid microspheres were prepared by a two-stage reaction with silica particles' grafting of 3-(methacryloxy)propyltrimethoxysilane (MPS) as core and PDVB or PEGDMA as shell, in which the MPS-modified silica core with diameter of 238 nm was synthesized by Stöber method and subsequently grafted with MPS as the first-stage reaction. The PDVB or PEGDMA shell was then encapsulated over the MPS-modified silica core by distillation precipitation polymerization of divinylbenzene (DVB) or ethyleneglycol dimethacrylate (EGDMA) in neat acetonitrile with 2,2′-azobisisobutyronitrile (AIBN) initiator as the second-stage reaction. The encapsulation of PDVB and PEGDMA on modified silica core particles was driven by the capture of DVB or EGDMA oligomer radicals via the vinyl groups on the surface of the modified silica cores during the second-stage polymerization in the absence of any stabilizer or surfactant. The shell thickness of the core-shell hybrid particles was controlled by the feed of DVB or EGDMA monomer during the polymerization. Hollow PDVB or PEGDMA microspheres with various shell thickness were further developed after selective removal of the modified silica cores with hydrofluoric acid. The resultant core-shell hybrid materials and hollow microspheres were characterized by transmission electron microscopy (TEM), and Fourier transform infrared spectra (FT-IR).     

Simultaneous synchrotron radiation X-ray diffraction-DSC analysis of melting and crystallization behavior of trilauroylglycerol in nanoparticles of oil-in-water emulsion

Crystallization, polymorphic transformation, and melting behavior of nanoparticles of trilauroylglycerol (LLL) in oil-in-water (O/W) emulsion were examined initially by DSC, and then by simultaneous synchrotron radiation small-angle (SAXS) and wide-angle (WAXS) X-ray diffraction and DSC (SR-SAXS /WAXS/DSC). The O/W nanoparticles emulsions having average diameters of 42 to 120 nm were prepared by application of mechanical shear using a high-pressure homogenizer. The following results were obtained: (i) The DSC study showed that the melting temperature of the stable β form of LLL was reduced from 46.7 (bulk) to 26.5–44.0°C (nanoparticles); this variation as assumed to be due to the size distribution of the nanoparticles. Crystallization temperature was also reduced from 18.9 (bulk) to −9.5±0.5°C (nanoparticles). These results were consistent with those of previous studies of nanoparticles of fats obtained in the O/W emulsion. (ii) The results obtained by the SR-SAXS/WAXS/DSC technique during the cooling process to −20°C showed that the first-occurring polymorph of LLL in the bulk liquid was β′, whereas α was first nucleated and transformed to β′ around −10°C during cooling in the nanoparticles. (iii) The SR-SAXS/WAXS/DSC data taken during the heating process from −20°C after the crystallization showed that β′ transformed to β around 0°C and that the melting of β started at 30°C and ended at 44°C. The present study showed that forming nanoparticles of LLL in the O/W emulsion having the diameters of 42 to 120 nm reduced the melting and crystallization temperatures and increased the transformation rate of α→β′→β in comparison to the LLL crystals formed in the bulk phase.     

Preparation and characterization of controlled-release microencapsulated acids for deep acidizing of carbonate reservoirs

Based on the deficiency of traditional acidification or acid pressure technology in the development of carbonate oil and gas resources, a microcapsule which wraps hydrochloric acid and can be released through temperature control was prepared by using microcapsule technology. The microcapsules were prepared with polyurethane prepolymer (PUA) and 1,6-hexadiol diacrylate (HDDA) polymer as wall material and hydrochloric acid as core material by two emulsification and photocatalysis methods. Its parcel rate is 61.9%. Fourier transform infrared spectroscopy characterization confirmed the successful photopolymerization of PUA prepolymer and HDDA in a strong acid environment. The microscopic morphology analysis of electron microscope showed that the microcapsule was regular and uniform spherical with smooth and dense surface. The particle size analysis showed that the microcapsules were mainly distributed between 40 and 300 μm, and the average particle size was 114.02 μm.The glass temperature of microcapsule wall material was 97°C by DSC method. The release rate of microcapsules was accelerated with the increase of release temperature. The cumulative release rate of acid solution of microcapsules for 3 h reached 28.4%, and the final release rate of microcapsules for 12 h reached 90.7% under 100°C. In addition, the release of microcapsules is less affected by the formation salinity. At 90°C, the maximum release rate of 7.5 g/L CaCL₂ was 49.1%, lower than that of 59.4% in pure water, showing the good salt resistance of the wall materials of microcapsules.     

