聚[2-(甲基丙烯酰氧)乙基三甲基氯化铵]/阿拉伯胶复凝聚法十二醇微胶囊的制备

将聚[2-(甲基丙烯酰氧)乙基三甲基氯化铵](PMTC)和阿拉伯胶(GA)在一定条件下进行了复凝聚,并对影响复凝聚实验的壁材配比、壁材浓度、离子强度等因素进行了考察.实验结果表明,PMTC与GA配比为1/3.22,壁材总浓度为4%时复凝聚效率最高;体系中不同浓度的氯化钠的存在会对复凝聚起到不同程度的抑制作用.在实验确定的最佳复凝聚条件下以有机小分子化合物十二醇作为芯材进行了包覆,制备了不同壁芯比例的微胶囊.对微胶囊的包覆率及载药量进行了测量,并对它们的释放行为进行了考察.包覆有十二醇的复合微胶囊大小一般在几微米.随着壁材与芯材比例的增大,胶囊载药量逐渐降低,微胶囊释放十二醇的速率明显变小,但包覆率却无明显变化规律.     

大豆分离蛋白-十二烷基硫酸钠微胶囊的制备与表征

以大豆分离蛋白(SPI)和十二烷基硫酸钠(SDS)为壁材, 以十六烷为芯材, 通过复凝聚法制备了微胶囊. 首先确定了SPI和SDS发生复凝聚的适宜pH、SPI/SDS配比、壁材浓度等. 在确定的实验条件下进行复凝聚, 凝聚物产率可达85%. 改变搅拌转速和芯壁比, 考察它们对微胶囊性能的影响. 用光学显微镜观察了微胶囊形貌. 用气相色谱测定了微胶囊的载药量和包覆率. 芯壁比为2、搅拌转速为400 r/min时所制备微胶囊的载药量可达61%. 随着芯壁比的增大, 微胶囊粒径及载药量都逐渐增大.     

复凝聚法制备昆虫激素模拟物十二醇微胶囊及其释放性能

以明胶(GE)和阿拉伯胶(AG)为壁材, 通过复凝聚法将昆虫激素模拟物十二醇(C12OH)包覆在微胶囊中, 改变微胶囊壁材的浓度和交联度, 探讨了体系中C12OH的可控释放性能. 通过对壁材质量比为1及不同pH条件下的壁材凝聚率测试确定最佳复凝聚的pH为4.0; 考察了不同分散剂对微胶囊及其分散液性能的影响, 确定以Tween 20/Span 80(质量比1∶1)作为复凝聚法包覆C12OH体系的分散剂. 在壁材质量分数大于或等于3%条件下制备的微胶囊粒径大于壁材质量分数为2%的微胶囊, 胶囊的载药量和C12OH包覆率明显高于后者. 增加交联剂的用量, 壁材交联度、胶囊的载药量和C12OH包覆率都显著提高. 在相同用量的情况下, 用甲醛作交联剂时得到的微胶囊的交联度比用戊二醛作交联剂时的要低, 但其对C12OH的包覆率更高. 通过扫描电镜对微胶囊进行了分析, 认为GE与AG通过复凝聚能够将C12OH包覆在微胶囊内部. 对胶囊中C12OH在恒温恒湿条件下的释放研究结果表明, 3%与4%壁材含量下1%戊二醛交联的微胶囊和5%壁材含量下4%戊二醛交联的微胶囊中C12OH的释放行为有明显的可控性. 通过调节微胶囊的壁材含量和交联度可以达到昆虫激素可控释放的目的.     

单凝聚与复凝聚法制备昆虫激素十二醇微胶囊及其释放行为

通过向明胶溶液中加入硫酸钠溶液的单凝聚方法以及将明胶溶液加入到阿拉伯胶溶液的复凝聚方法,制备了聚合物包覆昆虫激素十二醇的水分散体系微胶囊.通过对凝聚过程中ζ电位与透光率跟踪测试确定了单凝聚中加入硫酸钠的最佳用量以及复凝聚中明胶与阿拉伯胶的相对量.在壁材浓度大于或等于3%条件下制备的复凝聚胶囊的尺寸大于单凝聚微胶囊,但后者的大小分布更均一.除非在2%壁材浓度下,其他条件下复凝聚制备的胶囊的十二醇包覆率明显高于单凝聚胶囊.对胶囊中十二醇在恒湿恒温条件下的释放研究表明,单凝聚胶囊中十二醇很快释放完毕,变化壁材浓度不明显改变其释放行为.相比之下复凝聚胶囊中十二醇的释放对壁材浓度有明显的依赖性.2%壁材浓度制备的胶囊其释放行为类似于单凝聚胶囊;但3%到5%壁材浓度制备的胶囊中十二醇的释放明显分为3个区间,即较快的初始释放、较长时间的恒速释放以及最后阶段释放速率的再次提高直至释放完毕.复凝聚胶囊中十二醇的释放表现出了明显的可控性.文中亦对该体系中昆虫激素十二醇的释放机理作了初步讨论.     

