液液聚结分离器原理及石油化工中的应用

对非均相液-液两相的聚结分离机理,以纤维类介质为例,将聚结过程分为液滴捕集、液滴聚结和液滴沉降,同时也对影响聚结分离的因素进行了阐述.在此基础之上,介绍了目前在石油化工行业中应用比较广泛的高效的液-液两相分离设备:单级聚结器和二级聚结分离器,重点论述滤芯式聚结分离设备.为在石油化工领域中液-液分离提供指导和借鉴作用,为实现经济、有效的分离操作提供理论和实践支持.最后指出液-液两相聚结分离技术及设备的发展方向.     

液—液两相聚结分离原理及实际应用

对非均相液—液两相的聚结分离机理进行了阐述,以纤维类聚结介质为例,将聚结过程分为液滴捕集、液滴聚结和液滴沉降三个阶段。在聚结原理基础之上,对液—液聚结分离用的聚结材料进行分类,在此基础之上,详细介绍了目前应用比较广泛的液—液两相分离设备。最后指出液—液两相聚结分离技术及设备的发展方向。     

新型液-液分离设备——斜板沉降器

介绍了斜板沉降器的结构和操作特性，并对液滴在斜板层膜上的聚结过程以及影响液滴聚结的因素进行了分析；提出了液滴在斜板上有效聚结作为斜板沉降器的设计依据，最后对斜板沉降器的进一步研究重点提出了建议。     

对置液柱撞击液膜破裂特征

采用高速摄像仪对两液柱撞击产生液膜的破裂过程进行了实验研究。分析了撞击液膜的破裂过程及表面波产生和传播过程,考察了射流直径、喷嘴间距和射流Weber数（We）对撞击液膜破裂的影响;定量分析了液膜表面波频率的变化及液膜破裂后的粒径分布情况。研究结果表明,液膜表面波传播频率随We的增大而增大,并沿液膜径向方向逐渐减小;随着射流We的增加,液膜边缘的液滴脱落频率增加;当We>1000时,液膜表面产生大量液滴团,且液滴团对液膜破裂具有促进作用;液柱撞击液膜发生破裂后90%以上的量纲1液滴粒径分布在0～1之间。     

液液雾化特性与粒径分布规律

液液雾化过程是液液循环流化床的关键技术之一，在流化床常态实验装置上，采用快速摄像与图像处理相结合的方法，获得了实验流量范围内液滴形成过程的图像以及形成液滴的粒径信息，运用数学分布函数对液滴的粒径分布进行了研究。研究结果表明，各流量工况下，液滴的粒径分布与Rosin-Rammler分布符合得较好;在实验流量范围内，形成液滴的区域有单液滴形成区域、过渡区域和多液滴形成区域，且液滴中位径的总体趋势是减小的，当水的流量为50 ml·min-1时，形成液滴的粒径主要集中在0.7～1.0 mm之间;在单液滴形成区域和多液滴形成区域，液滴粒径的均匀性先减小后增大，中位径呈减小趋势，但在多液滴形成区域两者的变化幅度较小，在过渡区域，液滴粒径的均匀性与中位径基本不变。研究结果可为液液循环流化床基于设计粒径的要求合理选取运行流量提供可靠依据。     

液滴行为与液-液混合设备

总结了液-液非均相混合过程中的液滴运动速率计算模型,分析了液滴破碎及合并的机理。在结合各种工业应用的基础上,总结了搅拌釜、射流混合器、静态混合器、撞击流混合器及纤维液膜混合器等五种混合设备的混合原理及研究现状。展望了液-液混合设备的研究前景。     

小液滴在水平液液界面上的聚并

对纯净系统中的小液滴在水平液液界面上聚并时的薄液膜排液过程进行了理论分析，研究两相物理性质、范德华力、界面切向运动对聚并速率的影响，得到了计算聚并时间的公式．理论预测与实验结果符合良好．     