Composition and thermal properties of cattle fats

The physical‐chemical properties, fatty acid composition and thermal properties of cattle subcutaneous, tallow and intestinal fats were determined. Subcutaneous fat differed from the other fat types with respect to its lower melting point (29.0 °C) and higher saponification (211.4 mg KOH/g) and iodine (50.55) values. The cattle fat types contained palmitic acid (16:0), stearic acid (18:0), oleic acid (18:1n‐9) and linoleic acid (18:2n‐6) as the major components of fatty acid composition (24.58–25.90%, 10.21–33.33%, 28.18–46.05%, 1.54–1.73%, respectively). A differential scanning calorimetry (DSC) study revealed that two characteristic peaks were detected in both crystallization and melting curves. Major peaks (T_peak) of tallow and intestinal fats were similar and determined as 24.10–27.71 °C and 2.16–4.75 °C, respectively, for crystallization peaks and 7.09–9.39 °C and 43.28–46.49 °C, respectively, for melting peaks in DSC curves; however, those of subcutaneous fat (12.48 °C and –6.79 °C for crystallization peaks and 3.56 °C and 23.55 °C for melting peaks) differed remarkably from those of the other fat types.     

Microencapsulation of imidazole curing agent for epoxy resin

An epoxy resin–imidazole system was used to form the adhesives for the anisotropic conducting film (ACF), and a latent curing system was necessary for the ACF. In this study, 2-phenylimidazole (2PhI) was encapsulated for the latent curing system. Polycaprolactone (PCL) was used as the wall material, and the solvent evaporation method was used to form the microcapsule. The effects of the ratio of 2PhI and PCL, and the effects of the molecular weight of PCL were investigated during the microcapsule formation. The amount of 2PhI in the microcapsule was measured using TGA. The permeability of the microcapsules was measured in ethanol, and the shelf life of the microcapsules was also studied for the epoxy resin. The curing behavior was examined using DSC. In the curing reaction of the epoxy resin, the microcapsule of 2PhI exhibited a delayed kinetic behavior compared to pure 2PhI. This microcapsule of 2PhI exhibited a long shelf life, and the curing did not occur in this microcapsule–epoxy resin system at 20 °C for more than 30 days.     

Effect of poly(propylene carbonate) on the crystallization and melting behavior of poly(β‐hydroxybutyrate‐co‐β‐hydroxyvalerate)

The crystallization and melting behavior of poly(β‐hydroxybutyrate‐co‐β‐hydroxyvalerate) (PHBV) and a 30/70 (w/w) PHBV/poly(propylene carbonate) (PPC) blend was investigated with differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR). The transesterification reaction between PHBV and PPC was detected in the melt‐blending process. The interaction between the two macromolecules was confirmed by means of FTIR analysis. During the crystallization process from the melt, the crystallization temperature of the PHBV/PPC blend decreased about 8°C, the melting temperature was depressed by 4°C, and the degree of crystallinity of PHBV in the blend decreased about 9.4%; this was calculated through a comparison of the DSC heating traces for the blend and pure PHBV. These results indicated that imperfect crystals of PHBV formed, crystallization was inhibited, and the crystallization ability of PHBV was weakened in the blend. The equilibrium melting temperatures of PHBV and the 30/70 PHBV/PPC blend isothermally crystallized were 187.1 and 179°C, respectively. The isothermal crystallization kinetics were also studied. The fold surface free energy of the developing crystals of PHBV isothermally crystallized from the melt decreased; however, a depression in the relative degree of crystallization, a reduction of the linear growth rate of the spherulites, and decreases in the equilibrium melting temperature and crystallization capability of PHBV were detected with the addition of PPC. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 2514–2521, 2004     

Expansion space and thermal stability of microencapsulated n‐octadecane

5.0–50.0 vt% of cyclohexane was mixed with 95.0–50.0 vt% of n‐octadecane as the oil‐phase during the emulsion process in the in situ polymerization of melamine‐formaldehyde. By heat‐treating the microcapsules in an oven at 100°C, the cyclohexane was removed and expansion space was formed inside the microcapsules. The microcapsules were characterized by using FTIR, SEM, DSC, TGA, and gas chromatography. When the microcapsules are heat‐treated at temperatures higher than 180°C, Tm, ΔHm, Tc, and ΔHc of the microcapsules decrease. The attenuation of enthalpy of the microcapsules containing expansion space is obviously lower than that of the control sample, however. The permeability of the microcapsule shell decreases with the increase of cyclohexane content. There is a maximum between the thermal stabilities of the microcapsules and the cyclohexane contents. The microcapsules synthesized with 30.0–40.0 vt% of cyclohexane have the highest thermal stabilities, with 230°C and 289°C in air and nitrogen atmosphere, respectively. The thermal stable temperatures are approximately 67°C and 102°C higher than that of the control sample, respectively. The expansion space inside the microcapsules allows the n‐octadecane to expand in the temperature rising process and exert lower pressure to the shell, therefore keeping the shell intact and increasing the thermal stabilities of the microcapsules. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 390–396, 2005     

