亲水颗粒和短链双亲分子协同稳定的Pickering乳液
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摘要
乳液是一种液体以液滴的形式分散在另一种与之互不相溶的液体中形成的胶体分散体系,人们对于传统乳化剂(表面活性剂和具有表面活性的聚合物)稳定的乳液体系从理论和实际应用上的研究都已经较为成熟。在20世纪初,Pickering和Ramsden关于固体颗粒可以作为乳液稳定剂的发现,为制备性能优异的乳液提供了一种新方法。迄今为止,Pickering乳液已成功应用于食品、化妆品、医药和原油开采等领域,同时随着纳米科技的兴起,也被成功应用于多孔结构、微胶囊、中空结构及其它具有特殊功能的材料制备,进一步扩展了Pickering乳液的应用范围。在Pickering乳液的许多应用中,因为很多乳液产品需要长时间的保持其自身特性,所以乳液必须要稳定。影响乳液稳定性的因素有很多,其中颗粒的润湿性是Pickering乳液稳定性的关键因素。一般来说,纳米颗粒本身不具备适宜的亲水疏水性,很难吸附在油水界面上从而得到稳定的乳液。
在很多的研究工作中,表面活性剂经常被用于调控颗粒的润湿性,使颗粒更容易在油水界面上吸附从而获得稳定的Pickering乳液。然而,表面活性剂与颗粒在共同稳定乳液的过程中还会存在竞争作用,它们在油／水界面的竞争吸附往往会影响乳液的稳定性,表面活性剂甚至能够直接导致颗粒从油／水界面脱附,为Pickering乳液的应用带来诸多不利影响。与表面活性剂相比,短链双亲分子在油水界面上的吸附能力较弱且无法单独稳定乳液,因此,它们作为颗粒改性剂的使用可以有效的避免这一问题的出现。不仅如此,短链双亲分子在水溶液中具有高的溶解度和临界聚集浓度,在固体颗粒含量较高的分散体系中对颗粒进行润湿性调节时更具优势。迄今为止,人们对短链双亲分子与颗粒的协同作用已有了初步的认识,但是对该复合体系在稳定乳液过程中表现出来的规律仍然缺乏系统的研究。
本文选择了两种带相反电荷且具有不同形貌的亲水性颗粒作为模型颗粒一带有负电荷的圆盘状锂皂石(Laponite)和带有正电荷的层状双金属氢氧化物(Layered double hydroxide compounds,简称LDH)。首先,系统研究了Laponite颗粒和短链脂肪胺共同稳定的乳液体系。继而,我们在LDH颗粒稳定的乳液体系中引入了一种具有荧光性质的短链双亲分子甲基橙,得到了稳定的乳液并以此为模板制备了中空胶囊。最后,我们在短链羧酸钠(丁酸钠和苯甲酸钠)原位改性的LDH颗粒稳定的乳液中发现了非球形乳液滴并对此进行了研究。
本文的主要内容包括以下三部分：
1.短链脂肪胺改性的Laponite颗粒稳定的乳液
考察了由盘状Laponite颗粒与短链脂肪胺(二乙胺DEA和三乙胺TEA)混合水分散体系制备的Pickering乳液的稳定性。首先,我们考察了当锂皂石颗粒浓度较低(0.5wt%)时短链胺的加入对分散体系和最终所得乳液性质的影响。红外光谱和zeta电位的表征证明了短链胺分子在锂皂石颗粒表面的吸附。由于DEA和TEA分子结构中都存在极性氨基,在一定pH的水溶液中会发生部分水解而带正电,因此可与带有相反电荷的锂皂石颗粒产生静电相互作用而吸附在颗粒表面。随着胺浓度的增加,胺分子在锂皂石颗粒表面的吸附量逐渐增加并最终达到平台,此时胺分子在颗粒表面的吸附达到饱和。胺分子的吸附使锂皂石颗粒表面变得部分疏水,表现为其三相接触角随着胺浓度的增加而增大并最终到达平台值。对应的乳液也随着胺浓度的增大逐渐变得稳定,到达平台之后不再发生变化。荧光显微镜和扫描电子显微镜观察共同证实了短链胺改性的锂皂石颗粒在乳液滴表面的吸附。
当Laponite浓度较高(4.0wt%)时,我们通过流变实验证实了胺分子的加入使锂皂石颗粒水分散体系的粘度降低,有利于乳液的形成。并且,高浓度分散体系和乳液稳定性随着胺浓度的增加的变化规律与低浓度时基本一致,但是所制备的乳液稳定性极佳,放置长达六个月的时间也不会出现分水分油的现象。
2. LDH颗粒与甲基橙共同稳定的乳液
颗粒在乳液滴表面的自组装使Pickering乳液可以作为模板来制备中空胶囊等材料,而具有特殊性质的功能性颗粒稳定的乳液通常可以得到功能性材料。利用功能分子来调节颗粒润湿性将为一些特殊功能材料的制备提供一种简便的方法。以往将颗粒改性的方法仅仅局限于对颗粒润湿性的调节,功能性分子很少被用于调节颗粒润湿性从而稳定乳液以得到相应的功能性材料。
