有机改性蒙脱土在非极性介质中的分散及其稳定的Pickering乳液
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摘要
蒙脱土由于具有很强的吸附能力和膨胀性等特殊的性质,因而有着广泛的应用,但其表面亲水性强,限制了其在非水介质中的应用。利用蒙脱土层间阳离子的可交换性,将阳离子表面活性剂引入蒙脱土层间对其进行有机改性,使其表面疏水化,增大粘土的层间距,从而提高其与有机物的相容性。由于有机改性的蒙脱土(又称有机土)在涂料、胶黏剂、润滑油脂、复合材料、污水处理和钻井液等行业中具有广泛的应用,因而人们对有机土从基础理论和应用方面进行了广泛研究。有机土最重要的特性之一就是可以在有机介质中膨胀形成具有触变性的凝胶结构,同时由于其具有廉价易得,用量低,抗高温性能好,不易受其他化学物质影响等优点,因而有机土在很多领域被用作增粘剂或胶凝剂。
最近有机土在纳米复合材料领域的应用引起了人们的极大关注。粘土颗粒由于其特殊的层状结构和物理性能,被认为是优良的填充材料,可以提高材料的强度和耐温性等性能。但是由于蒙脱土的强亲水性,与有机物的亲和力较差,这就需要对蒙脱土进行有机改性。由于蒙脱土的有机化改性降低了其与有机物之间的界面能,从而使有机土可以和聚合物相容。其次,由于有机改性分子可与聚合物分子上的基团发生反应,进一步增强有机土与聚合物分子之间的相互作用力,从而制备出均一的复合材料。
油基钻井液是以油作为连续相的钻井液。与水基钻井液相比较,油基钻井液具有抗高温,很强的抑制性和抗盐、抗钙污染的能力,润滑性能好,并可有效地减轻对油气层的损害等优势,因此在深井、高温井、复杂地层复杂井、大位移井等特殊结构井及储层保护要求高的井中具有显著优势,并且已在国内外大量使用。但是随着人们对环境保护越来越重视,当人们用毒性较低的白油等芳烃含量少的非极性油来代替原油、柴油作为基础油时,有机土存在着在白油中成胶、分散能力弱的问题。另外,在油包水(W/O)钻井液中,有机土可以吸附在油水界面,提高乳液的稳定性,增加钻井液的粘度。
本文基于以上背景,研究了有机土的制备和有机土在非极性溶剂中的分散以及改进其分散稳定性的方法,测定了分散体系的流变行为,并对有机土稳定的乳液和影响乳液稳定性的因素进行了研究。
1.有机土的制备及其在白油中的流变行为
用双十八烷基二甲基氯化铵对蒙脱土进行表面疏水改性制备有机土,并用傅里叶转变红外光谱(FTIR)、X-射线衍射(XRD)、热重分析(TGA)和扫描电子显微镜(SEM)等手段对有机土进行了表征。考察了反应时间、反应温度、反应体系的pH值以及改性剂用量对有机土层间距、有机物含量及其在非极性分散介质中沉降稳定性的影响,确定最佳反应时间为3h,反应温度50～90℃,不需要调节反应体系的pH值,改性剂用量为蒙脱土土阳离子交换容量的1.0倍即1.0CEC。增大改性剂用量,有机土的层间距增大,热稳定性降低。当改性剂用量增大至1.4CEC时,改性剂在蒙脱土上双层吸附。
随着石油勘探开发的不断深入和社会对环保问题的逐渐重视,毒性较小,更加环保的矿物油如白油等逐渐取代了芳烃含量较高的柴油作为油基钻井液的基础油。有机土在白油基钻井液中分散能力较差,增粘效果不理想,需要增大有机土的浓度来调整体系的流变性能。但是当有机土的浓度较高时,油基钻井液的塑性粘度也会随之上升,即体系的剪切稀释性变差。因而本文研究了有机土在白油中的流变行为,发现随着改性剂用量的增大,有机土／白油分散体系的粘度先增大后减小,1.0CEC有机土在白油中的分散稳定性、增粘效果和分散体系的剪切稀释性最好。同时对比了有机土和纳米二氧化硅颗粒的白油分散体系的流变性能,发现亲水性的纳米二氧化硅颗粒的分散体系的稳定性、粘度和剪切稀释性要远优于有机土／白油分散体系。
2.有机土在非极性介质中的分散
颗粒在非极性分散介质中的分散体系在工业中具有广泛应用,例如陶瓷制备、显影技术、油墨、油漆和化妆品等。但是颗粒在非极性介质中的分散体系的稳定性往往较差,通常需要加入分散剂来提高其稳定性。关于分散剂的作用机理,一般认为是空间稳定作用起主导作用。由于分散介质的介电常数较低,颗粒间的静电斥力作用一般被忽略。然而最近的一些研究发现,在非极性介质中静电稳定作用起着重要的作用。人们对球型颗粒在非极性介质中的分散体系研究较多,而对于非等轴胶体颗粒的分散体系研究较少。有机土在非极性介质中的均匀分散是制备纳米复合材料和提高其性能的关键一步,另外研究有机土在非极性介质中的分散状态对于有机土在润滑油脂和油基钻井液中的应用具有指导意义。
有机土在非极性介质中的分散性较差,颗粒迅速沉降。向分散体系中加入非离子表面活性剂脱水山梨醇单油酸酯(Span80)、脱水山梨醇三油酸酯(Span85)和甘油单油酸酯以及阴离子表面活性剂2-乙基己基)磺化琥珀酸钠(AOT)都可以提高有机土分散体系的稳定性。通过紫外、元素分析、小角X-射线衍射等手段,我们发现表面活性剂在有机土表面发生吸附,增大有机土表面的疏水性；表面活性剂吸附在有机土颗粒表面,可以阻碍颗粒聚集,提供空间稳定作用；表面活性剂不仅吸附在有机土表面,而且能够进入有机土层间,进一步增大有机土的层间距,有利于有机土片层在分散介质中剥离,使有机土颗粒尺寸减小；通过测定有机土在非极性分散介质中的zeta电势,发现表面活性剂吸附在颗粒上可以增大颗粒的zeta电势,表面活性剂与有机土颗粒表面通过酸碱相互作用发生电荷转移,使有机土颗粒表面带电,增大了颗粒之间的静电斥力,从而有助于分散体系的稳定性的提高。表面活性剂通过空间稳定和静电稳定作用提高有机土／非极性介质分散体系的稳定性。
3.有机土稳定W／O乳液的研究
