摘要
新型功能性纳米颗粒材料及其稳定的皮克林乳液，在很多领域中的研究与应用引起了人们极大的重视和关注。片状粘土颗粒作为无机固体矿物材料，其资源储量十分丰富，是廉价、环保的矿物资源之一。迄今为止，粘土资源在乳状液的乳化和破乳技术中的潜在价值远没有得到完全开发和利用，尤其是在造纸乳剂类化学品中的应用并未得到充分的研究，如何有效、高值化利用粘土矿物制备造纸化学品将成为制浆造纸清洁生产及无少污染生产研究的重要课题。微粒乳化技术和皮克林乳液在造纸工业中的应用和研究尚属空白，而乳液型助剂在造纸工业中的应用十分广泛，为开发更有效的乳化与分散体系，促进皮克林乳液型造纸助剂及化学品的研究与应用，本论文对片状粘土纳米颗粒乳化稳定的ASA皮克林乳液的乳化性能、稳定机理及施胶应用等方面进行了系统研究。这些研究的开展不仅为微粒乳化稳定机理提供基础研究，而且为造纸助剂的开发和应用领域开辟了新方向。
1.阴离子片状粘土颗粒乳化稳定的ASA皮克林乳液。MMT颗粒浓度影响颗粒界面吸附性能及连续相中3D网络结构的形成，当C_p为1%时即可制备出粒径均一的乳液，C_p为1.5%时可制备出小粒径、高稳定性的ASA乳液。油相体积分数影响乳液的稳定性及乳液类型，Фo在0.8处发生突变转相。调节MMT水分散液的pH值可以控制颗粒润湿性、颗粒—颗粒（油/水界面上）以及颗粒—界面之间的静电作用力，改善颗粒的界面吸附以及乳液稳定性能，在pH=7时可以制备出均一稳定的ASA乳液。电解质的添加降低了带电粒子之间的相互排斥作用并使颗粒膜变得更致密。不同链长的烷烃对ASA乳液乳化性能及稳定性有明显影响，十二烷与ASA复配的乳化效果最佳。乳液CLSM证明了颗粒在皮克林乳液油/水界面处的吸附，形成的固体颗粒界面膜有效阻止乳滴间的聚结，起到稳定乳液的作用。
2.阳离子片状粘土颗粒及与阴离子片状粘土颗粒复配乳化体系乳化稳定ASA皮克林乳液。NaCl的添加对LDHs乳化的ASA乳液稳定性具有促进作用，增大NaCl浓度可以改善LDHs颗粒在油/水界面的吸附，促进致密颗粒膜的形成，从而降低ASA乳液液滴粒径。油相体积分数的增大使乳液黏度的迅速提高，有利于乳液的分层稳定性。MMT与LDHs组成的复配固体颗粒乳化体系，在MMT/LDHs质量比为0.11或9时可以制备出均一稳定的ASA乳液，并且复配体系要比颗粒单独使用时乳化稳定作用更好。粘土颗粒卡片房结构由片状颗粒的正电边缘和负电端面通过静电吸引作用搭接而成，其形状为多边网格结构，并且随着三角格和四边格结构通过边—面搭接，可能进一步形成六角形结构单元，这种结构单元将作为卡片房网络结构以及粘土颗粒空间三维网络结构体的基本结构单元。颗粒浓度的提高使乳液储能模量提高，颗粒之间的作用力变强，三维网络结构体更为致密，乳液表现出强弹性行为。这种流变性为可用修复性三维网络结构的形成来解释。而颗粒三维网络结构的恢复和形成具有滞后性，并且复配颗粒的滞后性现象更为明显。复配颗粒乳化的ASA乳液在150min内具有良好的施胶性能。原子力显微镜显示了施胶纸张纤维形貌、排列变化和片状颗粒在纤维表面的留着。
3.改性蒙脱石乳化稳定ODSA乳液。利用末端带有反应型三功能基的硅烷偶联剂γ-MPTMS对纳米级钠基蒙脱石固体颗粒进行表面接枝改性，经SEM、表面接触角、FT-IR和TGA等检测表明MPTMS成功接枝到蒙脱石表面。乳化体系的pH值对MPTMS改性蒙脱石制备的ODSA皮克林乳液稳定性有重要的影响，pH为7时可以制备出粒径均一稳定的油包水型乳液。油水比会影响ODSA皮克林乳液的乳液类型，1.5%浓度改性颗粒制备的乳液在油水比为3:1时发生转向，由水包油乳液转变为油包水乳液，随着颗粒浓度的提高，转向点随之提高。颗粒浓度C_p对乳液稳定性具有重要的影响，C_p~1.0%时可以将ODSA液滴完全包裹，C_p~1.5%时连续相中形成完整致密的颗粒3D网络结构，制备出均一稳定的乳液。所制备的ODSA皮克林乳液为非牛顿流体，具有明显的类固体流变性，随着C_p的增大呈现明显的剪切变稀性。ODSA乳液LRS及FT-IR分析表明改性颗粒对乳液水解稳定性具有明显的改善作用，改性蒙脱石乳化的ODSA乳液较未改性颗粒及常规表面活性剂乳化的乳液具有更好的施胶活性。
4.改性MMT乳化稳定ASALP乳液及其稳定机理。利用三功能基硅烷偶联剂表面接枝改性的纳米蒙脱石固体颗粒制备均一稳定的ASALP皮克林乳液，液体石蜡添加量在30%～60%时即可制备出小粒径的水包油型乳液。乳液CLSM分析显示了改性蒙脱石固体颗粒在油水界面处的吸附，以及固体颗粒膜对液滴聚并的保护稳定作用。乳液流变性分析表明ASALP乳液为类似固体黏弹性的非牛顿流体，揭示了连续相中固体颗粒网络结构及有机改性颗粒之间相互作用对乳液流变性的影响。乳液制备完成后的5h内具有较高的水解稳定性，10h后水解完全。LP的添加改善了ASA的施胶效果，ASALP皮克林乳液浆内施胶纸张表面具有类荷叶结构，明显改善纸张的表面疏水性能，为复配型施胶剂的设计和开发提供理论依据和参考。
5.磁性纳米颗粒乳化稳定ASA乳液。Fe_3O_4颗粒浓度、油相体积分数、pH值对ODSA乳液稳定性、乳液的类型以及液滴形态有明显影响，磁性纳米Fe_3O_4颗粒作为稳定乳化剂可以制备稳定的皮克林型ASA施胶剂乳液。随着固体颗粒用量的增加，乳液稳定性先升高后降低，固体粒子用量在0.1~0.3wt%时乳液具有较好分层稳定性。油相体积分数的增加会引起乳液类型的转变，但乳液稳定性增强，油相体积分数为0.5~0.66时乳液分层稳定性较好且为O/W型乳液。当pH值为7~8时，可以制备粒径小、分布均一的乳液。乳液放置时间1h内具有良好的施胶活性，随着放置时间的增长，施胶性能逐渐降低。
