利用新型膜乳化器制备粒径均一的PLGA微球

用恒流泵替代气瓶给压装置得到新型膜乳化器,以改善膜乳化法制备微球的工艺稳定性;以聚乳酸-羟基乙酸共聚物(PLGA)为膜材,利用水包油(O/W)乳化法制备PLGA微球,研究了新型膜乳化器与传统膜乳化器对微球形貌、粒径及粒径分布的影响,考察了搅拌速度、稳定剂浓度、PLGA浓度及分散相流速对微球形貌、粒径及其分布的影响.结果表明,在微孔膜孔径2mm、搅拌速度300 r/min、稳定剂浓度1.0%(w)及PLGA浓度60 mg/m L、分散相流速20mL/h的条件下,可制得表面光滑、粒径均一(粒径分布系数Rspan0.50)的PLGA微球,各批产品的粒径相对标准偏差为1.99%,产品批次重复性良好.     

微孔膜乳化与悬浮聚合结合法制备均一PST-DVB多孔微球

使用自制的微孔膜乳化装置,通过微孔膜乳化结合悬浮聚合方法,批量制备了微米级的聚(苯乙烯-二乙烯基苯)(PST-DVB)微球. 实验中采用孔径为5.2 mm的微孔膜,考察了膜线剪切力、管线速度和膜乳化压力对微球粒径及其分布的影响,以及膜乳化压力和膜线剪切力对分散相流速的影响. 研究结果表明,膜线剪切力在合适的范围内对微球粒径影响不大,而管线速度在14.38~26.49 m/min之间、膜乳化压力在0.008~0.012 MPa之间时,所制备微球的尺寸均一. 研究还发现膜乳化压力是影响分散相流速的最主要因素. 研究结果为装置的规模化放大奠定了理论基础.     

微孔膜乳化法制备大粒径琼脂糖微球

以6%的琼脂糖溶液为水相,不同体积配比的液体石蜡(LP)和石油醚(PE)的混合溶液为油相,PO-5S为乳化剂,采用微孔膜乳化法制备了平均粒径为90 mm的琼脂糖微球. 考察了SPG膜孔大小、油相组成、反应温度、压力等因素对成球粒径及其分布的影响. 结果表明,在使用膜孔为25.9 mm的微孔膜、LP/PE体积比为11:1及65℃的条件下可制得均一的大粒径琼脂糖微球,微球平均粒径为93.3 mm,粒度分布系数为1.25,且各批产品的相对标准偏差仅为1.34%,产品重复性良好.     

辐射余热回收用相变微胶囊的制备与表征

用原位聚合法制备了以58号石蜡为芯材、脲醛树脂为壁材的微胶囊。基于正交实验法得到了九组样品,并且对微胶囊产物的化学组成、相变特性、微观形貌和粒径分布进行了测试分析,考察了芯壁比、聚合反应温度、乳化搅拌转速和乳化剂添加量等因素对微胶囊制备过程及产物性能的影响。得到较佳的微胶囊产物为白色粉末,平均粒径81. 3μm,部分颗粒为球形,相变潜热约90 J/g。为得到适用于辐射余热回收的相变微胶囊,还需进一步优化制备工艺。     

对原位聚合法制备微胶囊技术的研究

本文讨论了用原位聚合法制备微胶囊的工艺，研究了影响微胶囊粒径大小，分布和影响微胶囊释放性能的各种因素。实验结果表明：随乳化分散剂用量的增加，搅拌速度和搅拌时间的增加，微胶囊粒径变小，粒径分布变窄。微胶囊壁材的聚合反应速率大，交联密度高，则孔隙率大，释放速率快；而壁膜厚度增大，则其释放速率减慢。     

快速膜乳化法制备尺寸均一及结构可控聚苯乙烯微粒

以苯乙烯为单体、二乙烯基苯为交联剂,采用快速膜乳化法制备了聚苯乙烯微粒,对其粒径分布、制备重复性、颗粒结构进行了表征,并考察了致孔剂种类及用量对不同粒径颗粒形态结构的影响规律. 结果表明,聚苯乙烯颗粒粒径与所用膜孔径呈线性关系,最佳乳化压力与膜孔径呈反函数关系. 优化工艺条件下所制颗粒粒径为1~6 mm,粒径分布系数均小于0.8,批次相对标准偏差低于3%. 体积效应对小粒径颗粒的成型结构影响较大;粒径越小,颗粒成型时致孔剂与聚合物间的相分离程度越低,颗粒粒径小于2 mm时液体石蜡无法形成完整颗粒,颗粒粒径大于2 mm时十六烷用量在60%(w)以下才能形成大孔结构.     