有机土在油基钻井液中一般是用作增粘剂,在W／O钻井液中,有机土可以吸附在油水界面,提高乳液的稳定性,增加体系的粘度。油基钻井液的水相通常含有较高浓度的盐,因而研究有机土稳定的W／O乳液以及盐对乳液稳定性的影响具有重要意义,本文考察了有机土的改性剂用量和水相中的盐浓度对有机土稳定的W／O乳液稳定性的影响。
固定体系的油水比和颗粒浓度,改变有机土改性剂用量可以改变有机土稳定的乳液类型。蒙脱土自身亲水性强,不能够形成稳定的乳液；用季铵盐对其进行有机改性,使颗粒表面疏水性增强,当改性剂用量低于0.8CEC时,由于颗粒表面亲水,形成水包油(O／W)乳液；当改性剂用量在0.8～1.2CEC时,颗粒表面的疏水性增强,形成W／O乳液。继续增大改性剂用量,改性剂通过烷基链段间的疏水作用在有机土上双层吸附,使颗粒表面重新亲水,但是却得到O／W乳液,这可能是由于有机土制备过程中的洗涤步骤去除了游离的表面活性剂,而在乳化过程中通过疏水作用吸附的改性剂从颗粒表面发生脱附,颗粒表面的亲水性不够强,因此乳液类型不再随改性剂浓度的进一步增加反转为O／W型。
一般来说,向颗粒水分散体系中加入盐,会屏蔽带电颗粒间的静电斥力同时还会使颗粒表面的亲水性降低,从而促使粘土水分散体系发生絮凝。当盐浓度较低时,颗粒水分散体系会发生弱絮凝,有利于形成稳定的乳液；当盐浓度较高时,颗粒水分散体系发生强絮凝,不利于形成稳定的乳液。本文首次研究了盐浓度对W／O乳液稳定性的影响。将有机土分散在液体石蜡中,改变水相中的盐浓度,发现随着水相中盐浓度的增大,W／O乳液的稳定性降低,当水相中盐浓度超过一定值时,不能形成稳定的乳液。在相同的盐浓度条件下,1.2CEC有机土制备的乳液的稳定性优于1.0CEC有机土,0.8CEC有机土制备的乳液的稳定性最差。通过测定有机土／盐水体系离心后上清液中有机物含量,发现随着盐浓度增大,改性剂在有机土上的脱附量增大。通过测定有机土和不同浓度盐水的接触角,发现随着盐浓度的增大,有机土颗粒表面亲水性增强。综上所述,随着盐浓度的增加有机土稳定的W／O乳液的稳定性降低,这是由于盐的加入促使吸附在有机土外表面的季铵盐发生脱附,导致有机土表面亲水性增强。
Montmorillonite finds wide range of applications for its special properties:natural abundance, fine size, easy modification. The applications of montmorillonite in nonaqueous media were limited for the strong hydrophilicity. However, cation-exchange reactions with organic cationic surfactants have been exploited to render the clay mineral hydrophobic at the surface and increase the basal spacing. Organic modification of montmorillonite (organoclay) has been widely used in industrial applications such as oil-field drilling fluids, paints, lubricating greases, wastewater treatment, and composite material. Thus the modifications of clay minerals have been widely studied fundamentally and in practical applications. One of the most important properties of organoclay is the ability for swelling and thixotropic gel formation in organic media. The advantages of organoclay as flow modifiers include:low volume fractions, good thermal stability, resistant to gel-breaking effects from other chemicals. Organoclay is generally used to control the rheologic property of hydrocarbon fluids.
Recently, the use of organoclay in materials science and technology has attracted considerable attention. Clay, having a large aspect ratio and size, has been recognized as potential candidates for filler materials, because it exhibits superior physical and mechanical properties when compared with the pure polymer. Organic modification of clay mineral, making it hydrophobic and