复凝聚法辣椒油树脂微胶囊的制备

以辣椒油树脂为芯材,明胶和阿拉伯胶为壁材,采用复凝聚法制得辣椒油树脂微胶囊.考察了45℃、体系浓度为5%时,pH值、乳化剂的用量、搅拌速度等几个因素对微胶囊形成的影响.     

一种致密的相变储能微胶囊的制备与表征

制备了以聚脲为第一壁材、苯乙烯-二乙烯苯为第二壁材,以相变点在16℃左右的石蜡为芯材的相变储能微胶囊。采用红外光谱、差示扫描量热分析、热重分析测试技术表征了制备的相变储能微胶囊的结构组成以及热性能;采用溶剂淋洗法研究了影响包覆率的因素。结果表明,相变储热微胶囊是复合相变材料,微胶囊的热稳定性好,致密性优良;通过对水油比、乳化剂及苯乙烯-二乙烯苯用量等各因素对微胶囊包覆率影响的讨论,得出在水与油质量比3.2,乳化剂相对于水的质量分数为2%时,加入苯乙烯与二乙烯苯质量比为10∶1混合液的质量分数为6.0%时,其包覆率达81.14%;制备的微胶囊能耐较高温度,在150℃以下无质量损失,且微胶囊储热能力高达80J/g。同时发现,储热能力与芯壁比有关,比值越大储热潜能越高。     

不同相对分子质量羟乙基纤维素对甲维盐微胶囊制备的影响

采用原位聚合法以三聚氰胺-甲醛树脂为壁材制备了甲维盐微胶囊。 探讨了不同黏均相对分子质量羟乙基纤维素作为乳化剂对微胶囊表面形貌、粒径及其分布、包覆率与载药量的影响,对使用不同黏均相对分子质量羟乙基纤维素作为乳化剂制备的微胶囊的释放性能进行了表征。 结果表明,以相对分子质量较小的羟乙基纤维素制备的微胶囊外形规则、致密且无黏连现象。 随羟乙基纤维素黏均相对分子质量的增加所得微胶囊的平均粒径及粒径分布逐渐增大,包覆率与载药量逐渐减小。 释放性能的研究表明,采用相对分子质量较小的羟乙基纤维素制备的微胶囊的释放性能较好。     

昆虫激素模拟化合物十二醇微胶囊的制备与释放行为研究

利用昆虫雌性激素对昆虫进行干扰交配是近年来使用的一种新技术,可替代农药杀虫剂达到高选择性无毒无药灭害的目的.鉴于十二醇(C12H25OH)与简单的昆虫激素化合物十二碳烯醇、十二碳烯二醇等结构相近,使用C12H25OH作为昆虫激素的模拟物,探索使用聚合物微球水分散体系将昆虫激素模拟物C12H25OH包覆在聚合物微球中,通过改变水分散体系的制备方法、复合微球壁的交联度等探讨了此类体系对C12H25OH的可控释放.首先通过测定阿拉伯胶明胶复凝聚过程的透光率、ζ电位,确定了阿拉伯胶-明胶的质量配比为1时可达最大复凝聚.在此基础上,制备了一系列交联剂戊二醛含量不同的复合微胶囊.结果表明微胶囊壁材的交联度随交联剂量明显上升,其对C12H25OH的包覆率经1%戊二醛交联后即提高至未交联体系的约三倍.但进一步提高戊二醛的含量,虽然胶囊的交联度仍明显上升,但对C12H25OH的包覆率基本保持恒定.使用同样量的甲醛可达同样交联效果,但对C12H25OH的包覆率有明显提高.在恒温恒湿条件下对各胶囊的C12H25OH释放行为进行了表征,结果显示交联胶囊可明显提高C12H25OH的恒速释放时间,交联度越高,恒速释放越稳定.本工作表明通过本方法确实可以达到将昆虫激素包覆在聚合物颗粒中并达到可控释放.     