Biodegradable polymer blends of poly(3-hydroxybutyrate) and poly(DL-lactide)-co-poly(ethylene glycol)

The melting and crystallization behavior and phase morphology of poly(3-hydroxybutyrate) (PHB) and poly(DL-lactide)-co-poly(ethylene glycol) (PELA) blends were studied by DSC, SEM, and polarizing optical microscopy. The melting temperatures of PHB in the blends showed a slight shift, and the melting enthalpy of the blends decreased linearly with the increase of PELA content. The glass transition temperatures of PHB/PELA (60/40), (40/60), and (20/80) blends were found at about 30°C, close to that of the pure PELA component, during DSC heating runs for the original samples and samples after cooling from the melt at a rate of 20°C/min. After a DSC cooling run at a rate of 100°C/min, the blends showed glass transitions in the range of 10–30°C. Uniform distribution of two phases in the blends was observed by SEM. The crystallization of PHB in the blends from both the melt and the glassy state was affected by the PELA component. When crystallized from the melt during the DSC nonisothermal crystallization run at a rate of 20°C/min, the temperatures of crystallization decreased with the increase of PELA content. Compared with pure PHB, the cold crystallization peaks of PHB in the blends shifted to higher temperatures. Well-defined spherulites of PHB were found in both pure PHB and the blends with PHB content of 80 or 60%. The growth of spherulites of PHB in the blends was affected significantly by 60% PELA content. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 1849–1856, 1997     

Microencapsulation of imidazole curing agent by solvent evaporation method using W/O/W emulsion

The epoxy–imidazole resin system is used to form the anisotropic conducting film. The latent character of the system is very significant. In this study, imidazole (Im) or 2‐methylimidazole (2MI) was encapsulated for the latent curing system to use in the reaction of epoxy resin. Polycaprolactone was used as a wall material, and the solvent evaporation method was used to form the microcapsule using W/O/W emulsion. The shelf life of the microcapsules was studied for the epoxy resin, and the curing behavior of the microcapsules for epoxy resin was examined using a differential scanning calorimeter. The curing times at 150 and 180°C were estimated using an indentation method. The microcapsules of Im or 2MI exhibited a long shelf life for epoxy resin. When comparing the results of the previous methods with the results of this study using the W/O/W emulsion, finer microcapsules were formed and the microcapsule has longer shelf life. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation and characterization of paraffin microcapsules for energy-saving applications

A series of microencapsulated phase-change materials (PCMs) with styrene–divinyl benzene shells composed of an n-octadecane (OD or C₁₈)–n-hexadecane (HD or C₁₆) mixture as the core were synthesized by an emulsion polymerization method. The effects of the core/shell ratio (C/S) and surfactant concentration (C_surf) on the thermal properties and encapsulation ratios of the PCMs were investigated. The chemical structures and morphological properties of the microcapsules were characterized by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy analysis, respectively. The characteristic peaks of the paraffin mixtures and shell material located in the FTIR spectrum of the microencapsulated PCMs proved that the encapsulation of the PCM mixture was performed successfully. The thermal properties of the paraffin microcapsules were determined by differential scanning calorimetry (DSC) and thermogravimetric analysis. DSC analysis demonstrated that the microcapsules containing the maximum amount of paraffin mixture (C/S = 2:1) and the minimum C_surf (45 mmol/L) had the highest latent heat value of 88 kJ/kg and a latent heat of temperature of 21.06°C. Moreover, the maximum encapsulation ratio of the paraffin mixture was found to be 56.77%. With respect to the analysis results, the encapsulated binary mixture, which consisted of OD–HD with a poly(styrene-co-divinyl benzene) shell, is a promising material for thermal energy storage applications operating at low temperatures, such as in the thermal control of indoor temperatures and air-conditioning applications in buildings for desirable thermal comfort and energy conservation. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47874.     

