改性β-环糊精为载体的七氟菊酯微胶囊的制备及性能测试

[目的]制备以改性的β-环糊精为载体的七氟菊酯微胶囊。[方法]以聚乙烯醇-1788为乳化分散剂,运用溶剂挥发法制备微胶囊,使用激光粒度分析仪、光学显微镜、扫描电镜对微胶囊进行形貌表征,用紫外分光光度计研究微胶囊的缓释行为。[结果]β-环糊精与PBS按4∶3的比例共混改性后制备的载体微胶囊的包封率为87.08%、载药量为57.81%,平均粒径为10μm,缓释期为25~27 d。[结论]改性后的β-环糊精载体微胶囊具有较好的结构形貌,载药量和包封率均比脲醛树脂载体微胶囊高,且缓释性更好。     

溶剂挥发法制备噻唑磷微胶囊

制备基于聚乳酸(PLA)改性聚丁二酸丁二醇酯(PBS)为载体的噻唑磷微胶囊。采用溶剂挥发法以聚乙烯醇-1788为乳化分散剂制备微胶囊,通过激光粒度分析仪、光学显微镜、扫描电镜对微胶囊进行形貌表征,用紫外分光光度计研究微胶囊的缓释行为。经聚乳酸(PLA)共混改性后的PBS载体微胶囊的包封率为85.27%、载药量为61.64%,平均粒径为5.46μm,缓释期为30 d。改性后的微胶囊具有较好的形貌,载药量和包封率比纯PBS载体微胶囊高,药物缓释更长。     

基于改性PBS载体的噻虫嗪微胶囊的制备及性能测试

[目的]制备基于改性聚丁二酸丁二醇酯(PBS)为载体的噻虫嗪微胶囊。[方法]采用乳化-溶剂挥发法以聚乙烯醇-1788为乳化分散剂制备微胶囊,通过激光粒度分析仪、光学显微镜、扫描电镜对微胶囊进行形貌表征,用紫外分光光度计研究微胶囊的缓释行为。[结果]经聚碳酸亚丙酯(PPC)共混改性后的PBS载体微胶囊的包封率为80.53%、载药量为54.47%,平均粒径为4.83μm,缓释期为25 d。[结论]改性后的PBS载体微胶囊具有较好的形貌,载药量和包封率比纯PBS载体微胶囊高,药物缓释期限更长。     

蓝色电泳微胶囊的制备条件对其形态的影响

以尿素和甲醛为壁材,油性蓝和TiO2纳米粒子分散在四氯乙烯中作为囊芯,通过原位聚合法制备了蓝色电泳显示微胶囊。研究了电泳微胶囊制备时的预聚和缩聚条件对微胶囊形成和产品形态的影响,并通过设计正交实验得到了最优化的预聚条件,优化条件:脲∶甲醛(摩尔比)为1∶1.75;反应温度75℃;pH值8.5;反应时间1 h,以最优化的预聚条件制备出的预聚体作为反应物进行缩聚反应制备出的蓝色电泳微胶囊内外表面光滑,囊壁透明,分散性好且形态完整。     

界面聚合法制备黄色电子墨水微胶囊

通过界面聚合法,用戊二醛改性的三乙烯四胺,与2,4-甲苯二异氰酸酯反应,制备出含黄色电子墨水的聚脲微胶囊。在搅拌速度为800~1 000 r/m in、乳化剂OP-10的浓度为0.05~0.12 mol/L的条件下,制备的微胶囊干燥后不易破裂,有一定机械强度、韧性、耐水性和耐热性;微胶囊壁厚约2μm;在直流电场中有显著的电泳现象,响应时间为0.2 s。     

乙二醇改性聚脲微胶囊相变材料的研制

以硬脂酸丁酯为芯材,吐温80、司班80为乳化分散剂,以单体2,4-甲苯二异氰酸酯和三乙烯四胺反应,并采用乙二醇进行改性形成的聚脲树脂为壳体,采用界面聚合法制备微胶囊相变材料。采用差示扫描量热仪（DSC）、扫描电镜（SEM）、氮气吸脱附测试仪等对微胶囊热性能、表面形态和比表面积进行了分析表征。结果表明,所制备的乙二醇改性微胶囊相变温度为20.5℃,相变潜热为87.75 J/g;平均比表面积0.009 9 m2/g,致密性较好。     