甲胺基阿维菌素苯甲酸盐微胶囊的制备与表征

以三聚氰胺-甲醛树脂为壁材,采用原位聚合法制备了甲胺基阿维菌素苯甲酸盐微胶囊,研究了三聚氰胺与甲醛的质量比、芯壁比、乳化剂、搅拌速度与时间、pH值、温度等因素对微胶囊形成的影响,对制备的微胶囊进行了表征,测定了甲维盐微胶囊化前后的光解率。结果表明,三聚氰胺与甲醛质量比为1∶2、芯材与壁材质量比为3∶2、以质量分数1%羟乙基纤维素(HEC)为乳化剂、在1000r/min搅拌速度下、pH=5.0和50℃保温2h可制备出形貌较好、平均粒径4.4μm的甲维盐微胶囊。红外光谱分析证明,甲维盐已完全被包覆在微胶囊中。紫外分光光度法测定其缓释性能良好。光解实验表明,微胶囊化可有效降低甲维盐原药的光解。     

光致变色微胶囊的制备与性能

以蜜胺树脂为壁材、光致变色材料为芯材,采用原位聚合法制备了具有光致变色性能的微胶囊.研究了三聚氰胺/甲醛摩尔比、壁材与芯材的用量比、乳化剂浓度等因素对微胶囊形貌及性能的影响.在最佳工艺条件下制备的变色微胶囊,在日光和紫外光下具有快速、可逆的光致变色性能.     

Microencapsulation of dodecyl acetate by complex coacervation of whey protein with acacia gum and its release behavior

Complex coacervation of whey protein(WP) with acacia gum(AG) was carried out in water with the presence of dodecyl acetate (DA),a component of insect sex pheromones,in order to obtain microcapsules with DA as the core material and WP-AG coacervate as the wall materials.Through variations in wall/core ratios,concentrations of the wall materials in capsule preparations,DA encapsulation was optimized,which showed a high DA encapsulation was achieved when coacervation was conducted at pH 3.5 with wall/core mass ratio at 3 combined with concentration of wall materials at 1.0 wt%.Morphology and the structure of DA loaded microcapsules were examined by scanning electron microscope,which showed the microcapsules were of core/shell structure with DA encapsulated in the inner of the microcapsules.DA release was examined and the behavior of the release was discussed.     

昆虫激素十二醇微胶囊的制备与释放行为研究

利用昆虫雌性激素对昆虫进行干扰交配是近年来使用的一种新技术,可替代农药杀虫剂达到高选择性无毒无药灭害的目的。迄今为止的相关研究及应用技术都是使用载有昆虫激素的棉条、纸片、塑胶管等装置,以一定密度置于果园或农田。十二醇是较为简单的一个存在于多种昆虫的雌性激素中化合物。本文首次探索使用聚合物微球水分散体系将昆虫激素十二醇(C12OH)包覆在聚合物微球中,通过改变水分散体系的制备方法、复合微球壁的交联度等探讨了此类体系对C12OH的可控释放。本工作首先通过测定阿拉伯胶明胶复凝聚过程的透光率、ζ电位,确定了阿拉伯胶-明胶的重量配比为1时可达最大复凝聚。在此基础上,制备了一系列不同交联剂戊二醛含量的复合微胶囊。结果表明微胶囊壁材的交联度随交联剂量明显上升,其对C12OH的包覆率经1%戊二醛交联后即提高至未交联体系的约三倍。但进一步提高戊二醛的含量,虽然胶囊的交联度仍明显上升,但对C12OH的包覆率基本保持恒定。使用同样量的甲醛可达同样交联效果,但对C12OH的包覆率有明显提高。在恒温恒湿条件下对各胶囊的C12OH释放行为进行了表征,结果显示交联胶囊可明显提高C12OH的恒速释放时间,交联度越高,恒速释放越稳定。本工作表明通过本方法确实可以达到将昆虫激素包覆在聚合物颗粒中并达到可控释放。     

Study of Complex Coacervation of Gelatin A and Sodium Alginate for Microencapsulation of Olive Oil