我们引入了一种常见的荧光染料甲基橙作为双亲分子对LDH颗粒进行修饰并制备了稳定的Pickering乳液。这里甲基橙的特点在于可以同时将LDH颗粒进行疏水改性并赋予其荧光性质。为了考察甲基橙在LDH颗粒稳定的乳液中所发挥的作用,我们首先讨论了甲基橙作为双亲分子对LDH分散体系及其稳定的乳液的影响,通过吸附等温线和zeta电位测试证明了甲基橙分子在LDH表面的吸附,颗粒三相接触角的增大证实了甲基橙分子的吸附的确使LDH颗粒的疏水性增强,从而提高了所得乳液的稳定性,表现为乳液体积分数的增大和乳液滴平均粒径的减小。然后我们利用甲基橙分子的荧光性质在激光共聚焦显微镜下原位观察到了甲基橙改性的LDH颗粒在乳液滴表面的吸附。值得注意的是,甲基橙不仅可以吸附在LDH的外表面上,还可以通过阴离子交换进入其层间,为改性的LDH颗粒带来特殊的荧光性质。最后,我们以所得的Pickering乳液为模板制备了由甲基橙插层的LDH颗粒构成的中空胶囊,并且通过SEM观察了中空胶囊的形貌及壳层表面的片状颗粒的排布。甲基橙所发挥的荧光双亲分子的作用为荧光材料的制备提供了一种简便的方法。
3.LDH颗粒与短链羧酸钠共同稳定的非球形Pickering乳液
我们在短链羧酸钠(丁酸钠和苯甲酸钠)原位改性的LDH颗粒稳定的乳液中意外的发现了大量的非球形乳液滴。我们对此现象进行了研究,考察了乳化转速、短链羧酸钠浓度和类型对乳液滴的非球形化程度的影响。乳液滴的非球形化程度与乳液析油体积分数的变化趋势一致,较高的非球形化程度往往对应着较大的乳液析油体积分数,由此可以推断出非球形乳液滴的形成主要是乳化过程中液滴之间的有限聚结所导致的。
短链羧酸钠的类型和浓度对乳液滴的非球形化程度也有着显著的影响。当乳化转速固定时,不论是丁酸钠还是苯甲酸钠对应的乳液体系,乳液滴的非球形化程度均随着短链羧酸钠浓度的增大而减小,超过一定浓度后达到平台值。界面流变实验结果表明,短链羧酸钠浓度和类型的变化对乳液滴非球形化程度的影响与乳液滴表面的颗粒膜强度有关。我们通过对LDH/短链羧酸钠混合水分散体系中颗粒接触角和zeta电位的表征证明了颗粒疏水性的增加和静电斥力的减小,这两种因素使体系界面膜的粘弹性增加,进而导致乳液滴变形程度减小。此外,我们将乳液滴的内相固化后通过SEM对其形貌进行了观察,发现片状颗粒在非球形乳液滴表面明显呈“拥挤”状态,再次确认了非球形乳液滴的形成是乳液滴之间的有限聚结所导致的。
An emulsion is a thermodynamically unstable system which consists of dispersed droplets of one immiscible liquid in another. The system shows a tendency to break to reduce the interfacial area. Therefore a stabilizer is needed, including surfactants, surface-active polymers and solid particles. Emulsions stabilized by colloid particles, commonly named Pickering emulsions, have been studied extensively for their widespread use in practical applications, such as food, pharmaceutics, cosmetics, oil recovery and wastewater treatment since the beginning of20th century. In many of these applications, the stability of emulsions is necessary to keep their properties over long periods of time. Up to now, various theories about emulsions stabilized by solid particles have been developed and recently a thorough understanding of them has been achieved. According to these theories, particle wettability is a crucial parameter which determines the type and stability of the emulsions. Stable emulsions are prepared with particles of intermediate wettability.