compatible with polymers is necessary due to the hydrophilic nature of clay. The surface energy of clay and polymer could be reduced by organic modification. Additionally, the organic cations may contain various functional groups, which can react with the polymers and enhance the adhesion between clay particles and the matrix. Thus, it is possible to obtain nanocomposites with good dispersion quality.
Oil-based drilling fluid is the mud using oil as the continuous phase. The advantages of selecting an oil-based drilling fluid include:superior hole stability, enhanced shale inhibition, excellent lubrication, high temperature stability. For these benefits, oil-based drilling fluid is a better selection for drilling in deep well, high temperature well and complex conditions. For environment protection, miner oil of lower toxic was used to replace the crude oil or diesel which contains high content of aromatic hydrocarbons, but there is a problem that the organoclay could not disperse and gelling well in miner oil. In the water-in-oil (W/O) drilling fluid, orgaoclay can be adsorbed on the interface of oil and water, improving the stability of emulsion and the viscosity of drilling fluid.
In this context, we studied the dispersion of organoclay in octane in attempt to improve their stability. The rheological properties of organoclay suspensions were also investigated. The emulsion stabilized by organoclay was prepared, and the factors affecting their stability were evaluated.
The present dissertation includes three topics.
1. Preparation, characterization of organocaly and rheological properties of organoclay suspension
Cationic surfactant dimethyldioctadecylammoniurn chloride (DODMAC1) was used as the modifier to prepare organoclay, and the product was characterized by fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscope (SEM). The effects of reaction time, temperature, pH value and the amounts of organic modifier on the basal spacing and amounts of organic compounds of organoclay and the stability of organoclay suspension were investigated. The optimal reaction condition was carried at50-90℃for3h with1.0cation exchange capacity (CEC) cationic surfactant. If the amount of surfactant was increased, the thermal stability of the organoclay would decrease. When the addition of surfactant was more than1.4CEC, bilayer adsorption of surfactant would occur.