液-液两相高效分离技术及应用

在对非均相液-液两相的分离的重要性进行阐述基础之上,分析了影响液-液两相分离的因素,主要包括液-液两相的物性、聚结材料的选择等方面。此外详细地介绍了目前普遍使用的液-液两相高效的分离措施及设备,重点介绍了目前普遍使用的三种高效的设备：单级聚结器、两级聚结分离器以及三级过滤-聚结-分离器。为实际应用中非均相液-液两相实现最经济、有效的分离提供指导作用。     

气-液-液萃取传质效率的研究

在液-液萃取过程中,提高分散相的表面更新速率可有效提高萃取的传质效率.研究发现,在萃取过程中使用气体搅拌可以增加液液之间的接触面积,促进液相内的湍动和循环.据此,本文在气-液-液萃取条件下对不同填料的传质性能进行了测定.实验表明,通入气相后分散相液滴呈现稳定的“油包气”空心状态,这种结构大大降低了分散相液滴的传质层厚度,减小了传质距离,极大地强化传质效率.在适宜气速下,气-液-液萃取效率较传统萃取效率提高20％～40％.通过与散装填料对比,发现规整填料更利于强化萃取效果,传质效率提高约50％.     

液—液分散雾化形成液滴的模式

基于图像采集与处理方法实验研究了水喷入非相溶油中的液液分散雾化过程.结果表明,通过改变操作条件使水破碎形成3种水滴模式:滴流、层流射流和湍流射流,揭示了其演变规律及其形成机理,获得了分散液体破碎强度、射流长度脉动和液滴粒径分布参数随雷诺数Re、韦伯数We的变化规律.随Re和We增加,分散液体破碎强度持续增强,在Re=467,We=8.6时液滴形成模式由滴流向层流射流发展,在Re=3169,We=241时演变为湍流射流,且液滴的粒径均匀性和最小平均粒径均出现在湍流射流模式下;在滴流模式下,液滴的形成、长大与脱离喷嘴均由液滴受力的平衡机制控制;在层流射流模式下,射流柱破碎形成液滴主要由两相界面的表面波扰动引起,且射流长度的脉动具有随机和非周期的特点;在湍流射流模式下,射流柱表面出现拟序涡结构,其在射流起始段失稳,在射流扩散段大量形成较小粒径的液滴.     

Coalescence behaviour of water droplets in water‐oil interface under pulsatile electric fields

In this research, the deformation of water droplets in sunflower oil-interface under pulsatile electric field was studied experimentally. Three types of coalescence were observed:(i) complete coalescence, (ii) incomplete coalescence and (iii) no-coalescence. The first type is desirable because of leaving no secondary droplets. The second type that produced secondary droplets which caused by necking process, due to extreme elongation of droplets (mostly small droplets), was undesirable; because the small droplets were more difficult to coalesce and remove. The no-coalescence was caused by very fast coalescence and extensive pushing of droplet into the continuous phase. In this work the process was operated with the utilization of a batch cylindrical separator with high voltage system. The lower part of the cylinder was filled with the aqueous phase and its top part was filled with sunflower oil to form an interface between the two phases. The effects of electric field strength, frequency, and waveform types were investigated. It was found that, the ramp-ac waveform was the best waveform, avoiding the production of secondary droplets and in this case the frequency also played an important role.     

Neue proteinstabilisierte O/W-Emulsionen

New Protein Stabilized O/W-Emulsions The formation and stabilization of o/w-emulsions were investigated with faba bean globulin isolate and the corresponding acetylated derivative as model substances in dependence on concentration at constant pH-value and on pH-value at constant concentration as well. A centrifugal equilibrium method was developed and the protein distribution in the phases after centrifugation was determined. Optimal conditions (concentration, pH-value and preparation of emulsion) lead to a coating of the oil droplets with protein being stable against coalescence. It is possible to separate those coating droplets in a form of stabile concentrate of emulsion. The acetylated derivative is a more efficient emulsifier and stabilizer than the unmodified faba bean globulin is. For oil droplet size distribution and comparable stability less protein is needed in the case of acetylated derivative. At the same time a stronger interaction between the aqueous phase of the emulsion and the coated oil droplets was found. This is reflected by the existence of a mechanical barrier against the separation of this aqueous phase. The results fo the coalescence stable concentrates of emulsion are the reason to search for a new principle producing o/w-emulsions.     