To meet the need of appropriate wettability for stability of emulsions, the particles are usually modified via addition of surfactants. There is strong synergy in most combinations of particles and surfactants in stabilizing emulsions. Cationic, anionic, and nonionic surfactants have all been applied successfully to tailor the wettability of particles in liquids and thus prepare stable emulsions. However, there is always competitive adsorption at the oil/water interfaces between the modified particles and the free surfactant molecules in the bulk solution. The free surfactant molecules can even dominate and determine the properties of emulsions. This will bring about many disadvantages in the practical applications of Pickering emulsions. The introduction of short-chain amphiphiles can resolve this problem effectively, due to the incapability of displacing particles at the oil/water interfaces. In addition, the short amphiphiles exhibit high solubility and critical micelle concentrations in water, enabling the surface modification of high concentrations of particles.
Based on the study on emulsion field above, two kinds of hydrophilic particles with different shapes and opposite charges, layered double hydroxides (LDH) and Laponite, are investigated. First, liquid paraffin-in-water emulsions stabilized by Laponite particles modified with short-chain aliphatic amines (diethylamine, DEA or triethylamine, TEA) were prepared. Then, methyl orange molecules have been used as fluorescent amphiphiles in preparation of emulsions stabilized by LDH particles. The self-assembly of fluorescent particles at droplet surfaces is accomplished, which has been exploited to produce hollow colloidosomes. Nonspherical droplets in emulsions stabilized by LDH particles in situ modified with sodium alkyl carboxylates (sodium butyrate, C4Na or sodium benzoate, C7Na) can be obtained directly through emulsification. The presence of nonspherical droplets is mainly attributed to the partial coalescence of neighboring droplets.
The present dissertation includes three topics.
1. Pickering emulsions stabilized by Laponite particles modified with short-chain aliphatic amines
Liquid paraffin-in-water emulsions were successfully prepared by mixing oil with Laponite suspensions after in situ modification of the particles with short-chain aliphatic amines, DEA and TEA. The adsorption of DEA or TEA brings about enhancement of particle hydrophobicity and decrease of zeta potential, which make it easier for them to adsorb at oil-water interfaces. It was found that, at low clay concentration (0.5wt%), stable emulsions can be obtained when the clay-amine suspensions are flocculated. The emulsion stability improves with amine addition and reaches a plateau above a certain amine concentration. The variation of mean droplet size of emulsions is consistent with the emulsion stability. Emulsions of best stability are formed from the most unstable particle suspensions. The adsorption of the modified clay particles on the droplet surface results in emulsion stabilization, which was confirmed by laser-induced fluorescent confocal micrographs and SEM observations.
Furthermore, extremely stable emulsions, where no oil and aqueous phase release within the observation time (6months after emulsification), were prepared in high concentrated suspensions (4.0wt%). The emulsion stability can be attributed to the particle adsorption onto the droplet surface, and more importantly, the gel structure of the suspension. This kind of emulsions with high particle loading and outstanding stability can be potential candidates for macroporous materials.
