具有自修复功能的新型乙烯基硅油微胶囊的制备

以聚乙烯醇(PVA)作为分散剂,聚脲甲醛(PUF)为囊壁,乙烯基硅油为囊芯,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.实验研究了PVA浓度和搅拌速度对微胶囊的表面形貌及浓度和粒径分布的影响.分别采用傅里叶变换红外光谱、偏光显微镜对微胶囊的结构和形貌进行表征,采用激光粒度仪及同步热分析仪测定微胶囊的粒径大小及分布、热稳定性.结果表明:当PVA浓度为2％,搅拌速率为1 600r/min时,微胶囊粒径均匀,产率可高达90％;在240℃下,微胶囊的热稳定性良好.     

聚醚硅油微胶囊的制备与性能研究

以聚脲甲醛为囊壁,聚醚硅油为囊芯,采用原位聚合法制备了粒径均匀、致密性良好的新型聚脲甲醛(PUF)包覆聚醚硅油微胶囊。考察了不同种类乳化剂及不同搅拌速率对PUF包覆聚醚硅油微胶囊合成工艺的影响。采用傅立叶变换红外光谱及扫描电子显微镜等对聚醚硅油微胶囊试样进行表征。结果表明,实验成功地合成了PUF包覆聚醚硅油微胶囊,所制备的聚醚硅油微胶囊包覆率高达90%,载药率约为16.7%,囊芯结构良好,表面形貌光滑,平均粒径为250μm,在室温密闭环境下可保存72 h以上。     

原位聚合法制备分散染料微胶囊

以尿素和甲醛为壁材,分散染料酸性红GP(C.I.266)为囊芯制备了分散染料微胶囊。用SEM和Zeta激光粒度测定仪观察分析微胶囊的粒径分布,讨论了反应条件对微胶囊粒径分布的影响。通过实验,提出了制备该分散染料微胶囊的最佳反应条件为:壁材n(尿素)∶n(甲醛)=2∶3,分散剂阿拉伯树胶质量分数为5%,m(芯材)∶m(壁材)∶m(分散剂)=1∶7 25∶2 5,在pH=3,80℃和搅拌速率为1500r/min的体系中反应2h。     

溶剂蒸发法制备改性胺固化剂微胶囊的研究

以改性胺固化剂(1618)为囊芯、聚醚酰亚胺(PEI)为囊壁,采用溶剂蒸发法制备了EP(环氧树脂)固化用PEI包覆1618微胶囊。研究结果表明:固化剂芯材已被微胶囊PEI壁材成功包覆,其热稳定温度为130℃;以明胶作为分散剂时,制得的固化剂微胶囊表面光滑,分散性较好;随着芯壁比的增加,固化剂微胶囊的表面变得光滑、致密,并且其平均粒径减小(当芯壁比从1.0∶2.0增至1.5∶1.0时,平均粒径由45.8μm减至24.7μm)。     

氨基改性丙烯酸酯

西北工业大学的邢瑞英等人以乙烯基硅油为囊芯、聚脲甲醛为囊壁,采用原位聚合法制得了微胶囊。其用途是利用乙烯基硅油分子链上乙烯基的反应活性,添加光敏剂,使其在受到外力破坏时囊芯材料溢出并在紫外环境下固化,实现有机硅涂层的自修复。并优化了的微胶囊制备工艺。结果发现,当十二烷基苯磺酸质量分数为1％、搅拌速度为600r／min时,可得到平均粒径为123um的微胶囊。     

石蜡-密胺树脂微胶囊相变材料制备与表征

研究中采用了正十八烷石蜡相变材料(PCM)芯材,密胺树脂作为囊壁材料,用原位聚合法制备成微胶囊材料。通过改变芯材和囊壁材料的质量比,探讨了微胶囊制备过程中O/W乳化液的相稳定性,并采用SEM,FT-IR,粒度分析仪和DSC对微胶囊的形态及性能进行表征。结果表明芯材增大O/W乳化液的相稳定性下降,微胶囊数量平均粒径和体积平均粒径均减小,当芯材和囊壁材料的质量比(Core/Shell)为1.5∶1时,微胶囊表面光滑致密,平均粒径为3.6μm,相变焓为98.6 MJ/mg。     

低温固化EP用微胶囊固化剂的制备及性能表征

以PMF(聚三聚氰胺-甲醛树脂)为壁材、TMPMP[三羟甲基丙烷三(3-巯基丙酸酯)]为芯材,采用原位乳液聚合法制备了微胶囊固化剂。探讨了乳化剂类型及掺量、芯壳比[即m(囊芯)∶m(囊壁)]、反应温度、反应时间和p H等对合成微胶囊的粒径和稳定性等影响。研究结果表明:当m(EP)∶m(微胶囊固化剂)∶m[固化促进剂(DMP-30)]=100∶120∶1、芯壳比为2∶1、反应时间为60 min、反应温度为60℃、p H为3和搅拌速率为400 r/min时,微胶囊的粒径为50~125μm,并且具有很好的封闭性和耐热性,能在0℃以上达到较好的固化效果。     