成囊工艺对环氧树脂微胶囊形成状态影响

研究了分散、乳化条件及成囊工艺对以苯乙烯为壁材,采用原位聚合法制备苯乙烯微胶囊状态的影响。讨论了不同乳化剂及其配比,不同乳化分散时间、搅拌速度和固化温度对微胶囊的包覆率、粒径的大小及分布情况的影响,最终确定以阿拉伯树胶和DBS按1∶3的比例混合作为乳化剂,1500 r/min搅拌,分散乳化60 min,85℃固化3 h作为制备环氧树脂微胶囊的优化工艺条件。在此条件下得到平均粒径为15μm左右,粒度分布均匀的球形微胶囊,包覆率在80%以上。     

一体化陶瓷外膜乳化装置制备O/W型乳状液

引　言膜乳化技术是将分散相以很小的压力压过膜孔 ,在膜表面形成微小的液滴 ,并通过剪切力的作用使小液滴从膜表面脱落而进入连续相的新型乳化技术 .该方法具有低能耗、低剪切力、需要表面活性剂较少、生成的乳液颗粒均匀等特性[1,2 ] ,所用的膜主要有微孔玻璃膜[3] 和陶瓷膜两种[4 ] .微孔玻璃膜的孔径分布较窄 ,通常在小于平均孔径±15 %的范围内变化 ,因此制备出的乳状液粒径分布较窄 ,但对称膜固有的高阻力导致膜的通量较小(通常在 2～ 4 0L·m- 2 ·h- 1) ,制约了其在工业领域的应用 .而陶瓷膜由于具有较高的通量被较多地用于工业化…     

乳化条件对正十八烷微胶囊制备的影响

以正十八烷为囊芯,密胺树脂(MF)为高分子囊壁材料,采用原位聚合法制备了相变材料微胶囊。利用光学显微镜、激光粒度分布仪、差示扫描量热仪和傅立叶变换红外光谱仪分别研究了微胶囊的表面形貌、粒径分布、相变性能和化学结构等。讨论了乳化方式和乳化剂种类对微胶囊性质的影响。结果表明:当采用十二烷基苯磺酸钠为乳化剂,将预聚物与熔融的正十八烷混合后再乳化时,所得微胶囊结构完好,粒径分布均匀,体积平均粒径约为150μm,囊芯含量高达67.3(wt)%。     

膜乳化法制备单分散聚苯乙烯多孔微球

为了解决用传统方法制备微球粒径不均的缺点，实验使用自制的膜乳化装置，通过膜乳化法制备粒径在12～20μm、单分散系数小于20％的聚苯乙烯多孔微球．使用扫描电镜考察多孔微球的表面形貌及孔径．结果表明：膜孔径是影响微球粒径的决定性因素；适当的膜乳化压力、乳化剂和分散剂浓度是生产粒径均一微球的重要条件；在致孔剂DBP质量分数为20％时，微球的平均孔径为0．12μm．     

In situ polymerization of uniform poly(urea–formaldehyde) microcapsules containing paraffins under the high-speed agitation without emulsifier

In this paper, uniform spherical poly(urea–formaldehyde) (PUF) microcapsules containing paraffins, which can be used as phase change materials for energy storage, were prepared by in situ polymerization method under high-speed agitation (≥10,000?rpm) without emulsifier. The influence of high-speed agitation on particle size of as-prepared microcapsules and the tightness of microcapsules were also investigated. The results show that, all the microcapsules have <10?μm mean particles-size and narrow-size distribution, and the mean particle size decreases with the increase of agitation rate. Furthermore, when the agitation rate is >16,000?rpm, the effectiveness of reducing particle size by high-speed stirring is not as remarkable as that of lower speed agitation. In order to gain good tightness of PUF microcapsules under the high-speed agitation conditions, the final pH value of reaction solution should be lower down compared with that of conventional agitation. In our investigation, when the agitation rate was 10,000?rpm, microcapsules fabricated at pH value <2.0 were sealed and own good tightness, however, those fabricated at pH value >2.2 were not sealed.     

快速膜乳化法制备粒径均一的PLGA微球和微囊

以聚(乳酸-羟基乙酸)(PLGA)为膜材,采用快速膜乳化结合溶剂萃取法制备了胰高血糖素样肽-1(GLP-1)微囊,研究了PLGA分子量对药物装载率、药物活性和体外释放行为的影响. 制备均一微球的优化条件为过膜压力1000 kPa,过膜次数3次,外水相稳定剂聚乙烯醇浓度19 g/L,油水体积比1:5. 在此条件下,制备了粒径350 nm左右、多分散系数小于0.050的载GLP-1的PLGA微囊,GLP-1包埋率达65%以上,活性保留达85%以上,药物体外释药可达20 d.     