2. Pickering emulsions stabilized by LDH particles and methyl orange
The adsorption of colloidal particles on liquid droplets in Pickering emulsions has also been exploited to produce colloidosomes and macroporous materials. Emulsions stabilized by the functional particles could result in the materials with expected function. However, very few studies focused on the particle hydrophobization through the adsorption of functional amphiphiles, although it could offer a facile way to fabricate functional materials. Liquid paraffin-in-water emulsions have been prepared by mixing oil with LDH dispersions after in situ modification of the particles with MO. The roles of MO in the emulsions stabilized by LDH particles have been investigated in detail. MO can tailor the wettability of particles in liquids, confirmed by the increased contact angles and enhanced emulsion stability. Then the fluorescence of MO was exploited to offer the in situ microscopic images of particle adsorption onto droplet surface using confocal fluorescence microscopy. Finally, with the obtained emulsion as a soft template, hollow colloidosomes composed of MO-modified LDH with fluorescence were fabricated and observed with SEM.
Owing to the fluorescence and amphiphilic property of MO, the LDH particles are rendered fluorescent and partially hydrophobic in a single-step process, leading to the self-assembly of fluorescent particles at oil/water interfaces. This could open further opportunities for the development of a facile way to fabricate fluorescent materials. Moreover, due to the fact that some dye molecules may affect the particles at liquid interfaces, we also offer a valuable warning for future investigations that fluorescent dyes should not be blindly employed as probes in Pickering emulsions.
3. Nonspherical droplets of emulsions stabilized by layered double hydroxide particles modified with sodium alkyl carboxylates
Nonspherical droplets of emulsions stabilized by layered double hydroxide (LDH) particles in situ modified with sodium alkyl carboxylates (sodium butyrate, C4Na or sodium benzoate, C7Na) were prepared directly through emulsification. The nonspherical degree of droplets as a function of sodium alkyl carboxylate concentration at different rotating speeds was discussed and the origin of nonspherical droplets was investigated.
Based on the results of nonspherical degree, optical microscope images and releasing oil fraction, the generation of nonspherical droplets can be ascribed to partial coalescence of droplets with vacant holes in the particle layer induced by shear during emulsification. The increased contact angles of hydrophilic LDH particles (closer to90°) as a result of the increased sodium alkyl carboxylate concentration leads to the strong affinity of particles for the water/oil interface. Besides, the decreased zeta potential of LDH particles confers the decrease of the electrostatic repulsion among the particles. In this case, a denser particle layer will form at the oil/water interface. Besides, the decrease of particle