过氧化苯甲酰微胶囊的制备与应用

以尿素、三聚氰胺和甲醛的预缩合物为壁材,过氧化苯甲酰为囊芯,采用原位聚合的方法制备了过氧化苯甲酰微胶囊。讨论了在过氧化苯甲酰微胶囊形成过程中不同种类的润湿分散剂及其用量、酸的加入速度等对微胶囊状态及粒径分布的影响,通过大量对比实验,得出制备过氧化苯甲酰微胶囊的最佳反应条件、适宜的分散剂及用量。同时,通过相关的胶黏剂配方试验表明,将制备的微胶囊应用于螺纹锁固厌氧胶中,取得良了好的效果,能够很好满足客户的技术要求。     

彩色双粒子微胶囊电泳显示的研究进展

电子纸综合了传统纸张和新时代电子器件的优点,既如纸张一样阅读舒适、可弯曲折叠,又可以如液晶显示器一样不断转换刷新显示内容。微胶囊电泳显示使粒子的扩散和聚集禁锢在有限的空间范围内,改善了电泳液稳定性问题,延长了使用寿命,被认为是最具有发展前景的显示技术。本文在介绍各种电泳显示技术的基础上,着重介绍了微胶囊电泳显示技术。介绍了电泳白色无机粒子的表面改性,其次是电泳彩色有机粒子的表面改性,然后是电子墨水的制备方法以及微胶囊电泳显示的国内外商品化发展现状。     

层层自主装法制备GO杂化多壁微胶囊及其稳定性的影响探究

氧化石墨烯(GO)纳米粒子片层结构可用作Pickering乳液分散剂,芯材离子液体的稳定分散是制备微胶囊的关键,以GO作为Pickering乳液分散剂,并设计以GO为单一壁材制备了自润滑微胶囊,考虑到GO具有优异的耐摩擦性能和良好的热稳定性,再通过层层自主装法,使得壁层之间可以通过静电吸附和氢键作用连接,从而合成多层GO壁自润滑微胶囊。重点研究pH值、油水比、GO的质量浓度对GO的Pickering乳液的影响及GO杂化多壁微胶囊制备的最佳稳定条件。实验证明在pH值为2,油水质量比为5%,GO质量浓度为0.1 mg/L的实验条件下制备的微胶囊最佳。     

脲醛预聚条件对电泳微胶囊形态的影响

以尿素和甲醛为壁材,油性蓝和二氧化钛纳米粒子分散在四氯乙烯中作为囊芯,通过原位聚合法制备了电泳微胶囊. 研究了脲醛预聚体制备条件对微胶囊形成和产品形态的影响,并通过设计正交实验得到了最优化的制备条件,即脲:甲醛为1:1.75(摩尔比),反应温度75℃,pH值8.5,反应时间1 h. 在最优化条件下制备出的电泳微胶囊内外表面光滑,囊壁透明,分散性好且形态完整.     

电子墨水用白色电泳颗粒的制备及其表面改性

为制备出适用于电子墨水的白色电泳颗粒,采用控制正硅酸乙酯在氨水-乙醇溶液中的水解来合成S iO2颗粒。为提高S iO2颗粒于四氯乙烯溶液中的电泳性能,取1 g合成的S iO2颗粒,于30℃经w(H2O2)=30%的双氧水浸泡12 h后,与3 g丁二酸在100 mL乙腈介质中,于75℃进行回流加热反应24 h,将丁二酸化学键合于S iO2颗粒表面。最后,为降低电泳颗粒密度,将0.2 g经丁二酸改性的S iO2颗粒,于90℃时加入已溶解了0.1 g聚乙烯(PE)的50 mL二甲苯中,冷却静置12 h后,以10 000 r/m in的速度离心,使PE沉积包覆于电泳颗粒表面。傅里叶红外光谱(FTIR)图表明,丁二酸一端的羧酸基团与S iO2颗粒表面的羟基发生了酯化反应。透射电镜(TEM)证明,经丁二酸改性的S iO2颗粒被PE包覆,且包覆后的形貌为球状,粒径在300 nm左右。Zeta电位测试结果显示,经表面改性后,S iO2颗粒在四氯乙烯溶剂中的Zeta电位由-4.261 mV提高到了-27.84 mV,提高了5.53倍。     