厌氧胶固化引发剂微胶囊的制备

用原位聚合法制备了以厌氧胶固化引发剂过氧化羟基异丙苯为芯材、脲甲醛树脂为壁材的微胶囊。通过单因素比较法讨论了影响微胶囊制备的几个主要因素。实验表明,制备脲甲醛树脂微胶囊的最佳反应条件为:n(尿素)∶n(甲醛)=1.0∶2.0,壁材与芯材的质量比为10∶3,阿拉伯树胶的质量分数为2.5%,乳化剪切速度为2 000 r/m in,加酸速度为40 m in内把pH降到1.5。实验制备的微胶囊分散性好、粒径分布窄、平均粒径约为100μm。     

溶剂挥发法制备氟乐灵微胶囊工艺条件

为了提高氟乐灵的光稳定性和药效,以聚羟基烷酸酯为壁材,采用溶剂挥发法制备氟乐灵微胶囊,并讨论芯壁比、分散剂质量分数、剪切时间和速度、油水相体积比对氟乐灵微胶囊成囊的影响。结果表明:当芯壁比为1∶5,油水相比为(20∶100)~(30∶90),聚乙烯醇(PVA-1788)的质量分数为1%,剪切时间为3 min,剪切速度为8000 r/min,所得氟乐灵微胶囊呈球形,平均粒径在6.23~7.57μm,包封率为83.36%,载药量为14.62%。     

溶剂挥发法制备氟乐灵微胶囊工艺条件

为了提高氟乐灵的光稳定性和药效,以聚羟基烷酸酯为壁材,采用溶剂挥发法制备氟乐灵微胶囊,并讨论芯壁比、分散剂质量分数、剪切时间和速度、油水相体积比对氟乐灵微胶囊成囊的影响。结果表明:当芯壁比为1∶5,油水相比为20∶100~30∶90,聚乙烯醇(PVA-1788)的质量分数为1%,剪切时间为3 min,剪切速度为8000 r/min,所得氟乐灵微胶囊呈球形,平均粒径在6.23~7.57μm,包封率为83.36%,载药量为14.62%。     

溶剂挥发法制备聚砜包覆桐油自修复微胶囊

以聚砜为壁材,桐油为芯材,采用溶剂挥发法制备了聚砜（PSF）包覆桐油自修复微胶囊。考查了不同种类的分散剂、搅拌速度、芯壁比（芯材与壁材的质量比）等工艺参数对微胶囊性能的影响,通过扫描电子显微镜、光学显微镜和热重分析仪等对微胶囊的表观形貌、粒径、壁厚、包覆率和热稳定性能等进行表征。采用所合成的微胶囊制备了环氧树脂基防腐蚀涂层,并对其防腐蚀性能进行了评价。结果表明,30 ℃时,以明胶/聚乙烯醇复配体系作为分散剂,芯材与壁材质量比为1.3:1,搅拌速度为700 r/min时制备出的微胶囊表面光滑致密,粒径在130 μm左右,热稳定温度为350 ℃;盐雾实验结果表明,所制备的微胶囊自修复涂层具有良好的防腐蚀性能。     

醇酸树脂微胶囊的制备及环氧涂层自修复性能

采用三聚氰胺-脲醛树脂（MUF）为壁材、合成的花椒籽油醇酸树脂为芯材，原位聚合法制备自修复微胶囊，探讨了微胶囊的制备工艺。并采用扫描电子显微镜（SEM）、红外光谱仪（FTIR）、热重分析仪（TGA）和粒径分析仪对微胶囊的表面形貌、化学结构、热稳定性及其粒径分布进行了测试表征。将醇酸树脂微胶囊分散到环氧基体中，研究了环氧涂层的力学性能和自修复性能。实验结果表明，当乳化剂浓度为2.0g/L、芯壁比为2∶1、终点pH为3.5时，微胶囊呈球形结构，无明显的缺陷和损伤，平均粒径为97.44μm，热稳定性良好。当添加质量分数5%的微胶囊时，与未添加微胶囊的自修复涂层相比，其弯曲强度、拉伸强度、黏结强度及其冲击强度分别提高了50.4%、50.0%、40.0%及25.2%，且涂层的自修复性能良好。     

聚砜包覆环氧树脂微胶囊的制备

采用溶剂蒸发法制备了聚砜包覆双酚A型环氧树脂微胶囊,通过光学显微镜、激光粒度分布仪和微机差热天平对微胶囊的形貌、粒径分布及热性能进行了表征,讨论了分散剂种类及用量、搅拌速度、反应温度以及壁材与芯材投料质量比对微胶囊制备的影响。结果表明,反应温度过高时不能形成微胶囊;选择1.0 %（质量分数,下同）的聚乙烯醇分散剂、搅拌速度为750 r/min、反应温度为30 ℃、壁材与芯材投料质量比为2∶1时制得的微胶囊呈规则球形,产率较高,微胶囊分散较好,平均粒径在100 μm之内。     