surface charge density can also promote the attachment of particles at the droplet surface. These factors would facilitate the formation of a stronger structure composed of particles at the interface, corresponding to a lower value of deformation degree. SEM was employed to observe the morphology and surfaces of emulsion droplets. The nonspherical droplets were surrounded with the jammed plate-like particles, demonstrating that nonspherical shapes are preserved by the jammed particle shells resulted from the partial coalescence of neighboring droplets as well.
在很多的研究工作中,表面活性剂经常被用于调控颗粒的润湿性,使颗粒更容易在油水界面上吸附从而获得稳定的Pickering乳液。然而,表面活性剂与颗粒在共同稳定乳液的过程中还会存在竞争作用,它们在油／水界面的竞争吸附往往会影响乳液的稳定性,表面活性剂甚至能够直接导致颗粒从油／水界面脱附,为Pickering乳液的应用带来诸多不利影响。与表面活性剂相比,短链双亲分子在油水界面上的吸附能力较弱且无法单独稳定乳液,因此,它们作为颗粒改性剂的使用可以有效的避免这一问题的出现。不仅如此,短链双亲分子在水溶液中具有高的溶解度和临界聚集浓度,在固体颗粒含量较高的分散体系中对颗粒进行润湿性调节时更具优势。迄今为止,人们对短链双亲分子与颗粒的协同作用已有了初步的认识,但是对该复合体系在稳定乳液过程中表现出来的规律仍然缺乏系统的研究。
本文选择了两种带相反电荷且具有不同形貌的亲水性颗粒作为模型颗粒一带有负电荷的圆盘状锂皂石(Laponite)和带有正电荷的层状双金属氢氧化物(Layered double hydroxide compounds,简称LDH)。首先,系统研究了Laponite颗粒和短链脂肪胺共同稳定的乳液体系。继而,我们在LDH颗粒稳定的乳液体系中引入了一种具有荧光性质的短链双亲分子甲基橙,得到了稳定的乳液并以此为模板制备了中空胶囊。最后,我们在短链羧酸钠(丁酸钠和苯甲酸钠)原位改性的LDH颗粒稳定的乳液中发现了非球形乳液滴并对此进行了研究。
本文的主要内容包括以下三部分：
1.短链脂肪胺改性的Laponite颗粒稳定的乳液
考察了由盘状Laponite颗粒与短链脂肪胺(二乙胺DEA和三乙胺TEA)混合水分散体系制备的Pickering乳液的稳定性。首先,我们考察了当锂皂石颗粒浓度较低(0.5wt%)时短链胺的加入对分散体系和最终所得乳液性质的影响。红外光谱和zeta电位的表征证明了短链胺分子在锂皂石颗粒表面的吸附。由于DEA和TEA分子结构中都存在极性氨基,在一定pH的水溶液中会发生部分水解而带正电,因此可与带有相反电荷的锂皂石颗粒产生静电相互作用而吸附在颗粒表面。随着胺浓度的增加,胺分子在锂皂石颗粒表面的吸附量逐渐增加并最终达到平台,此时胺分子在颗粒表面的吸附达到饱和。胺分子的吸附使锂皂石颗粒表面变得部分疏水,表现为其三相接触角随着胺浓度的增加而增大并最终到达平台值。对应的乳液也随着胺浓度的增大逐渐变得稳定,到达平台之后不再发生变化。荧光显微镜和扫描电子显微镜观察共同证实了短链胺改性的锂皂石颗粒在乳液滴表面的吸附。
当Laponite浓度较高(4.0wt%)时,我们通过流变实验证实了胺分子的加入使锂皂石颗粒水分散体系的粘度降低,有利于乳液的形成。并且,高浓度分散体系和乳液稳定性随着胺浓度的增加的变化规律与低浓度时基本一致,但是所制备的乳液稳定性极佳,放置长达六个月的时间也不会出现分水分油的现象。
2. LDH颗粒与甲基橙共同稳定的乳液
颗粒在乳液滴表面的自组装使Pickering乳液可以作为模板来制备中空胶囊等材料,而具有特殊性质的功能性颗粒稳定的乳液通常可以得到功能性材料。利用功能分子来调节颗粒润湿性将为一些特殊功能材料的制备提供一种简便的方法。以往将颗粒改性的方法仅仅局限于对颗粒润湿性的调节,功能性分子很少被用于调节颗粒润湿性从而稳定乳液以得到相应的功能性材料。
我们引入了一种常见的荧光染料甲基橙作为双亲分子对LDH颗粒进行修饰并制备了稳定的Pickering乳液。这里甲基橙的特点在于可以同时将LDH颗粒进行疏水改性并赋予其荧光性质。为了考察甲基橙在LDH颗粒稳定的乳液中所发挥的作用,我们首先讨论了甲基橙作为双亲分子对LDH分散体系及其稳定的乳液的影响,通过吸附等温线和zeta电位测试证明了甲基橙分子在LDH表面的吸附,颗粒三相接触角的增大证实了甲基橙分子的吸附的确使LDH颗粒的疏水性增强,从而提高了所得乳液的稳定性,表现为乳液体积分数的增大和乳液滴平均粒径的减小。然后我们利用甲基橙分子的荧光性质在激光共聚焦显微镜下原位观察到了甲基橙改性的LDH颗粒在乳液滴表面的吸附。值得注意的是,甲基橙不仅可以吸附在LDH的外表面上,还可以通过阴离子交换进入其层间,为改性的LDH颗粒带来特殊的荧光性质。最后,我们以所得的Pickering乳液为模板制备了由甲基橙插层的LDH颗粒构成的中空胶囊,并且通过SEM观察了中空胶囊的形貌及壳层表面的片状颗粒的排布。甲基橙所发挥的荧光双亲分子的作用为荧光材料的制备提供了一种简便的方法。
3.LDH颗粒与短链羧酸钠共同稳定的非球形Pickering乳液
我们在短链羧酸钠(丁酸钠和苯甲酸钠)原位改性的LDH颗粒稳定的乳液中意外的发现了大量的非球形乳液滴。我们对此现象进行了研究,考察了乳化转速、短链羧酸钠浓度和类型对乳液滴的非球形化程度的影响。乳液滴的非球形化程度与乳液析油体积分数的变化趋势一致,较高的非球形化程度往往对应着较大的乳液析油体积分数,由此可以推断出非球形乳液滴的形成主要是乳化过程中液滴之间的有限聚结所导致的。
短链羧酸钠的类型和浓度对乳液滴的非球形化程度也有着显著的影响。当乳化转速固定时,不论是丁酸钠还是苯甲酸钠对应的乳液体系,乳液滴的非球形化程度均随着短链羧酸钠浓度的增大而减小,超过一定浓度后达到平台值。界面流变实验结果表明,短链羧酸钠浓度和类型的变化对乳液滴非球形化程度的影响与乳液滴表面的颗粒膜强度有关。我们通过对LDH/短链羧酸钠混合水分散体系中颗粒接触角和zeta电位的表征证明了颗粒疏水性的增加和静电斥力的减小,这两种因素使体系界面膜的粘弹性增加,进而导致乳液滴变形程度减小。此外,我们将乳液滴的内相固化后通过SEM对其形貌进行了观察,发现片状颗粒在非球形乳液滴表面明显呈“拥挤”状态,再次确认了非球形乳液滴的形成是乳液滴之间的有限聚结所导致的。