Preraration and application of novel and functional nanoparticle materials and Pickeringemulsions have attracted extensive attention because of the particular performances andapplications in wide fields. As an inorganic solid mineral material, clay mineral particle is richin resources, low-cost and environment-friendly. However, the potential value of the clays inthe particulate emulsification and demulsification technology has not been effectivelyexploited, especially in the papermaking industry. Effective and high-value utilization of claysin the emulsification of paper chemicals is one of the most important and challenging researchareas in the cleaner and non-pollution production.To the best of our knowledge, few studieshave been conducted on the application of particulate emulsifiers in the papermaking industry.For the purpose of efficiently emusification dispersion systems and promoting the researchand application of Pickering-type emulsions of papermaking additives, the current workfocused on emulsification performance, stability mechanism and sizing performance of ASAemulsions stabilized by layered clay nanoparticles. This study on Pickering-type ASAemulsions not only provied the basic research, but also opens up a new route to thepreparation of a variety of paper sizing agents in the papermaking industry.
1. Pickering-type ASA emulsions stabilized by anionic layered clay particle. Particleconcentration of MMT had greatly effects on both the enrichment of these particles at theoil–water interface and the formation of the three-dimensional network built-up by the MMTlamellae. Stable ASA emulsions containing1wt%MMT particles could be obtained and morestable emulsion with smaller doplet diameter could be prepared at C_p~1.5wt%. The initialoil fraction obviously influenced on the type and stability of ASA emulion. Catastrophic phaseinversion occured when the value of Фowas0.8. Adjusting the pH value of MMT aqueousdispersion changed the wettability and electrostatic interactions of particle-particle andparticle-interface, promoting the stability of emulsion. Stable ASA emulsion withoutseparated phase was prepared at pH~7. The addition of sults weakened the electrostaticinteractions of charged MMT particles, which enhancing the envelope of particles. Theemulsification and stability was obviously influenced when the alkanes with different chainscooperated with ASA oil. The synergic effect of dodecane was more obvious than other alkenes. The CLSM analysis indicated the enrichment of these particles at the oil–waterinterface of Pickering emulsions and the envelope of particles creates a barrier which impededthe droplets from coalescence.