Preparation and characterization of poly(urea-formaldehyde) microcapsules filled with epoxy resins

The preparation of microcapsules applied to the fabrication of self-healing composites has been paid more attentions. A new series of microcapsules were prepared by in situ polymerization technology with poly(urea-formaldehyde) (PUF) as a shell material and a mixture of epoxy resins (diglycidyl ether of bisphenol A: DGEBPA) and 1-butyl glycidyl ether (BGE) as core materials. The microencapsulating process of core material was monitored using optical microscopy (OM). The chemical structure of microcapsule was characterized using Fourier-transform infrared spectroscopy (FTIR). Morphology and shell wall thickness of microcapsule were observed using metalloscope (MS), scanning electron microscopy (SEM) and OM, respectively. The effects of different pre-polymers, weight ratios of urea to formaldehyde (U-F) and the agitation rates on the physical properties of microcapsules were investigated. The storage stability of microcapsules at different times and temperatures was analyzed. The thermal properties of microcapsules were investigated using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results indicate that PUF microcapsules containing epoxy resins can be synthesized successfully, and during the microencapsulation, the epoxide rings in epoxy resins are hardly affected by the surrounding media. The rough outer surface of microcapsule is composed of agglomerated PUF nanoparticles. The size and surface morphology of microcapsule can be controlled by selecting different processing parameters. The microcapsules basically exhibit good storage stability at room temperature, and they are chemically stable before the heating temperature is up to approximately 238 °C.     

2％阿维菌素微胶囊水悬浮剂的制备

以甲苯二异氰酸酯和水溶性成膜单体乙二胺为壁材,采用界面聚合法制备阿维菌素微胶囊水悬浮剂.研究了分散剂、溶剂、芯壁比、乳化搅拌速度、聚合反应时间对微胶囊包囊率和包囊形态的影响.结果表明:该法芯材比可达到6-7.5,体系浓度可达到10％,而且制得微胶囊阿维菌素包囊率＞90％,粒径≤10μm,粒径分布均匀,贮存稳定性合格,可...     

改性蜜胺树脂香精微胶囊的制备研究

为解决日化香精易挥发变质的问题,拓宽其应用领域,采用原位聚合法制备了一系列蜜胺树脂（MF）香精微胶囊。以低甲醚化蜜胺（L-MMF）树脂为例,傅立叶变换红外光谱（FT-IR）的结果证实了微胶囊对香精的良好包覆性,热失重〈TGDTG）分析说明微胶囊大幅提高了香精的耐热性能。进一步采用脲、间苯二酚、聚乙烯醇（PVA）、聚乙二醇（PEG）、氯化钠对蜜胺树脂进行改性并与未改性的树脂及不同甲醚化程度的蜜胺树脂进行对比,研究了改性对微胶囊包覆效果的影响。结果表明,低甲醚化蜜胺树脂和聚乙烯醇改性蜜胺树脂对香精的包覆效果较好,所得香精微胶囊粒径小,分布窄,包覆率高。     

聚砜包覆双环戊二烯微胶囊的制备

采用简单易控的溶剂挥发法成功制备了聚砜包覆双环戊二烯微胶囊,讨论了反应温度、分散剂、芯壁比及搅拌速度对微胶囊性能的影响,并通过扫描电子显微镜、光学显微镜和热重分析仪对微胶囊的表面结构、形貌和热性能进行了研究。结果表明,选择明胶溶液作为分散剂,反应温度为30 ℃时,可制备出粒径和壁厚可控的具有规则球形的微胶囊;随着芯材比例的增大,微胶囊壁厚减小;粒径随着搅拌速度的加快而减小。     

聚苯乙烯接枝包覆硫磺微胶囊的制备与表征

以合成硫磺为芯材,聚苯乙烯为壳材,采用原位接枝改性聚合方法制备了聚苯乙烯接枝包覆硫磺微胶囊,研究了不同苯乙烯/硫磺颗粒配比对微胶囊形貌的影响,制备了粒径均一分布的硫磺微胶囊,且分散均匀。结果表明苯乙烯的含量对微胶囊的表面形貌有很大影响,经包覆之后硫磺微胶囊的热稳定性提高。     

Preparation and properties of microcapsule with EVA core‐PU shell structure

Microcapsule with poly(ethylene‐co‐vinylacetate) (EVA) core‐polyurethane (PU) shell structure was synthesized by interfacial polymerization in aqueous polyol dispersion with ethylene diamine as the chain extender of toluene diisocyanate in poly(vinyl alcohol) aqueous solution as the stabilizing agent. The effects of polyol constituent on the average particle size and distributions, morphologies, color strength, and friction fastness of core‐shell particles were investigated to design microcapsule. The friction fastness of printed fabrics with EVA core‐PU shell microcapsules became the increase to 4–5 grades. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 893–902, 2007     

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.