An emulsion is a thermodynamically unstable system which consists of dispersed droplets of one immiscible liquid in another. The system shows a tendency to break to reduce the interfacial area. Therefore a stabilizer is needed, including surfactants, surface-active polymers and solid particles. Emulsions stabilized by colloid particles, commonly named Pickering emulsions, have been studied extensively for their widespread use in practical applications, such as food, pharmaceutics, cosmetics, oil recovery and wastewater treatment since the beginning of20th century. In many of these applications, the stability of emulsions is necessary to keep their properties over long periods of time. Up to now, various theories about emulsions stabilized by solid particles have been developed and recently a thorough understanding of them has been achieved. According to these theories, particle wettability is a crucial parameter which determines the type and stability of the emulsions. Stable emulsions are prepared with particles of intermediate wettability.
To meet the need of appropriate wettability for stability of emulsions, the particles are usually modified via addition of surfactants. There is strong synergy in most combinations of particles and surfactants in stabilizing emulsions. Cationic, anionic, and nonionic surfactants have all been applied successfully to tailor the wettability of particles in liquids and thus prepare stable emulsions. However, there is always competitive adsorption at the oil/water interfaces between the modified particles and the free surfactant molecules in the bulk solution. The free surfactant molecules can even dominate and determine the properties of emulsions. This will bring about many disadvantages in the practical applications of Pickering emulsions. The introduction of short-chain amphiphiles can resolve this problem effectively, due to the incapability of displacing particles at the oil/water interfaces. In addition, the short amphiphiles exhibit high solubility and critical micelle concentrations in water, enabling the surface modification of high concentrations of particles.
Based on the study on emulsion field above, two kinds of hydrophilic particles with different shapes and opposite charges, layered double hydroxides (LDH) and Laponite, are investigated. First, liquid paraffin-in-water emulsions stabilized by Laponite particles modified with short-chain aliphatic amines (diethylamine, DEA or triethylamine, TEA) were prepared. Then, methyl orange molecules have been used as fluorescent amphiphiles in preparation of emulsions stabilized by LDH particles. The self-assembly of fluorescent particles at droplet surfaces is accomplished, which has been exploited to produce hollow colloidosomes. Nonspherical droplets in emulsions stabilized by LDH particles in situ modified with sodium alkyl carboxylates (sodium butyrate, C4Na or sodium benzoate, C7Na) can be obtained directly through emulsification. The presence of nonspherical droplets is mainly attributed to the partial coalescence of neighboring droplets.
The present dissertation includes three topics.