When organoclay is used as thickener in nonpolar miner oil such as white oil based drilling fluid, ideal result could not be achieved. Therefore we studied the rheological properties of organoclay/white oil suspension. The viscosity of the suspension increased with the dosage of DODMAC1first, and then decreased. The suspension containing organoclay of1.0CEC exhibited the maximum stability, viscosity and share thinning property. The rheological properties of silica nanoparticles suspended in a non-polar mineral oil were also investigated. The stability, viscosity and thixotropic property of silica nanoparticles are much better than organoclay.
2. Dispersion of organoclay in nonpolar media
Dispersions of particles in nonpolar media have many applications in ceramics, paints, lubricants and oil-based drilling fluid. Usually, dispersions of particles in nonpolar media are unstable, and dispersants are used to improve the stability of the dispersions. The mechanism of dispersant to improve the stability of dispersions is steric stabilization. Usually, electrostatic stabilization in nonpolar media was neglected because of the low dielectric constant. However, many recent studies have shown that electrostatic stabilization can play an important role. To improve the dispersion stability of organoclay in nonpolar media is important for improving the properties of polymer-clay nanocomposites, lubricants and oil-based drilling fluids. Thus we investigated the stabilization mechanism of organoclay in octane.
The dispersion of organoclay can be improved by the addition of the nonionic surfactants sorbitan monoleate (Span80), sorbitan trioleate (Span85) and1-oleoyl-rac-glycerol and anion surfactant sodium bis(2-ethylhexyl) sulfosuccinate (AOT). The relation between the adsorption of surfactants on organoclay particles and the stability of the dispersions was investigated. The effects of the surfactants on the basal spacing of particles, electrostatic interactions between particles and rheological properties of dispersions were also measured. Based on the decrease of the particle size and the increase of the zeta potential, the improvement of the dispersion stability could be interpreted by steric and electrostatic stabilization. This work sheds some light on the selection of dispersants for improving the dispersion stability of particles in nonpolar media.
3. Pickering emulsion stabilized by organoclay
Organoclay typically is used to control the rheology in oil-based drilling fluid. In drilling fluid, the organoclay could also adsorb at the surface of water droplets to stabilize the W/O emulsions and improve the viscosity of mud. The aqueous phase of mud is usually comprised of high concentration of salt, to minimize water exchange between drilling fluid and the formation being drilled. Because the wettability of organoclay and salt concentration in the aqueous phase could affect the stability of the emulsion, we investigated the effects of modifier dosage of organoclay and salt concentration in the aqueous phase on the stability of W/O emulsions stabilized by organoclay.
Emulsion inversion could be induced by increasing the addition of cationic surfactant modifier, as the wettability of organoclay was changed from hydrophilicity to hydrophobicity. When the amount of surfactant was less than0.8CEC, the emulsions stabilized by organoclay were O/W. When the amount of surfactant was more than0.8CEC, W/O emulsions were prepared by the hydrophobic organoclay. If the addition of surfactant was increased further, O/W emulsions were not obtained. This may be due to the removal the free surfactant in the washing process in the preparation of organoclay and the reduction of organoclay hydrophobicity by desorption of the adsorbed bilayer surfactant in emulsification process.
The addition of salt could increase the hydrophobicity of particles and decrease particle zeta potential leading particle adsorption at the oil-water interface. Salts could also flocculate the particles to form visco-elastic three-dimensional network, which enhance the creaming stability of emulsion. Here, the effect of salt concentration on the W/O emulsions stabilized by organoclay was studied. The stability of emulsions decreased with the salt concentration, and stable emulsion could not be prepared when the salt concentration was above a certain value. The emulsion prepared with organoclay of1.2CEC was more stable than organoclay of1.0CEC and0.8CEC. The desorption of cationic surfactant from organoclay was measured by Total Organic Carbon Analyzer. The amount of surfactant desorbed increased with salt concentration. The desorption of cationic surfactant modifier would increase the hydrophilicity of organoclay, which is not conductive for the formation of W/O emulsion. The reasons of the decrease of the emulsion stability caused by the addition of salt were the reduction of organoclay hydrophobicity and the desorption of cationic surfactant at high salt concentration.