中空黑色一氧化钛粒子的制备、改性及电泳性能

无机电泳颗粒由于密度相对较大,在分散介质中容易出现沉降,不能很好地分散于介质中。以单层核-壳聚合物粒子为模板,表面沉积钛酸四丁酯,通过湿化学法制备中空的黑色一氧化钛超微/纳米粒子。考察了二氧化硅、三氧化二铝和十二烷基苯磺酸钠（SDBS）对一氧化钛的包覆改性,并用红外光谱、X射线衍射、扫描电镜和透射电镜进行了表征,通过微电泳仪测定粒子的电泳淌度和Zeta电位。研究表明,中空结构能降低粒子的密度,改性后的粒子分散性和Zeta电位有明显的变化。使用三氧化二铝改性时,其电泳性能得到了很大的提高,Zeta电位绝对值高达40.70 mV,具有很好的电泳性能。      

An improvement of color electrophoretic paint via ultrafine modified pigment paste

The ultrafine paste used in electrophoretic paint was prepared via ultrasonic method with pigment yellow 83 (P.Y.83), octadecyl dimethyl benzyl ammonium chloride, and deionized water. The average particle size of the ultrafine paste was only 196?nm and zeta potential was 30?mV with ultrasound for 30?min and 2?wt.% cationic dispersant. The conductivity of the paint was improved as the cationic dispersant increased. Centrifugal stability of the paint with ultrafine paste reached the maximum at 2?wt.% cationic dispersant. Compared with the performances of cathodic electrophoretic paint with the ultrafine yellow paste, the anodic film was smooth, uniform, and neat with 0.5?wt.% cationic dispersant in the ultrafine yellow paste. Deposited amount of the anodic film was 27?g/m², which was higher than the cathodic film. The curing property, adhesion, and chemical resistance of the cathodic film were better than the anodic film. Properties of five color cathodic paints (blue, yellow, red, black, and green) were discussed and were compared with the film of electrophoretic paint containing commercial pastes. Except the green film, the blue, yellow, red, and black films were smooth, fine, and uniform, and also provided good L-effect. The deposited amount of these films with excellent adhesive force was about 14–19?g/m². The electrophoretic paints containing modified pigment pastes and commercial pigment pastes present good adhesion and chemical resistance.     

用于微杯显示的黑白电子墨水的制备研究

采用炭黑、TiO2作为黑白电泳颗粒,通过表面改性改善其电泳性能及在有机介质中的分散能力。用红外光谱(FT-IR)、扫描电镜与激光粒度仪对粒子进行了表征;采用静态沉降法探讨了粒子在四氯乙烯中的稳定性,并利用电泳特性仪对电泳粒子的电场响应特性进行了测试。结果表明,炭黑颗粒分散过程中加入相对含量为10%CH-6时,黑色粒子粒径为100 nm左右,沉降率降为4%,Zeta电位为30 mV,响应时间为300 ms;水解法制备金红石型TiO2粉末,经硅烷偶联剂改性后得到粒径为270 nm左右的球形颗粒,其Zeta电位为.25 mV,响应时间为340 ms;当TiO2与炭黑质量比为25:1时,显示对比度最高,此时刷屏时间为420 ms。     

The electric response behavior and microencapsulation of the pigment phthalocyanine green G using interfacial polymerization

The polyamide microcapsules for the electrophoretic display have been prepared via interfacial polymerization. The core material of the microcapsules is electrophoretic fluid consisted of pigment phthalocyanine green G (CAS No. 1328-53-6) modified with octadecylamine, tetrachloroethylene, and polyoxyethylene octylphenol ether (OP-10). The wall of the polyamide is synthesized from paraphthaloyl chloride and diethylenetriamine. FT-IR indicated that octadecylamine was bonded to pigment phthalocyanine green G with the hydrogen bond. The effect of the amount of octadecylamine on the dispersibility of the pigment suspended in tetrachloroethylene was investigated. Compared to the unmodified pigment, the dispersibility of the modified pigment was improved by 66.7%. The modified pigment migrated to the positive electrode under the direct voltage and the electric response time was about 85 s in 20 V/mm. The average particle size of microcapsules decreased from 834.5 to 258.2 nm as the dosage of OP-10 increased, and the microcapsule yield reached maximum of 83.5% at the OP-10 concentration of 1.5 wt%. With the reduction of the core/wall weight ratio in the range from 1:6 to 1:14, the average particle size improved from 267.4 to 554.4 nm. However, the maximum of the microcapsule yield was 87.6% at the core/wall weight ratio of 1:10. The microcapsule yield reached a peak of 87.6% as the pH value was 12. The average particle size of the microcapsules that obtained at 25 °C was 327.4 nm, which was smaller than those prepared in other temperatures. The formed polyamide microcapsules had a regular spherical shape.     