1. Pickering emulsions stabilized by Laponite particles modified with short-chain aliphatic amines
Liquid paraffin-in-water emulsions were successfully prepared by mixing oil with Laponite suspensions after in situ modification of the particles with short-chain aliphatic amines, DEA and TEA. The adsorption of DEA or TEA brings about enhancement of particle hydrophobicity and decrease of zeta potential, which make it easier for them to adsorb at oil-water interfaces. It was found that, at low clay concentration (0.5wt%), stable emulsions can be obtained when the clay-amine suspensions are flocculated. The emulsion stability improves with amine addition and reaches a plateau above a certain amine concentration. The variation of mean droplet size of emulsions is consistent with the emulsion stability. Emulsions of best stability are formed from the most unstable particle suspensions. The adsorption of the modified clay particles on the droplet surface results in emulsion stabilization, which was confirmed by laser-induced fluorescent confocal micrographs and SEM observations.
Furthermore, extremely stable emulsions, where no oil and aqueous phase release within the observation time (6months after emulsification), were prepared in high concentrated suspensions (4.0wt%). The emulsion stability can be attributed to the particle adsorption onto the droplet surface, and more importantly, the gel structure of the suspension. This kind of emulsions with high particle loading and outstanding stability can be potential candidates for macroporous materials.
2. Pickering emulsions stabilized by LDH particles and methyl orange
The adsorption of colloidal particles on liquid droplets in Pickering emulsions has also been exploited to produce colloidosomes and macroporous materials. Emulsions stabilized by the functional particles could result in the materials with expected function. However, very few studies focused on the particle hydrophobization through the adsorption of functional amphiphiles, although it could offer a facile way to fabricate functional materials. Liquid paraffin-in-water emulsions have been prepared by mixing oil with LDH dispersions after in situ modification of the particles with MO. The roles of MO in the emulsions stabilized by LDH particles have been investigated in detail. MO can tailor the wettability of particles in liquids, confirmed by the increased contact angles and enhanced emulsion stability. Then the fluorescence of MO was exploited to offer the in situ microscopic images of particle adsorption onto droplet surface using confocal fluorescence microscopy. Finally, with the obtained emulsion as a soft template, hollow colloidosomes composed of MO-modified LDH with fluorescence were fabricated and observed with SEM.
Owing to the fluorescence and amphiphilic property of MO, the LDH particles are rendered fluorescent and partially hydrophobic in a single-step process, leading to the self-assembly of fluorescent particles at oil/water interfaces. This could open further opportunities for the development of a facile way to fabricate fluorescent materials. Moreover, due to the fact that some dye molecules may affect the particles at liquid interfaces, we also offer a valuable warning for future investigations that fluorescent dyes should not be blindly employed as probes in Pickering emulsions.
3. Nonspherical droplets of emulsions stabilized by layered double hydroxide particles modified with sodium alkyl carboxylates
Nonspherical droplets of emulsions stabilized by layered double hydroxide (LDH) particles in situ modified with sodium alkyl carboxylates (sodium butyrate, C4Na or sodium benzoate, C7Na) were prepared directly through emulsification. The nonspherical degree of droplets as a function of sodium alkyl carboxylate concentration at different rotating speeds was discussed and the origin of nonspherical droplets was investigated.
Based on the results of nonspherical degree, optical microscope images and releasing oil fraction, the generation of nonspherical droplets can be ascribed to partial coalescence of droplets with vacant holes in the particle layer induced by shear during emulsification. The increased contact angles of hydrophilic LDH particles (closer to90°) as a result of the increased sodium alkyl carboxylate concentration leads to the strong affinity of particles for the water/oil interface. Besides, the decreased zeta potential of LDH particles confers the decrease of the electrostatic repulsion among the particles. In this case, a denser particle layer will form at the oil/water interface. Besides, the decrease of particle surface charge density can also promote the attachment of particles at the droplet surface. These factors would facilitate the formation of a stronger structure composed of particles at the interface, corresponding to a lower value of deformation degree. SEM was employed to observe the morphology and surfaces of emulsion droplets. The nonspherical droplets were surrounded with the jammed plate-like particles, demonstrating that nonspherical shapes are preserved by the jammed particle shells resulted from the partial coalescence of neighboring droplets as well.
引文
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