气体抗溶剂法制备乙基纤维素微细颗粒

利用超临界流体制备微细颗粒是一门新兴的技术,将其中的气体抗溶剂（GAS）法首次应用于制备乙基纤维素微粒,在系统的近临界和超临界范围进行了较为详细的实验研究.在实验范围内,制得微粒的平均粒径为2～15 μm.研究得到温度、压力、不同有机溶剂对微粒粒径及其分布的影响,并应用相平衡知识对结果进行了分析和讨论.此研究为制备粒径较小,具有缓释、靶向、黏附等功能的乙基纤维素含药微粒做了准备.     

体抗溶剂法制备乙基纤维素微细颗粒

利用超临界流体制备微细颗粒是一门新兴的技术 ,将其中的气体抗溶剂 (GAS)法首次应用于制备乙基纤维素微粒 ,在系统的近临界和超临界范围进行了较为详细的实验研究 .在实验范围内 ,制得微粒的平均粒径为 2～ 15 μm .研究得到温度、压力、不同有机溶剂对微粒粒径及其分布的影响 ,并应用相平衡知识对结果进行了分析和讨论 .此研究为制备粒径较小 ,具有缓释、靶向、黏附等功能的乙基纤维素含药微粒做了准备 .     

超临界流体技术及其在生物工程中的应用

介绍了在生物工程有着广泛的应用前景的多种超临界流体技术，包括提取生物活性物质的超临界流体萃取，超临界条件二氧化碳中制备手性药物制备和淀粉水解制取葡萄糖的非水酶催化反应，超临界水条件下纤维素水解制备葡萄糖，超临界流体中的细胞破碎，制备缓释药物和色说载体的超临界流体溶液快速膨胀和气体抗溶剂结晶和沉淀技术。     

超临界流体强制分散溶液技术及其在药物领域的应用

超临界流体强制分散溶液技术以其独特的优点,在药物超细化和微胶囊化等方面得到了广泛的应用。介绍了该技术的基本原理及工艺改进的研究情况,综述了该技术在药物及药物载体超细微粒和药物微囊制备方面的应用进展。利用SEDS过程能制备粒度分布窄的微米级甚至纳米级的微粒,能够将残留溶剂减小到非常低的质量浓度并且容易控制微粒粒径及粒度分布。     

超临界CO2抗溶剂法制备乙基纤维素微球试验

通过自行设计的超临界CO2微球制备装置,利用乙基纤维素丙酮混合溶液,制备了粒径偏差较小、表面光滑与球形度较好的乙基纤维素微球,采用正交试验讨论了温度、压力、溶液质量浓度、CO2流量对微球粒径与粒径分布的影响,分析了进气与进液方式对试验过程的影响。试验结果表明:改变工艺参数,可在较大范围内调控微球大小,所制微球平均粒径为0.2—2.6μm,粒径偏差为0.07—0.85μm;溶液质量浓度是主要影响因素;不同的汽液接触方式也将影响微球的大小。     

氮气增强溶液雾化技术制备聚乙二醇微粒

以超临界流体增强溶液分散技术为基础,用N2取代C02以实现该过程更好的雾化效果.实验研究以聚乙二醇(PEG6000)/丙酮溶液制备PEG微颗粒,探讨预膨胀压力和溶液流量对粒径及粒径分布的影响.结果表明,超临界N2增强的溶液雾化技术可以制得形态基本上为球形的PEG微粒,并且粒径分布可以方便地控制在1～5μm.PEG微粒随预膨胀压力增大而减少,粒径分布变窄;低PEG/丙酮溶液流量下制备的微粒粒径分布较窄.     

超临界流体在聚苯乙烯制备中的应用

综述了超临界流体在聚苯乙烯(PS)制备中的应用。超临界流体分级能方便地通过调节温度和压力对溶解度进行控制。获得相对分子质量分布较窄的PS级分;采用超临界流体可以连续稳定地制备纯度高和粒径分布均匀的微细PS;运用超临界溶液快速膨胀技术制得了微粒形态良好、粒径分布较窄的微米级PS微粒;采用超临界气体制备的微孔发泡PS复合材料具有较高的机械强度和性价比;PS超临界流体脱挥分具有能耗低、传质效率高的特点,而且不会引起聚合物的降解;使用超临界流体制备PS复合材料成为人们关注的研究热点。     