2. ASA Pickering emulsions stabilized by cationic layered clay particles solely andco-stabilized with anionic layered clay particles. Sults boosted the stability of LDHs stabilizedASA emulison. Increasing the content of NaCl could improve the adsorption of particle at theoil/water interface and the creation of compact particulate envelope, reducing the droplet size.The stability of ASA emulsion to separation depended on the viscosity and oil volumefraction. For the MMT/LDHs co-stabilizer system, homogeneous and stable ASA emulsionscould be prepared when the mass ratio of MMT/LDHs was0.11or9. The house-cardstructure of clay particles that formed through the electrostatic attraction between positive andnegative platelet-edages would evolve into hexagonal structure, which could be the basicstructure unit of the clay-particle3D-network. We also found that co-stabilization system wasbetter than the solo stabilization system on the ASA emulsion. At low strain amplitude, thehiger the particle concentration was, the greater the storage modulus was, indicating astronger interparticle interaction and the three-dimensional network and a solidlikeviscoelastic behavior of the emulsion. This rheological behavior can be explained by theformation of the reversible particulate network in the emulsion. However, the rebuilding ofthree-dimensional network exhibited hysteresis, especially in the co-stabilizer system.MMT/LDHs stabilized ASA emulsion had good sizing performance within150min storagetime. AFM analysis indicated the change of fiber morphology and arrangement and theadsorption of layered particles.
3. ODSA emulsion stabilized by γ-Methacryloxy propyl trimethoxysilane grafted MMT. Toprepare stable ODSA Pickering emulsions, montmorillonite clay-particles modified byγ-Methacryloxy propyl trimethoxysilane (γ-MPTMS) were used as particulate emulsifiers ofODSA and water at room temperature. The effects of pH value, oil-to-water ratio, and particleconcentration on the stability of the Pickering emulsions were investigated. The stability ofODSA emulsions in the presence of grafted-MMT first increased and then decreased as thepH value of the aqueous phase decreased. The critical pH for the phase separation of theODSA emulsions was~7. Addition of ODSA oil induced phase inversion from an O/W emulsion to a W/O emulsion when the ratio of oil-to-water passed a specific threshold of3:1(C_p~1.5wt%). The particle concentration was linked to the formation of particle films atoil–water interface and of clay particle networks in water phase. The ODSA emulsionsstabilized by grafted-MMT could have good sizing performance and lifespan. This study onODSA Pickering emulsions based on MPTMS-grafted MMT particles opens up a new route tothe preparation of a variety of paper sizing agents in the papermaking industry.
4. Stablization and mechanism of ASALP emulsion prepared by grafted-MMT particles.Based on this study, it was found that MPTMS-grafted-MMT particles could be used forpreparing stable oil-in-water Pickering emulsions of ASA by emulsification in combinationwith30~60vol.%paraffin oil. The ASALP Pickering emulsions exhibited some kind of asolidlike viscoelastic behavior, which may be resulted from the particulate network formed bygrafted-MMT particles at oil/water interface and influence of the organic coemulsifier on theparticle–particle interactions. LP oil added not only improveed the stability of ASA Pickeringemulsions stabilized by particulate emulsifier, but also significantly promoted the stability andinternal paper sizing performance of ASA. Lotus-leaf-like paper surface structure would formthrough the ASALP internal sizing, which would facilitate the design of composite sizingagents.
5. ASA emulsions stabilized by Magnetic Fe_3O_4nanoparticles. Magnetic Fe_3O_4nanoparticles were used as the stabilizer to prepare Pickering-type ASA emulsions. Particleconcentration, oil/water volume ratio, oil polarity, pH value of aqueous phase had significanteffects on the type, stability, and morphology of ASA emulsion. With the increase of Fe_3O_4particle concentration, the stability of emulsion to creaming and coalescence initiallyincreased and then decrease, and0.1~0.3wt%particles performed good stabilizationperformance. Increasing the volume fraction of ASA oil phase lead to phase conversation butincreased the stability of emulsion to separeation. Stable O/W type ASA emulsion wasprepared when the value of Φowas0.5~0.66. Adjusting the pH value of aqueous couldinprove the stability of emulsions to coalescence and separation. Homogeneous ASAemulsions with small droplet size were prepared at pH7~8. Fe_3O_4particles stabilized ASAemulsions presented well sizing performance in about1h storage time. However, there was asignificant reduction of sizing degree in prolonged storage time.
引文
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