Release behaviors of porous poly(butylene succinate)/poly(epsilon-caprolactone) microcapsules containing indomethacin

The biodegradable poly(butylene succinate)/poly(epsilon-caprolactone) (PBS/PCL) microcapsules containing indomethacin were prepared by emulsion solvent evaporation method. The morphologies, thermal properties, and release behaviors of PBS/PCL microcapsules were investigated. As a result, the microcapsules exhibited porous and spherical form in the presence of gelatin as a surfactant. From the DSC result, the PBS/PCL microcapsules showed the two exothermic peaks meaning the melting points of PCL and PBS. The results of FT-IR and DSC proved that the PBS and PCL were mixed so that the PBS/PCL microcapsules were composed of two wall-forming materials. And the release rate of indomethacin from the microcapsules was decreased with increasing the PCL content. It was noted that an addition of PCL on the PBS led to the decrease of pore size in the PBS/PCL microcapsules.     

热敏显色微胶囊的制备与表征

热敏显色微胶囊是用于传真、条形码系统、医用图像、各种打印等领域的重要材料,它是一种内部含有染料隐色体的球形胶囊。染料隐色体是一种内酯结构的无色染料,在一定条件下,与显色剂发生显色反应。由于染料隐色体的化学惰性不够理想,易受外界因素的干扰,因而在应用中受到一定限制,所以为了克服其存在的不足,常将其微胶囊化。微胶囊的芯壁结构可以将芯材与外界隔离,提高芯材的稳定性,同时保留芯材原有的化学性质。当环境温度在微胶囊的玻璃化温度以上时,由于形成微胶囊壁的物质透过性显著增加,因此显色成分接触而发生显色反应。本文利用界面聚合法,以聚乙烯醇为保护胶体,曲拉通X-100为表面活性剂,聚氨酯为壁材,染料隐色体为芯材,合成了聚氨酯热敏显色微胶囊。研究了三个主要因素对微胶囊的粒径及其分布、表面形貌和热敏显色性能的影响。结果表明,增大保护胶体浓度,提高乳化速度,增加乳化剂用量,微胶囊的平均粒径变小,粒径分布变窄,表面变得光滑而且致密,具有较高的热敏显色密度。利用红外光谱仪确认了微胶囊的结构,在最优条件下,所制备的微胶囊玻璃化温度为131 ℃,并具有良好的热稳定性。     

Effect of oxygen plasma treatment on the release behaviors of poly(epsilon-caprolactone) microcapsules containing tocopherol

The biodegradable poly(epsilon-caprolactone) microcapsules (PCL) containing tocopherol (TC) were prepared by emulsion solvent evaporation method, and microcapsules were treated by oxygen plasma to enhance the hydrophilic microcapsules. The morphologies and thermal properties of the microcapsules were determined by SEM and DSC measurements. The microcapsules studied were characterized by surface free energy or work of adhesion through contact angle measurement. As a result, the features of the microcapsules could be adjusted by manufacturing condition, such as surfactant and core ratio. The surface free energy or work of adhesion of the microcapsules was increased with increasing the time of plasma treatment, which could be attributed to the increased hydrophilic groups during oxygen plasma treatment. The release profile of the microcapsules was determined by UV-vis spectroscopy and the microcapsules containing tocopherol showed the rapid release rate, as compared with untreated ones.     

Properties of poly(lactic acid-co-glycolic acid) film modified by blending with polyurethane

A number of poly(lactic acid-co-glycolic acid)/polyurethane (PLGA/PU) blend films with various PU mole contents were prepared by casting the polymer blend solution in chloroform. The surface morphologies of the PLGA/PU blend films were studied by scanning electron microscopy (SEM). The thermal, mechanical and chemical properties of the PLGA/PU blend films were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), tensile tests and surface contact angle tests. The results revealed that the introduction of PU could markedly modify the properties of PLGA films.     