最近有机土在纳米复合材料领域的应用引起了人们的极大关注。粘土颗粒由于其特殊的层状结构和物理性能,被认为是优良的填充材料,可以提高材料的强度和耐温性等性能。但是由于蒙脱土的强亲水性,与有机物的亲和力较差,这就需要对蒙脱土进行有机改性。由于蒙脱土的有机化改性降低了其与有机物之间的界面能,从而使有机土可以和聚合物相容。其次,由于有机改性分子可与聚合物分子上的基团发生反应,进一步增强有机土与聚合物分子之间的相互作用力,从而制备出均一的复合材料。
油基钻井液是以油作为连续相的钻井液。与水基钻井液相比较,油基钻井液具有抗高温,很强的抑制性和抗盐、抗钙污染的能力,润滑性能好,并可有效地减轻对油气层的损害等优势,因此在深井、高温井、复杂地层复杂井、大位移井等特殊结构井及储层保护要求高的井中具有显著优势,并且已在国内外大量使用。但是随着人们对环境保护越来越重视,当人们用毒性较低的白油等芳烃含量少的非极性油来代替原油、柴油作为基础油时,有机土存在着在白油中成胶、分散能力弱的问题。另外,在油包水(W/O)钻井液中,有机土可以吸附在油水界面,提高乳液的稳定性,增加钻井液的粘度。
本文基于以上背景,研究了有机土的制备和有机土在非极性溶剂中的分散以及改进其分散稳定性的方法,测定了分散体系的流变行为,并对有机土稳定的乳液和影响乳液稳定性的因素进行了研究。
1.有机土的制备及其在白油中的流变行为
用双十八烷基二甲基氯化铵对蒙脱土进行表面疏水改性制备有机土,并用傅里叶转变红外光谱(FTIR)、X-射线衍射(XRD)、热重分析(TGA)和扫描电子显微镜(SEM)等手段对有机土进行了表征。考察了反应时间、反应温度、反应体系的pH值以及改性剂用量对有机土层间距、有机物含量及其在非极性分散介质中沉降稳定性的影响,确定最佳反应时间为3h,反应温度50～90℃,不需要调节反应体系的pH值,改性剂用量为蒙脱土土阳离子交换容量的1.0倍即1.0CEC。增大改性剂用量,有机土的层间距增大,热稳定性降低。当改性剂用量增大至1.4CEC时,改性剂在蒙脱土上双层吸附。
随着石油勘探开发的不断深入和社会对环保问题的逐渐重视,毒性较小,更加环保的矿物油如白油等逐渐取代了芳烃含量较高的柴油作为油基钻井液的基础油。有机土在白油基钻井液中分散能力较差,增粘效果不理想,需要增大有机土的浓度来调整体系的流变性能。但是当有机土的浓度较高时,油基钻井液的塑性粘度也会随之上升,即体系的剪切稀释性变差。因而本文研究了有机土在白油中的流变行为,发现随着改性剂用量的增大,有机土／白油分散体系的粘度先增大后减小,1.0CEC有机土在白油中的分散稳定性、增粘效果和分散体系的剪切稀释性最好。同时对比了有机土和纳米二氧化硅颗粒的白油分散体系的流变性能,发现亲水性的纳米二氧化硅颗粒的分散体系的稳定性、粘度和剪切稀释性要远优于有机土／白油分散体系。
2.有机土在非极性介质中的分散
颗粒在非极性分散介质中的分散体系在工业中具有广泛应用,例如陶瓷制备、显影技术、油墨、油漆和化妆品等。但是颗粒在非极性介质中的分散体系的稳定性往往较差,通常需要加入分散剂来提高其稳定性。关于分散剂的作用机理,一般认为是空间稳定作用起主导作用。由于分散介质的介电常数较低,颗粒间的静电斥力作用一般被忽略。然而最近的一些研究发现,在非极性介质中静电稳定作用起着重要的作用。人们对球型颗粒在非极性介质中的分散体系研究较多,而对于非等轴胶体颗粒的分散体系研究较少。有机土在非极性介质中的均匀分散是制备纳米复合材料和提高其性能的关键一步,另外研究有机土在非极性介质中的分散状态对于有机土在润滑油脂和油基钻井液中的应用具有指导意义。
有机土在非极性介质中的分散性较差,颗粒迅速沉降。向分散体系中加入非离子表面活性剂脱水山梨醇单油酸酯(Span80)、脱水山梨醇三油酸酯(Span85)和甘油单油酸酯以及阴离子表面活性剂2-乙基己基)磺化琥珀酸钠(AOT)都可以提高有机土分散体系的稳定性。通过紫外、元素分析、小角X-射线衍射等手段,我们发现表面活性剂在有机土表面发生吸附,增大有机土表面的疏水性；表面活性剂吸附在有机土颗粒表面,可以阻碍颗粒聚集,提供空间稳定作用；表面活性剂不仅吸附在有机土表面,而且能够进入有机土层间,进一步增大有机土的层间距,有利于有机土片层在分散介质中剥离,使有机土颗粒尺寸减小；通过测定有机土在非极性分散介质中的zeta电势,发现表面活性剂吸附在颗粒上可以增大颗粒的zeta电势,表面活性剂与有机土颗粒表面通过酸碱相互作用发生电荷转移,使有机土颗粒表面带电,增大了颗粒之间的静电斥力,从而有助于分散体系的稳定性的提高。表面活性剂通过空间稳定和静电稳定作用提高有机土／非极性介质分散体系的稳定性。
3.有机土稳定W／O乳液的研究
有机土在油基钻井液中一般是用作增粘剂,在W／O钻井液中,有机土可以吸附在油水界面,提高乳液的稳定性,增加体系的粘度。油基钻井液的水相通常含有较高浓度的盐,因而研究有机土稳定的W／O乳液以及盐对乳液稳定性的影响具有重要意义,本文考察了有机土的改性剂用量和水相中的盐浓度对有机土稳定的W／O乳液稳定性的影响。