不同溶剂条件下利用SEDS法制备乙基纤维素微粒的实验研究

分别利用二氯甲烷、丙酮和乙醇作为溶剂采用超临界流体增强溶液分散法(SEDS)制备了乙基纤维素微粒,考察了不同压力、温度和溶剂条件下所制备微粒的粒径大小及形态。实验表明:在体系亚临界和超临界状态下制备的微粒粒径及形态完全不同;聚合物的玻璃化温度的降低对微粒的形态影响比较大;溶剂对微粒粒径及形态也有较大影响,特别是对可制备微粒的压力及温度的范围的影响。     

超临界溶液浸渍法制备缓释药物

超临界溶液浸渍法(supercritical solution impregnation,SSI)是一种将小分子物质负载到聚合物中的过程技术,主要是利用超临界流体的高扩散系数、低黏度及其对聚合物的溶胀作用,使小分子物质通过分子扩散作用迅速进入溶胀的聚合物并包裹于其中。近年来该技术已用于制备缓释药物/聚合物复合微球、薄膜和纤维等。该法的主要优点在于载体结构灵活,拓展了超临界技术在控释药物制备中的应用。本文主要介绍了SSI法的原理、流程及其在缓释药物制备中的应用,并展望了SSI法的发展趋势。     

喷雾干燥法制备磁性缓释微囊

目的:探索喷雾干燥技术制备壳聚糖磁性微囊的最佳工艺。方法:以微囊含水量、外形为评价指标,对喷雾干燥工艺参数进行单因素考察及正交优化设计。结果:最优工艺条件为壳聚糖浓度0.70%,进口温度为170℃出口温度95℃,进料速度15 r/min;壳聚糖微囊平均粒径为2.35μm,跨距0.43μm;磁场强度为300 mT时,磁性壳聚糖微囊磁化率为7.795×10-4cm3/g,制备的微囊外形好,包埋率为82.72%;在缓冲液中药物1 h释放量不超过30%,释放时间30 h。结论:制备工艺可行,微囊具有较好磁性能及缓释性。     

Preparation and properties of poly(propylene carbonate maleate) microcapsules for controlled release of pazufloxacin mesilate

A novel biodegradable aliphatic polycarbonate, poly(propylene carbonate maleate) (PPCMA) was synthesized by terpolymerization of carbon dioxide, propylene oxide, and maleic anhydride (MA), using a polymer supported bimetallic complex as catalyst. The utility of PPCMA to encapsulate and control the release of drug pazufloxacin mesilate (PZFX), via microcapsules, was investigated. PPCMA microcapsules containing PZFX were elaborated by solvent evaporation method based on the formation of double W/O/W emulsion. The manufacturing parameters such as the volume ratio of V(PPCMA) : V(PZFX), the concentration of stabilizer gelatin in outer aqueous phase played major roles on microcapsule characters, and were altered to optimize the process parameters. The PPCMA‐PZFX microcapsules were obtained with smooth and spherical surface under optimum condition, the mean diameter of microcapsules was ～ 2 μm, and the drug loading and drug encapsulation efficiency of the microcapsules were 22.9 ± 1.05% and 82.1 ± 2.03%, respectively. PZFX released from PPCMA microcapsules was found to reach 89.8 ± 2.89% after 36d in a pH 7.4 phosphate‐buffered solution, and the release profile obeyed the Higuchi equation. The results suggest that the new polymer PPCMA provides an alternative to degradable matrix polymers for long‐term sustained releasing drug delivery systems. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

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.     

Microcapsulated epoxy resin with nanosilica-urea formaldehyde composite shell

In this study, the epoxy microcapsules with the nanosilica (0, 1, 2, and 3 wt %)—urea formaldehyde composite shell were synthesized and then characterized by optical microscope (OM), field emission scanning electron microscope (FESEM), Fourier-transform infrared spectroscopy (FT-IR), and thermogravimetric analysis. According to the OM analysis, the without nanosilica microcapsules had the semitransparent structures and equal size distributions. Also, the formation of the microcapsule clusters and rupturing microcapsules in the sample containing 3 wt % nanosilica were observed by OM method. The FESEM analysis showed that without nanosilica, microcapsules had a smooth surface, whereas by increasing the percentage of nanosilica up to 2 wt %, the surface roughness was enhanced. It was also observed that on the surface of the microcapsules without nanosilica, two size ranges of the submicrocapsules with the average diameters of 1.12 μm and 208 nm were formed. By adding 1 wt % nanosilica, three size ranges of submicrocapsules were formed, with the average size of 2.63 μm, 824 and 179 nm. The interesting phenomena in the microcapsules containing 2 and 3 wt % nanosilica were the packing submicrocapsules with the polymeric shell and the formation of the microcapsule clusters, respectively. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48580.     