Microwave-assisted synthesis of poly(urea-formaldehyde)/lauryl alcohol phase change energy storage microcapsules

In this study, lauryl alcohol suitable for thermal energy storage applications was microencapsulated in a poly(urea-formaldehyde) shell. The microcapsules were prepared by microwave-assisted in situ polymerization. The morphology and particle size of the poly(urea-formaldehyde)/lauryl alcohol phase change energy storage microcapsules(UF/LA PCESMs) were analyzed using transmission electron microscopy, scanning electron microscopy, atomic force microscopy and dynamic light scattering. The latent heat storage capacities of lauryl alcohol and UF/LA PCESMs were determined using differential scanning calorimetry. The chemical composition of the microcapsules was characterized using Fourier transform infrared spectroscopy. All of the results show that UF/LA PCESMs were synthesized successfully and that the latent heat storage capacity and encapsulation efficiency were 156.0 J/g and 75.0%, respectively, and the diameter of each microcapsule was around 150 nm.     

Preparation and characterization of biodegradable poly(l-lactide)/poly(ethylene glycol) microcapsules containing erythromycin by emulsion solvent evaporation technique

In this work, the producing of a biodegradable poly(l-lactide) (PLA)/poly(ethylene glycol) (PEG) microcapsule by emulsion solvent evaporation method was investigated. The effect of PEG segments added to the PLA microcapsules on the degradation, size distribution, and release behavior was studied. According to the results, PLA/PEG copolymer was more hydrophilic than PLA homopolymer, and with lower glass transition temperature. The surface of PLA/PEG microcapsules was not as smooth as that of PLA microcapsules, the mean diameters of prepared PLA and PLA/PEG microcapsules were 40 and 57 microm, respectively. And spherical forms were observed by the image analyzer and the scanning electron microscope (SEM). Drug release from microcapsules was affected by the properties of PLA/PEG copolymers determined by UV-vis spectra. It was found that the drug release rates of the microcapsules were significantly increased with adding of PEG, which explained by increasing hydrophilic groups.     

Thermal stability of microencapsulated epoxy resins with poly(urea-formaldehyde)

A series of microcapsules filled with epoxy resins with poly(urea-formaldehyde) (PUF) shell were synthesized by in situ polymerization, and they were heat-treated for 2 h at 100 °C, 120 °C, 140 °C, 160 °C, 180 °C and 200 °C. The effects of surface morphology, wall shell thickness and diameter on the thermal stability of microcapsules were investigated. The chemical structure and surface morphology of microcapsules were investigated using Fourier-transform infrared spectroscope (FTIR) and scanning electron microscope (SEM), respectively. The thermal properties of microcapsules were investigated by thermogravimetric analysis (TGA and DTA) and by differential scanning calorimetry (DSC). The thermal damage mechanisms of microcapsules at lower temperature (<251 °C) are the diffusion of the core material out of the wall shell or the breakage of the wall shell owing to the mismatch of the thermal expansion of core and shell materials of microcapsules. The thermal damage mechanisms of microcapsules at higher temperature (>251 °C) are the decomposition of shell material and core materials. Increasing the wall shell thickness and surface compactness can enhance significantly the weight loss temperatures (T_d) of microcapsules. The microcapsules with mean wall shell thickness of 30 ± 5 μm and smoother surface exhibit higher thermal stability and can maintain quite intact up to approximately 180 °C.     

Effect of poly(ethylene oxide) on the release behaviors of poly(epsilon-caprolactone) microcapsules containing erythromycin

The biodegradable poly(epsilon-caprolactone) (PCL)/poly(ethylene oxide) (PEO) microcapsules and the analyzing of form and features for the manufacturing conditions were investigated in a prospective drug delivery systems (DDS) through drug release. The effects of emulsifier, emulsifier concentration, and stirring rate on the diameter and form of the microcapsules were examined using image analyzer (IA) and scanning electron microscope (SEM). The role of interfacial adhesion between PCL/PEO and drug was determined by contact angle measurements, and the drug release rate of the microcapsules was characterized by UV-vis spectroscopy. As a result, the microcapsules were made in spherical forms with a mean particle size of 170 nm approximately 68 microm. And the work of adhesion between water and PCL/PEO was increased with increasing the PEO content, which is due to higher hydrophilicity of PEO. The drug release rate of the microcapsules was significantly increased as the PEO content increased, which could be attributed to the increasing of the hydrophilic groups or the degree of adhesion at the interfaces.     