固定体系的油水比和颗粒浓度,改变有机土改性剂用量可以改变有机土稳定的乳液类型。蒙脱土自身亲水性强,不能够形成稳定的乳液；用季铵盐对其进行有机改性,使颗粒表面疏水性增强,当改性剂用量低于0.8CEC时,由于颗粒表面亲水,形成水包油(O／W)乳液；当改性剂用量在0.8～1.2CEC时,颗粒表面的疏水性增强,形成W／O乳液。继续增大改性剂用量,改性剂通过烷基链段间的疏水作用在有机土上双层吸附,使颗粒表面重新亲水,但是却得到O／W乳液,这可能是由于有机土制备过程中的洗涤步骤去除了游离的表面活性剂,而在乳化过程中通过疏水作用吸附的改性剂从颗粒表面发生脱附,颗粒表面的亲水性不够强,因此乳液类型不再随改性剂浓度的进一步增加反转为O／W型。
一般来说,向颗粒水分散体系中加入盐,会屏蔽带电颗粒间的静电斥力同时还会使颗粒表面的亲水性降低,从而促使粘土水分散体系发生絮凝。当盐浓度较低时,颗粒水分散体系会发生弱絮凝,有利于形成稳定的乳液；当盐浓度较高时,颗粒水分散体系发生强絮凝,不利于形成稳定的乳液。本文首次研究了盐浓度对W／O乳液稳定性的影响。将有机土分散在液体石蜡中,改变水相中的盐浓度,发现随着水相中盐浓度的增大,W／O乳液的稳定性降低,当水相中盐浓度超过一定值时,不能形成稳定的乳液。在相同的盐浓度条件下,1.2CEC有机土制备的乳液的稳定性优于1.0CEC有机土,0.8CEC有机土制备的乳液的稳定性最差。通过测定有机土／盐水体系离心后上清液中有机物含量,发现随着盐浓度增大,改性剂在有机土上的脱附量增大。通过测定有机土和不同浓度盐水的接触角,发现随着盐浓度的增大,有机土颗粒表面亲水性增强。综上所述,随着盐浓度的增加有机土稳定的W／O乳液的稳定性降低,这是由于盐的加入促使吸附在有机土外表面的季铵盐发生脱附,导致有机土表面亲水性增强。
Montmorillonite finds wide range of applications for its special properties:natural abundance, fine size, easy modification. The applications of montmorillonite in nonaqueous media were limited for the strong hydrophilicity. However, cation-exchange reactions with organic cationic surfactants have been exploited to render the clay mineral hydrophobic at the surface and increase the basal spacing. Organic modification of montmorillonite (organoclay) has been widely used in industrial applications such as oil-field drilling fluids, paints, lubricating greases, wastewater treatment, and composite material. Thus the modifications of clay minerals have been widely studied fundamentally and in practical applications. One of the most important properties of organoclay is the ability for swelling and thixotropic gel formation in organic media. The advantages of organoclay as flow modifiers include:low volume fractions, good thermal stability, resistant to gel-breaking effects from other chemicals. Organoclay is generally used to control the rheologic property of hydrocarbon fluids.
Recently, the use of organoclay in materials science and technology has attracted considerable attention. Clay, having a large aspect ratio and size, has been recognized as potential candidates for filler materials, because it exhibits superior physical and mechanical properties when compared with the pure polymer. Organic modification of clay mineral, making it hydrophobic and compatible with polymers is necessary due to the hydrophilic nature of clay. The surface energy of clay and polymer could be reduced by organic modification. Additionally, the organic cations may contain various functional groups, which can react with the polymers and enhance the adhesion between clay particles and the matrix. Thus, it is possible to obtain nanocomposites with good dispersion quality.