Optimization of microencapsulation of polyaspartic acid ester into UV curable epoxy-acrylate resin using Taguchi method of experimental design

Due to fast reaction with isocyanates, polyaspartic acid esters (PAAE) can be used for the development of microcapsules for self-healing coatings. Microcapsules with encapsulated PAAE into shell formed by UV-cured commercial epoxy-acrylate resin were produced through oil-in-water emulsion polymerization triggered by UV light. The obtained microcapsules were characterized by FTIR, TGA, optical microscopy, and SEM. Various encapsulation parameters, including core to shell ratio, agitation speed, emulsifier type and concentration, solvent type and its concentration in the oil phase, have been selected at four different levels. Microencapsulation was optimized using Taguchi L16 parameter design approach for determination of desired outcome as larger is better (maximal core content) and nominal is better (microcapsule diameter of 50 μm). It was determined that conditions to prepare microcapsules with the highest core content and the microcapsule size close to 50 μm are rather similar requiring core-to-shell ratio at about 4:1, low agitation speed of 500–1000 rpm, and the use of two polymeric emulsifiers poly(vinyl alcohol) and Gum Arabic at concentration of about 2%. Primary benefits of UV-induced shell formation during microencapsulation of active compounds are remarkably shorter time of the process and possibilities to reach high core content and prepare microcapsules of desirable size.     

一步法制备聚脲甲醛包覆反应性乙烯基硅油微胶囊

以聚脲甲醛(PUF)为囊壁,乙烯基硅油为囊芯,采用原位聚合"一步法"成功制备出具有自修复功能且粒径均匀的新型PUF包覆乙烯基硅油微胶囊。研究了分散剂/表面活性剂种类及用量、m(囊芯)∶m(囊壁)比例对微胶囊物理性能的影响,并通过扫描电镜(SEM)、金相显微镜、激光粒度分析仪和红外光谱(FT-IR)法等对微胶囊的形貌、粒径大小等进行了研究。结果表明:选用较高浓度的聚乙烯醇(PVA1799)作为分散剂时,有利于微胶囊的形成;当w(PVA1799)=3.00%(相对于体系总质量而言)、m(囊芯)∶m(囊壁)=2.8∶1.0时,在1500r/min条件下,可制备出平均粒径小于20μm且粒径分布较均匀的理想微胶囊。     

自修复微胶囊制备及微纳力学性能

采用一步原位聚合法制备了自修复微胶囊。应用光学显微镜、扫描电子显微镜和激光共聚焦显微镜对微胶囊壁厚、微结构进行了分析和表征。借助纳米探针对微胶囊及其壳材进行压痕实验测试其力学性能。结果表明,自修复微胶囊包裹完整,表面粗糙,微胶囊平均粒径为100μm,平均壁厚为10μm,微胶囊修复剂芯材含量约为75%;纳米压痕分析显示微胶囊的弹性模量比环氧树脂的略小,说明了当环氧树脂基体内裂纹扩展时,裂纹更易于向微胶囊扩展,证明了环氧树脂微裂纹打开微胶囊释放修复剂的可行性。     

Development of self-healing coatings based on urea-formaldehyde/polyurethane microcapsules containing epoxy resin

In this study, the synthesis of urea-formaldehyde/polyurethane (UF/PU) microcapsules containing epoxy resin for self-healing and anti-corrosion coatings with good stability has been reported. Spherical microcapsules were prepared with a diameter of about 50–720 μm and a shell thickness of 0.6–0.7 μm via in situ polymerization in an oil-in-water emulsion using 2,4-toluene diisocyanate-based pre-polymer along with the urea-formaldehyde. Scanning electron microscopy (SEM) and optical microscopy (OM) were employed to evaluate the shape and morphology of the microcapsules. Fourier transform infrared (FTIR) spectroscopy showed the absence of free isocyanate groups within the microcapsule shell confirming the completion of shell formation reactions. OM illustrated that the microcapsules were stable over a period of 30-days in toluene and xylene. Increasing microcapsule loading improved crack repairing and anti-corrosion performance of the coating layer. Low-carbon steel coupons coated with an epoxy resin containing 10 wt% microcapsules and scribed using a scalpel blade showed no visible sign of corrosion after up to 5 weeks of exposure in a standard salt spray test chamber.     