Preparation,thermal property,and thermal stability of microencapsulated n-octadecane with poly(stearyl methacrylate) as shell

This study focused on preparation and thermal properties of poly(stearyl methacrylate) shell (PSMA) microcapsules containing n-octadecane as a phase change material (PCM). Pentaerythritol triacrylate (PETA) and divinylbenzene (DVB) were employed as crosslinking agents. The surface morphologies, particle sizes, and distributions of the microencapsulated phase change material (microPCM) were studied by scanning electron microscopy. The thermal properties, thermal reliabilities, and thermal stabilities of the microPCMs were investigated by differential scanning calorimetry and thermal gravimetric analysis. The microPCM with DVB exhibits higher phase change enthalpies of melting (87.9 J g^?1) and crystallization (94.8 J g^?1) and a greater thermal stability in comparison with the microPCM with PETA. The phase change temperatures and enthalpies of the microPCMs varied little after thermal cycles. Thermal images showed that the gypsum board with PSMA/n-octadecane microPCM possessed temperature-regulated property. Therefore, microencapsulated n-octadecane with PSMA as shell has good thermal energy storage and thermal regulation potential.     

Preparation and characterization of poly(melamine-formaldehyde) microcapsules filled with propisochlor

A novel propisochlor microcapsules suspension (CS) was prepared via in-situ polymerization. The preparation of melamine-formaldehyde resin microcapsules containing propisochlor with different ratios of core-shell material was investigated. The synthesized microcapsules were characterized by Fourier Transform Infrared spectrometer, Scanning Electron Microscope, Ultraviolet spectrometry, Thermogravimetric analyses and particle size analyzer. As the ratio of core/shell was 1, the diameter of the prepared microcapsules was the smallest (3.55?µm), while narrowest size distribution (span: 1.19) and the melamine formaldehyde microcapsules possessed the highest encapsulation efficiency (93.26%). The surface of the microcapsules was smooth and the microcapsules had poor adhesion. These microcapsules had compact microstructures and global shapes, which had a good thermal stability and propisochlor could be preserved better in the poly(melamine-formaldehyde) (PMF) microcapsules. These results indicated that the prepared microcapsule had better performance. Additionally, the propisochlor was easily degraded through microorganisms and had a short half-life. The microcapsule suspension of propisochlor hasn’t been researched yet. Therefore, it is significant to prepare microcapsule suspension. The technology of controlled release has effectively prolonged the persistence of active ingredients. More importantly, there is no use of organic solvents in the preparation of microcapsules suspension, which avoided the pollution of solvents to the ecological environment.     

硬脂酸丁酯微胶囊的制备与表征

采用原位聚合法用脲醛树脂包覆硬脂酸丁酯,制得相变储热微胶囊.利用激光粒径分布仪、扫描电镜、差示扫描量热仪(DSC)和傅立叶转换红外光谱仪分别研究了微胶囊的粒径分布、表面形态、热性能和壳结构.结果表明,所得微胶囊粒径分布均匀,表面光洁,具有良好的韧性和致密性.不同的制备工艺对微胶囊粒径分布有一定的影响,其中在28 000 r/m in下乳化5 m in时,所得微胶囊的粒径分布集中在1~4μm.DSC测定结果显示硬脂酸丁酯微胶囊的最大相变焓为68 J/g.     

Modification of hydrophilic poly(vinyl alcohol) film via blending with hydrophobic poly(butyl acrylate-co-methyl methacrylate)

A series of poly(vinyl alcohol)/poly(butyl acrylate-co-methyl methacrylate) [PVA/P(BA-co-MMA)] blend films with different P(BA-co-MMA) content were prepared by the solution casting method. Surface morphologies of the PVA/P(BA-co-MMA) blend films were studied by scanning electron microscopy and atomic force microscopy. Thermal, mechanical, and chemical properties of PVA/P(BA-co-MMA) blend films were investigated by differential scanning calorimeter, thermogravimetric analysis, tensile tests, and surface contact angle tests. It was revealed that the introduction of P(BA-co-MMA) could affect the properties of the PVA films. The results also showed that, when P(BA-co-MMA) mole content is 3 %, the tensile strength and the surface contact angle of the polymer blend film are 20.4 MPa and 43.5°, respectively, suggesting that the polymer blend film holds both a better mechanical property and a better chemical property.     