丙烯酸类中空聚合物粒子的制备与电泳性能

以甲基丙烯酸甲酯、丙烯酸丁酯、α-甲基丙烯酸和苯乙烯为单体,以过硫酸钠为引发剂,温度控制在78℃,搅拌速度为800 r/min,采用半连续加料法,经乳液聚合分别制得了种子、核及具有核壳结构的聚合物粒子。用动态光散射(DLS)、原子力显微镜(AFM)、扫描电镜(SEM)测得其平均粒径分别为72.1、400及500 nm。核壳粒子用w(NaOH)=10%的水溶液进行溶胀,得到的粒子经透射电子显微镜(TEM)显示为中空结构,在SEM下观察,其平均粒径在900 nm左右。用微电泳仪测得,该中空粒子在四氯乙烯分散介质中电泳淌度为0.004 98 s2.mA.kg,Zeta电位为0.032 2 mV,在水分散相中,Zeta电位为-43.880 mV。     

Encapsulation of TiO2 in poly(4-vinyl pyridine)-based cationic microparticles for electrophoretic inks

Poly(4-vinyl pyridine) microparticles were prepared via surfactant-free emulsion polymerization in water with divinylbenzene as crosslinking agent. The synthesis was adapted for the encapsulation of TiO₂. The size, integrity and nature of the resulting hybrid microparticles were investigated by Scanning electron microscopy, Dynamic light scattering and Fourrier-transform infrared Spectroscopy measurements. The particles were quaternized using a modified copolymer, which was grafted via an alkylation reaction on particle surface followed in a second step by alkylation with methyl iodide. After quaternization, an electrophoretic ink was formulated using the TiO₂/poly(4-vinyl pyridine) cationic microparticles. Under electric field, the electrophoretic ink showed good optical properties, lifetime and stability.     

双壳结构绿色电泳粒子的制备及其应用

采用反相微乳液-表面溶剂聚合法制备了双壳结构的绿色电泳粒子(PIB/CT/S).采用SEM、TEM、XPS、FTIR和XRD对其进行了表征,以四氯乙烯为分散介质,PIB/CT/S为电泳粒子进行了电泳性能测试.结果表明,PIB/CT/S具有良好的球形结构,平均粒径为241.2 nm,是以二氧化硅球(S)为基体,以绿色钛酸钴(CT)为第一层包覆物,以离子液体聚合物〔聚(1-乙烯基-3-十二烷基)咪唑溴(PIB)〕为第二层包覆物,其密度为1.7905 g/cm3.可见光漫反射测试和电子墨水涂布平台测试表明,PIB/CT/S具有较好的光学性质.制备的简易电泳显示器(EPD)的响应时间为165 ms,明显优于商用EPD(响应时间为260～300 ms).     

超细酞菁蓝微粒的制备及其电泳性能的研究

实验采用反溶剂重结晶方法制备超细酞菁蓝(CuPc)颗粒,在重结晶过程中加入了不同类型的表面活性剂对酞菁蓝原料进行改性.用红外光谱(FT-IR)表征了重结晶粒子的表面组成,并通过扫描电镜(SEM)与激光粒度仪观察了粒子的形貌、分散情况及粒径分布.采用静态沉降法探讨了粒子在四氯乙烯中的稳定性,并利用电泳测试仪对粒子的电场响应特性进行测试.结果表明,重结晶过程中加入阴离子表面活剂十二烷基硫酸钠(SDS),所制得的粒子其分散稳定性和带电性最好.考察了SDS用量、反溶剂类型、反应温度对粒子稳定性和带电性的影响.得到的酞菁蓝最可几粒径为350 nm,沉降率22.3%,电场响应时间为6.1 s.     

电泳显示器用聚合物包覆颗粒的制备及其分散稳定性的紫外透光率表征

采用自由基接枝聚合法,将不同极性的单体修饰在黑色无机颜料颗粒表面,以紫外透光率法为主要表征手段,考察了聚合物包覆层的组成结构对颗粒在电泳体系中分散稳定性的影响. 结果表明,聚合物修饰后颗粒稳定时间至少提高5倍,且随所用包覆单体侧链长度增大而增大. 当单体支链的碳原子数大于4时,颗粒能很好地长时间分散在非水体系中. 所制黑白电泳显示器在5 V电压下,响应时间小于1 s,对比度达(4~5):1. 本结果为提高缺乏理论研究的电泳显示体系的分散稳定性和电泳显示效果及使用寿命提供了研究基础.