一种蜜胺树脂为壁材的相变储热微胶囊致密性研究

采用原位聚合法用蜜胺树脂包覆了一种相变点为24℃,相变热为225 5J/g的有机复合相变材料,并对所制备的相变储热微胶囊的致密性进行了研究。利用扫描电子显微镜对微胶囊的表面形态进行了观察;用722型分光光度计对不同工艺条件下所得微胶囊在密度为0.79g/mL乙醇中的渗透性进行了研究;采用压力法观察微胶囊在受压后的表面形貌,对其强度进行了评价。结果表明:相变储热微胶囊呈均匀的球形,表面光滑且致密,平均粒径110μm;由于蜜胺树脂有大的交联密度,微胶囊在乙醇中渗透缓慢,证明芯材包覆效果好,同时发现双层壁材微胶囊的致密性优于单层壁材的微胶囊;平均粒径为10μm的优于平均粒径为1μm的;随着壁材用量的增大,渗透性减弱,但为了保证相变储热微胶囊的储热效果,芯材与壁材质量比以3为好。所制备的微胶囊可以承受1 96×105Pa的压力而不破损。     

季铵化壳聚糖包覆腐殖酸微胶囊的制备与性能研究

以季铵化壳聚糖（QCTS）为壁材、腐殖酸(HA)为芯材,制备季铵化壳聚糖包覆腐殖酸(QCTS/HA)微胶囊。采用傅里叶红外光谱(FTIR)、偏光显微镜(POM)、扫描电子显微镜(SEM)对微胶囊的性能进行表征。以芯壁比〔m(HA):m(QCTS)〕、固化剂用量和搅拌速度作为单因素,探讨了微胶囊的最佳制备条件。并且对最佳制备条件下的微胶囊进行了形貌观测以及吸水和保水性能测试。结果表明,QCTS/HA微胶囊的最佳工艺参数为：m(HA):m(QCTS)=3:1,固化剂用量为总质量的1%,搅拌速度为500r/min;与相同条件下未改性的微胶囊CTS/HA相比,改性后的QCTS/HA微胶囊包覆层表面孔隙结构比较完善,分布均匀,孔洞较多,具有更加优异的吸水和保水性能,其12h的吸水率和保水率分别高达348%和208%。 关键词：季铵化壳聚糖;腐殖酸;核壳结构;微胶囊;吸水性能,保水性能     

Synthesis and characterization of chitosan/urea‐formaldehyde shell microcapsules containing dicyclopentadiene

Microcapsules containing healing agent have been used to develop the self‐healing composites. These microcapsules must possess special properties during the use of composites such as stability in surrounding, appropriate mechanical strength, and lower permeability. A new series of microcapsules containing dicyclopentadiene with chitosan/urea‐formaldehyde copolymer as shell materials were synthesized by in situ copolymerization technology. The microencapsulating mechanism was discussed and the process was explained. Also, the factors influencing the preparation of microcapsules were analyzed. The morphology and shell wall thickness of microcapsules were observed by using scanning electron microscopy. The size of microcapsules was measured using optical microscope and the size distribution was investigated based on data sets of at least 200 measurements. The chemical structure and thermal properties of microcapsules were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis, respectively. The storage stability and isothermal aging experiment of microcapsules were also investigated. Results indicted that the chitosan/urea‐formaldehyde microcapsules containing dicyclopentadiene were synthesized successfully; the copolymerization occurred between chitosan and urea‐formaldehyde prepolymer. The microcapsule size is in the range of 10–160 μm with an average of 45 μm. The shell thickness of microcapsules is in the range of 1–7 μm and the core content of microcapsules is 67%. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011