十八烷/聚(St-MMA)相变微胶囊制备及表征

采用乳液聚合的方法,分别选取聚苯乙烯(PS)、聚甲基丙烯酸甲酯(PMMA)或苯乙烯和甲基丙烯酸甲酯的共聚物为壁材,正十八烷为芯材,十二烷基苯磺酸钠(SDBS)为乳化剂,制作相变储能微胶囊。用粒径分析仪、透射电子显微镜(TEM)、热重分析仪(TG)和示差扫描量热测试仪(DSC)对微胶囊的形貌、相变热性能和热稳定性分别进行表征。结果表明:壁材选取两者共聚物,当两种单体的比例为St∶MMA=1∶5,SDBS用量为1.5g(总质量的3%)时,微胶囊粒径大小均匀,粒子分散性好,壁材的包裹性好。微胶囊的放热峰为起始温度为27.3℃,终止温度为31.9℃,相变温度为28.9℃,相变焓为48.4J/g。TG表明长期使用温度不能超过131℃。IR分析微胶囊中含有芯材和壁材。这种十八烷/聚(St-MMA)相变微胶囊可以用于诸能材料。     

Morphology and properties of nanostructured materials based on polypropylene/poly(butylene succinate) blend and organoclay

Nanostructured materials based on organically modified montmorillonite (OMMT) and polypropylene (PP)/poly(butylene succinate) (PBS) blend were prepared via melt-mixing of PP, PBS, and OMMT in a batch mixer. The weight ratio of PP and PBS was 70:30, and the OMMT loading varied from 0.5 to 5 wt%. The surface morphologies of unmodified and OMMT-modified blend were studied by field-emission scanning electron microscopy. Results showed that the particle size of the dispersed PBS phase was significantly reduced with the addition of a small amount of OMMT (1.5 wt%). Upon the addition of 5 wt% of OMMT, the domain size of the dispersed PBS phase changed significantly from the unmodified blend, and a homogeneous dispersion of very fine particles of PBS was observed. The degree of dispersion of silicate layers in the blend matrix was characterized by X-ray diffraction and transmission electron microscopy. The improved adhesion between the phases and the fine morphology of the dispersed phase contributed to the significant improvement in the properties and thermal stability of the final nanocomposite materials. On the basis of these results, we describe a general understanding of how the morphology is related to the final properties of OMMT-incorporated PP/PBS blend.     

Performance of biodegradable microcapsules of poly(butylene succinate), poly(butylene succinate-co-adipate) and poly(butylene terephthalate-co-adipate) as drug encapsulation systems

Poly(butylene succinate) (PBSu), poly(butylene succinate-co-adipate) (PBSA) and poly(butylene terephthalate-co-adipate) (PBTA) microcapsules were prepared by the double emulsion/solvent evaporation method. The effect of polymer and poly(vinyl alcohol) (PVA) concentration on the microcapsule morphologies, drug encapsulation efficiency (EE) and drug loading (DL) of bovine serum albumin (BSA) and all-trans retinoic acid (atRA) were all investigated. As a result, the sizes of PBSu, PBSA and PBTA microcapsules were increased significantly by varying polymer concentrations from 6 to 9%. atRA was encapsulated into the microcapsules with an high level of approximately 95% EE. The highest EE and DL of BSA were observed at 1% polymer concentration in values of 60 and 37%, respectively. 4% PVA was found as the optimum concentration and resulted in 75% EE and 14% DL of BSA. The BSA release from the capsules of PBSA was the longest, with 10% release in the first day and a steady release of 17% until the end of day 28. The release of atRA from PBSu microcapsules showed a zero-order profile for 2 weeks, keeping a steady release rate during 4 weeks with a 9% cumulative release. Similarly, the PBSA microcapsules showed a prolonged and a steady release of atRA during 6 weeks with 12% release. In the case of PBTA microcapsules, after a burst release of 10% in the first day, showed a parabolic release profile of atRA during 42 days, releasing 36% of atRA.     