Preparation and properties of phase‐change heat‐storage UV curable polyurethane acrylate coating

Phase‐change heat‐storage UV curable polyurethane acrylate (PUA) coating was prepared by applying microencapsulated phase change materials (microPCMs) to PUA coating. MicroPCMs containing paraffin core with melamine‐formaldehyde shell were synthesized by in situ polymerization. The effect of stirring speed, emulsification time, emulsifier amount, and core/shell mass ratio on particle size, morphology, and phase change properties of the microPCMs was studied by using laser particle size analyzer, Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopic analysis, scanning electron microscopy, and differential scanning calorimetry. The results showed that the diameter of the microcapsules decreased with the increase of stirring speed, emulsification time, and emulsifier amount. When the mass ratio of emulsifier to paraffin is 6%, microcapsules fabricated with a core/shell ratio of 75/25 have a compact surface and a mean particle size of 30 μm. The sample made under the above conditions has a higher efficiency of microencapsulation than other samples and was applied to PUA coating. The dispersion of microPCMs in coating and heat‐storage properties of the coating were investigated. The results illustrated that the phase‐change heat‐storage UV curable PUA coating can store energy and insulate heat. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41266.     

水泥基用相变微胶囊的颗粒特征与热力学性能

以石蜡、癸酸为芯材,脲醛树脂为壁材,间苯二酚为固化剂,采用原位聚合法制备相变微胶囊,采用ESEM、DSC、TGA来研究相变微胶囊颗粒形貌、粒径分布、热力学性能,以及相变微胶囊掺入水泥基体中的微观形貌.结果表明:微胶囊表面光滑,结构紧致;石蜡微胶囊的相变温度和相变焓分别是54.6℃和61.43 J/g,而癸酸微胶囊的相.变温度和相变焓分别是29.7℃和90.73 J/g;加入固化剂使得微胶囊产率从50％提升到78％以上;30次温度循环石蜡微胶囊相变晗无损失,癸酸微胶囊相变焓损失了31％;微胶囊在水泥基中分布均匀,形貌保存良好.     

Controllable preparation of uniform polystyrene nanospheres with premix membrane emulsification

The expansion of polymer nanosphere applications requires facile and versatile preparation techniques. In this study, combining circled premix membrane emulsification and thermally initiated miniemulsion polymerization, we developed a new strategy for preparing uniform polystyrene nanospheres within a duration as short as 1 h. The size of the nanospheres, ranging from 40 to 120 nm, was dependent on the premix membrane emulsification cycle number, the transmembrane flow rate, and the membrane pore size; this was almost consistent with characterizations of droplet size evolution. The coefficient of variation, around 15%, indicated that the size distribution of the nanospheres was still narrow, even as the monomer‐to‐water ratio was as high as 0.2. This method may be competitive for further applications because of its high production efficiency and low system requirements. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

快速膜乳化法制备载生长激素释放肽-6的PLGA微球

采用快速膜乳化法制备了聚(乳酸-羟基乙酸)(PLGA)微球,得到制备PLGA微球的优化条件为：过膜压力5 kPa,水相中PVA浓度19 g/L,油/水相体积比1:10,该条件下所制空白微球的平均粒径约为24 mm,粒径分布系数Span<0.7. 在此基础上制备载生长激素释放肽-6(GHRP-6)微球,油相乳化剂浓度2.5 g/L、外水相中NaCl浓度10 g/L条件下所制载GHRP-6微球包埋率最高可达85%,初乳制备方式对药物包埋率及体外释放行为均有较大影响,超声法制备的初乳所得微球内部结构紧密,药物包埋率较高(85%),但释药缓慢;而均质法制备的初乳所得微球内部结构疏松,药物包埋率较低(76.8%),但在体外释放更完全.     

微悬浮法制备有机颜料微胶囊中的粒径调控

为调控有机颜料微胶囊的粒径及其分布,在分析微悬浮聚合过程粒径变化的基础上,系统研究了微悬浮聚合工艺(均质化剪切速率、搅拌速率)和配方(有机颜料、分散剂含量)对颜料微胶囊粒径的影响。发现当搅拌速率为250 r·min^-1时,单体液滴的融合和乳胶粒的粘并现象均较少,聚合体系可较稳定地保持均质化单体液滴的尺寸。分散剂磷酸三钙TCP用量对体系稳定性影响明显,但其粒径调控能力有限。均质化强度对微胶囊粒径影响明显,具有较好的调控能力,而颜料含量对微胶囊粒径的影响较少。因而通过聚合工艺和配方的综合调节,可制得一系列颜料含量高、粒径分布窄、粒径可调范围较大的"石榴状"有机颜料微胶囊。     

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.