Thermal properties and isothermal crystallization of syndiotactic polypropylenes: Differential scanning calorimetry and overall crystallization kinetics

Isothermal crystallization and subsequent melting behavior of five samples of syndiotactic polypropylene are presented. Crystallization studies were carried out in the temperature range of 60°C to 97.5°C using a differential scanning calorimeter (DSC). Subsequent DSC scans of isothermally crystallized samples exhibited double melting endotherms. The high melting peak was concluded to be the result of the melting of crystals formed by recrystallization during the reheating process. Overall crystallization kinetics was studied based on the traditional Avrami analysis. Analysis of crystallization times based on the modified growth rate theory suggested that, within the crystallization temperature range studied, the syndiotactic polypropylenes crystallize in regime III. Kinetic crystallizability parameters also were evaluated, and were found to be in the range of 0.41°C s⁻¹ to 2.14°C s⁻¹. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 75: 44–59, 2000     

Preparation and characterization of double‐MF shell microPCMs used in building materials

A kind of double‐shell heat energy storage microcapsule was prepared used melamine formaldehyde (MF) resin as shell material, and the properties of the microcapsules were investigated. A phase change material, with melt point of 24°C and phase transition heat of 225.5J/g, was used as core. The microcapsules would be used in indoor walls to regulate the temperature and save energy. The surface morphological structure was examined by means of scanning electron microscopy. The strength of the shell was evaluated through observing the surface change after pressure by means of scanning electron microscopy. The average diameter of the microcapsules was 5 μm ～ 10 μm. Diameter of 1 μm ～ 5 μm could also be obtained by using different stirring speeds. The globular surface was smooth and compact. The thickness was 0.5 μm ～ 1 μm. Also, the melting point of the microcapsules was 24.7°C, nearly equal to the pure phase change material. The DSC results make clear that the polymer shell of the microcapsules does not influence the properties of the phase change material. It was also found that the avoiding penetration property of the double‐shell microcapsules was better than that of single shell, and the average diameter of 5 μm was better than 1 μm. With the increase of ratio of the core material, the compactability decreased, and the shell thickness decreased. The mass ratio of core and shell was 3 : 1 to ensure that the microcapsules had good heat storage function. The measuring test showed that the microcapsules did not rupture at a pressure of 1.96 × 10⁵ Pa. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 1755–1762, 2005     

Preparation of paraffin-based phase-change microcapsules and application in geopolymer coating

A type of paraffin phase-change microcapsule for thermal insulation of exterior walls was prepared by in situ polymerization of low-softening-point paraffin (46°C) as core material and acrylic copolymer as shell. The surface morphology, phase-change thermal properties, and thermal stability were characterized by scanning electron microscopy, laser particle size distribution analysis, differential scanning calorimetry, and thermogravimetric analysis, respectively. The results showed that, for polymerization reaction temperature of 75°C and paraffin/acrylic copolymer mass ratio of 1.8, the microcapsules prepared at rotation speed of 1600 r/min with 8% emulsifiers were spherical particles with smooth surface and average particle size of 0.68 μm. The phase-change temperature and latent heat storage capacity of the microcapsules were 47.8°C and 174 J/g, respectively. The paraffin phase-change microcapsules obtained using the optimum synthesis condition were mixed in a metakaolin-based geopolymer coating at different proportions, and the thermal insulation ability of the resulting phase-change thermal energy storage coating characterized.     

Mechanical,thermal properties and isothermal crystallization kinetics of biodegradable poly(butylene succinate-<Emphasis Type="Italic">co</Emphasis>-terephthalate) (PBST) fibers

Biodegradable copolymer poly(butylene succinate-co-terephthalate) (PBST), with 70 mol% butylene terephthalate (BT), was melt-spun into fibers with take-up velocity of 2 km/min. The mechanical and thermal properties of the as-spun fibers were investigated through tensile test, DSC and TGA. Compared to poly(butylene terephthalate) (PBT) fibers, PBST fibers exhibited lower initial tensile modulus and higher tensile elongation at break which indicated their better flexibility. DSC results showed high melting temperature (ca.180.7 °C) of PBST fibers helpful to the textile processing compared to other biodegradable polyesters. Furthermore, isothermal crystallization behaviors of PBST fibers at low and high supercoolings were investigated by DSC and DLI, respectively. The measurement of crystallization kinetics at low supercoolings indicated that Avrami exponent n for PBST fibers was at a range of 2.9 to 3.3, corresponding to the heterogeneous nucleation and a 3-dimensional spherulitic growth. Similar results were given for isothermal crystallization behavior at high supercoolings investigated by DLI technique. Additionally, the equilibrium melting temperature of PBST fibers was obtained for 206.5 °C by Hoffman-Weeks method. Further investigation through DLI measurement provided the temperature at maximum crystallization rate for PBST fibers located at about 90 °C, which was very useful to polymer processing.