Synthesis of poly(vinylidene chloride)-based composite latexes by emulsion polymerization from epoxy functional seeds for improved thermal stability

Poly(glycidyl methacrylate-co-butyl methacrylate)/poly(vinylidene chloride-co-methyl acrylate) (poly(GMA-co-BMA)/poly(VDC-co-MA)) composite latexes have been successfully synthesized via a two-stage emulsion polymerization process. In a first step, emulsion copolymerization of GMA and BMA was carried out in optimized conditions (low temperature, neutral pH, starved-feed conditions) to both limit the hydrolysis of epoxy groups and obtain small particle size (typically 30-50 nm size range). Composite latexes were then obtained by a second-stage seeded copolymerization of VDC and MA in the presence of tetrasodium pyrophosphate to control the pH and reach high molecular weight, leading to partial encapsulation of the seed particles (snow-man morphology, in agreement with theoretical expectations). Thermogravimetric analyses performed on the resulting composite particles showed that the epoxy-functionalized seed polymer behaved as an efficient thermal stabilizer of PVDC.     

Characterization of ovalbumin-containing polyurethane microcapsules with different structures

Ovalbumin (OVA)-containing polyurethane microcapsules were successfully prepared by a reaction between toluene diisocyanate (TDI) and different polyols such as glycerol, ethane diol, and propylene glycol. The structural and thermal properties of the resultant microcapsules and the release profile of the OVA from the wall membranes were studied. In conclusion, the microcapsules from the glycerol showed the highest thermal stability, with the formation of many hydrogen bonds. From the data of release profiles, it was confirmed that the particle size distribution and morphologies of microcapsules determined the release profiles of the OVA from the wall membranes.     

Reactive poly(glycidyl methacrylate) microspheres prepared by dispersion polymerization

Poly(glycidyl methacrylate) [poly(GMA)] microspheres of narrow size distribution were prepared in a simple one‐step procedure by dispersion radical polymerization. Depending on the solvent used, poly(GMA) particle size could be controlled in the range of 0.5–4 μm by changing the solubility parameter of the reaction mixture. In N,N′‐dimethylformamide (DMF)/methanol mixture, the particle size increased and the size distribution broadened with decreasing initial solubility parameter. While in the DMF/methanol solvent system, hydroxypropyl cellulose (HPC) or cellulose acetate butyrate (CAB) were taken as steric stabilizers of the dispersion polymerization, poly(vinylpyrrolidone) (PVP) was used in alcoholic media. Contrary to the DMF/methanol system, narrow particle size distributions were obtained with PVP‐stabilized polymerizations in ethanolic, methanolic, propan‐1‐olic or butan‐1‐olic medium. Both the particle size and polydispersity were reduced with increasing stabilizer concentration. If lower molecular‐weight PVP was used, larger microspheres were obtained. Poly(GMA) samples prepared in a neat alcoholic medium virtually quantitatively retained oxirane group content after the polymerization. Reactivity of the poly(GMA) microspheres was confirmed by their hydrolysis and aminolysis. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 3855–3863, 2000     

The effect of mono-sized liquid crystal domains on electro-optical properties in a polymer dispersed liquid crystal prepared by using monodisperse poly(methylmethacrylate)/liquid crystal microcapsules

Highly mono-sized poly(methyl methacrylate) (PMMA)/liquid crystal (LC) microcapsules having a mono-sized single LC domain were prepared by the solute codiffusion method and solvent evaporation. The size of the LC domain in the microcapsules could be controlled by the amount of LC introduced during the swelling stage. The electro-optical properties of the polymer dispersed liquid crystal (PDLC) prepared by using the microcapsules was highly improved. In particular, the threshold voltage was lowered and the switching behaviour with an applied electric field was sharpened drastically compared with PDLC prepared simply by solvent evaporation-induced phase separation.     

The effect of mono-sized liquid crystal domains on electro-optical properties in a polymer dispersed liquid crystal prepared by using monodisperse poly(methylmethacrylate)/liquid crystal microcapsules

Highly mono-sized poly(methyl methacrylate) (PMMA)/liquid crystal (LC) microcapsules having a mono-sized single LC domain were prepared by the solute codiffusion method and solvent evaporation. The size of the LC domain in the microcapsules could be controlled by the amount of LC introduced during the swelling stage. The electro-optical properties of the polymer dispersed liquid crystal (PDLC) prepared by using the microcapsules was highly improved. In particular, the threshold voltage was lowered and the switching behaviour with an applied electric field was sharpened drastically compared with PDLC prepared simply by solvent evaporation-induced phase separation.