Oil-based drilling fluid is the mud using oil as the continuous phase. The advantages of selecting an oil-based drilling fluid include:superior hole stability, enhanced shale inhibition, excellent lubrication, high temperature stability. For these benefits, oil-based drilling fluid is a better selection for drilling in deep well, high temperature well and complex conditions. For environment protection, miner oil of lower toxic was used to replace the crude oil or diesel which contains high content of aromatic hydrocarbons, but there is a problem that the organoclay could not disperse and gelling well in miner oil. In the water-in-oil (W/O) drilling fluid, orgaoclay can be adsorbed on the interface of oil and water, improving the stability of emulsion and the viscosity of drilling fluid.
In this context, we studied the dispersion of organoclay in octane in attempt to improve their stability. The rheological properties of organoclay suspensions were also investigated. The emulsion stabilized by organoclay was prepared, and the factors affecting their stability were evaluated.
The present dissertation includes three topics.
1. Preparation, characterization of organocaly and rheological properties of organoclay suspension
Cationic surfactant dimethyldioctadecylammoniurn chloride (DODMAC1) was used as the modifier to prepare organoclay, and the product was characterized by fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscope (SEM). The effects of reaction time, temperature, pH value and the amounts of organic modifier on the basal spacing and amounts of organic compounds of organoclay and the stability of organoclay suspension were investigated. The optimal reaction condition was carried at50-90℃for3h with1.0cation exchange capacity (CEC) cationic surfactant. If the amount of surfactant was increased, the thermal stability of the organoclay would decrease. When the addition of surfactant was more than1.4CEC, bilayer adsorption of surfactant would occur.