Complex coacervation of gelatin A and sodium alginate was carried out to obtain the maximum coacervate yield. Turbidity and coacervate yield (%) measurements were carried out to support the ratio of the two polymers and pH that produced maximum coacervation. The optimum ratio between gelatin A-sodium alginate and pH to form the maximum coacervate complex was found to be 3.5:1 and 3.5–3.8, respectively. Olive oil microencapsulation was carried out at the optimized ratio and pH. Microcapsules were crosslinked by using glutaraldehyde. Scanning electron microscopy studies confirmed the formation of free flowing spherical microcapsules of different sizes. The size of microcapsules increased with the increase in the concentration of the polymer. The encapsulation efficiency and the release rates of olive oil were dependent on the amount of crosslinker, oil loading and polymer concentration. Thermogravimetric study revealed improvement of thermal stability with crosslinking. Fourier Transform Infrared Spectroscopy study showed that there was no significant interaction between olive oil and gelatin-alginate complex.     

高取代度魔芋葡甘聚糖醋酸酯的制备及其热塑性和流变性研究

以魔芋葡甘聚糖(KGM)为原料,浓硫酸为催化剂,乙酸酐为改性剂,制备了KGM醋酸酯.研究了反应条件对KGM醋酸酯取代度(DS)的影响,KGM醋酸酯制备的最佳反应条件是乙醇∶水量比5∶5,反应时间2h,反应温度75℃,催化剂浓硫酸的浓度0.1mol/L,KGM与乙酸酐的量比5∶40(g/mL),取代度高达2.93,其分子量与KGM相比,则明显降低.运用傅立叶红外光谱仪(FTIR)、X射线衍射仪(XRD)、扫描电镜(SEM)、热重分析仪(TGA)、示差扫描量热仪(DSC)和旋转流变仪对KGM和高取代度KGM醋酸酯进行了表征.结果表明,KGM醋酸酯的羰基(CO)特征吸收峰较KGM明显增强,其表观形貌大部分为疏松絮状,KGM及其醋酸酯均为非晶态结构.与KGM相比,KGM醋酸酯的热稳定性下降,分解温度(Td)由KGM的261.10℃降低至KGM醋酸酯的204.56℃,KGM醋酸酯出现了明显的玻璃化转变,其玻璃化转变温度(Tg)为128.49℃.KGM醋酸酯是典型的黏弹性材料,其弹性比率占21.27%,其剪切黏度η对温度变化非常敏感,可通过温度的改变来调节KGM醋酸酯的加工流动性.KGM醋酸酯具有较好的热塑性.     

Soy glycinin microcapsules by simple coacervation method

Encapsulation of a dispersed oil phase (hexadecane) was realized by simple coacervation method using soy glycinin as the wall forming material. Suitable emulsification and coacervation conditions, that favor the formation of microcapsules wall, were identified and investigated. Mild acid (pH 2.0) and heat (55 degrees C) treatments of the reaction medium during the emulsification step enhanced significantly the deposition of coacervated glycinin around oil droplets. A pronounced correlation between glycinin concentration in the continuous phase, specific surface of the dispersed phase and the microencapsulation efficiency was also observed. Coacervation step study concerned the morphology and the stability of microcapsules. Controlled initiation of the coacervation, by slow readjustment of the pH, allowed a homogeneous precipitation of glycinin around oil droplets as well as the absence of aggregation phenomena. Since the morphology of microcapsules was considerably affected by a prolonged stirring of the reaction medium, the coacervation and reticulation time were optimized in order to preserve the homogeneity of the microcapsules size distribution and the microencapsulation efficiency.     

Preparation and utilization of perillyl acetate

Perillyl acetate is a fragrance compound that was prepared by the reaction of β-pinenoxide with acetic anhydride and using acetic acid as an acid catalyst. Several selected catalysts were tested (homogenous: phosphoric acid, boric acid, acetic acid, and citric acid; heterogeneous: zeolite USY, SSA, and montmorillonite K-10) and the reaction conditions optimized for this reaction. The yield 78.7 % of perillyl acetate was obtained. Mayol (4-isopropylcyclohexylmethanol), a valuable fragrance compound, was further obtained by a two-step synthesis from perillyl acetate. Firstly, perillyl acetate was saponified to perillyl alcohol. The yield of alcohol was 94.4 %. The last step of the entire preparation was the hydrogenation of perillyl alcohol to Mayol. The yield of the desired product of this reaction was 94.6 %.