When organoclay is used as thickener in nonpolar miner oil such as white oil based drilling fluid, ideal result could not be achieved. Therefore we studied the rheological properties of organoclay/white oil suspension. The viscosity of the suspension increased with the dosage of DODMAC1first, and then decreased. The suspension containing organoclay of1.0CEC exhibited the maximum stability, viscosity and share thinning property. The rheological properties of silica nanoparticles suspended in a non-polar mineral oil were also investigated. The stability, viscosity and thixotropic property of silica nanoparticles are much better than organoclay.
2. Dispersion of organoclay in nonpolar media
Dispersions of particles in nonpolar media have many applications in ceramics, paints, lubricants and oil-based drilling fluid. Usually, dispersions of particles in nonpolar media are unstable, and dispersants are used to improve the stability of the dispersions. The mechanism of dispersant to improve the stability of dispersions is steric stabilization. Usually, electrostatic stabilization in nonpolar media was neglected because of the low dielectric constant. However, many recent studies have shown that electrostatic stabilization can play an important role. To improve the dispersion stability of organoclay in nonpolar media is important for improving the properties of polymer-clay nanocomposites, lubricants and oil-based drilling fluids. Thus we investigated the stabilization mechanism of organoclay in octane.
The dispersion of organoclay can be improved by the addition of the nonionic surfactants sorbitan monoleate (Span80), sorbitan trioleate (Span85) and1-oleoyl-rac-glycerol and anion surfactant sodium bis(2-ethylhexyl) sulfosuccinate (AOT). The relation between the adsorption of surfactants on organoclay particles and the stability of the dispersions was investigated. The effects of the surfactants on the basal spacing of particles, electrostatic interactions between particles and rheological properties of dispersions were also measured. Based on the decrease of the particle size and the increase of the zeta potential, the improvement of the dispersion stability could be interpreted by steric and electrostatic stabilization. This work sheds some light on the selection of dispersants for improving the dispersion stability of particles in nonpolar media.
3. Pickering emulsion stabilized by organoclay
Organoclay typically is used to control the rheology in oil-based drilling fluid. In drilling fluid, the organoclay could also adsorb at the surface of water droplets to stabilize the W/O emulsions and improve the viscosity of mud. The aqueous phase of mud is usually comprised of high concentration of salt, to minimize water exchange between drilling fluid and the formation being drilled. Because the wettability of organoclay and salt concentration in the aqueous phase could affect the stability of the emulsion, we investigated the effects of modifier dosage of organoclay and salt concentration in the aqueous phase on the stability of W/O emulsions stabilized by organoclay.
Emulsion inversion could be induced by increasing the addition of cationic surfactant modifier, as the wettability of organoclay was changed from hydrophilicity to hydrophobicity. When the amount of surfactant was less than0.8CEC, the emulsions stabilized by organoclay were O/W. When the amount of surfactant was more than0.8CEC, W/O emulsions were prepared by the hydrophobic organoclay. If the addition of surfactant was increased further, O/W emulsions were not obtained. This may be due to the removal the free surfactant in the washing process in the preparation of organoclay and the reduction of organoclay hydrophobicity by desorption of the adsorbed bilayer surfactant in emulsification process.
The addition of salt could increase the hydrophobicity of particles and decrease particle zeta potential leading particle adsorption at the oil-water interface. Salts could also flocculate the particles to form visco-elastic three-dimensional network, which enhance the creaming stability of emulsion. Here, the effect of salt concentration on the W/O emulsions stabilized by organoclay was studied. The stability of emulsions decreased with the salt concentration, and stable emulsion could not be prepared when the salt concentration was above a certain value. The emulsion prepared with organoclay of1.2CEC was more stable than organoclay of1.0CEC and0.8CEC. The desorption of cationic surfactant from organoclay was measured by Total Organic Carbon Analyzer. The amount of surfactant desorbed increased with salt concentration. The desorption of cationic surfactant modifier would increase the hydrophilicity of organoclay, which is not conductive for the formation of W/O emulsion. The reasons of the decrease of the emulsion stability caused by the addition of salt were the reduction of organoclay hydrophobicity and the desorption of cationic surfactant at high salt concentration.
引文
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