De-emulsification of 2-ethyl-1-hexanol/water emulsion using oil-wet narrow channel combined with low-speed rotation

Low-speed rotation of disc in an internal circulation of a novel de-emulsification with rotation-dise horizental contactor (RHC-D) realized de-emulsification for O/W emulsions due to repeated coalescence in oil-wet narrow channels at a low rotation speed. For three emulsions included ethanol/water/2-ethyl-1-hexanol, ethanol/water/2-ethyl-1-hexanol/SDS (Sodium Dodecyl Sulfonate) and 2-ethyl-1-hexanol/water/SDS emulsion, deemulsification ratios of oil phase could reach 1, 1 and 0.67 respectively at 170 r·min^-1, and de-emulsification ratios increased obviously after agitating 10 min. De-emulsification experiment in the seam indicated that oil droplet sizes in O/W emulsion became larger after de-emulsification. The main de-emulsification mechanism in RHCD was the coalescence of oil droplets in oil-wet narrow channels. With increase of the rotation speed, oil droplets dispersed better in the aqueous phase. However, de-emulsification effect enhanced due to the increase of the coalescence rate at a bit higher rotation speed. In addition, internal circulation made those O/W emulsions to be broken repeatedly, consequently de-emulsification ratio increased. Repeated de-emulsification through internal circulation might make continuous extraction of ethanol come true at a low rotation speed.     

Influence of soybean protein isolates-phosphatidycholine interaction on the stability on oil-in-water emulsions

Soybean protein isolates and phospholipids present specific surface properties with synergistic or antagonistic effects on emulsion stability. Oil-in-water emulsions (25∶75 w/w) were prepared using native and denatured soybean isolates (NSI and DSI, respectively) with the addition of phosphatidylcholine (PC) (protein/PC ratio 100∶1 to 10∶1). The effect of ionic strength was also studied by adding sodium chloride (0–100 mM) to the aqueous phase. Analysis of NSI/PC and DSI/PC emulsions showed that the creaming rate diminished upon addition of PC, with the creamed phase showing more stability than those of the control systems. In DSI/PC systems, the coalescence process was partially controlled, as evidenced by a decrease in the size of oil droplets. Both systems were altered by the presence of sodium chloride, with an increase in the creaming rate attributable to flocculation and the coalescence of droplets. Under these conditions, DSI/PC emulsions exhibited a stronger protein-phospholipid interaction than those of NSI/PC.     

Utilizing cellulose ethers as suspension agents in the polymerization of vinyl chloride

Proper choice of a suspending agent will help the PVC manufacturer achieve control of resin particle size, particle size distribution, and resin bead porosity. The results of research work at Dow has revealed that certain properties of cellulsoe ethers (a hydroxypropyl methylcellulose ether structure) are useful in helping control the properties of the PVC resin. In vinyl chloride polymerizations, cellulose ethers act as both an emulsifier; and during the polymerization, as a protective colloid to prevent excessive coalescence of the monomer droplets. The average particle size of the organic droplets in the aqueous phase during the PVC polymerization reaction is a function of the interfacial tension, intensity of agitation, viscosity of the two phases, and the volume fraction of the dispersed phase. The average particle size of the PVC resin was found to be a direct function of the interfacial tension multiplied by the 0.2 power of the gel strength of the cellulose ether solution. The interfacial tension of the cellulose ether solution/organic interface is probably the most important factor in determining the resin particle size. Particle size distribution widens with an increase in interfacial tension. Resin bead porosity is also important and is directly related to the solubility of the cellulose ethers in the organic phase. This observation supports the proposed seed stabilization theory that can explain the formation of a porous resin bead. The use of a proper suspension agent like cellulose ethers with or without a secondary surfactant will help control important properties of the PVC resin product. Control of the average molecular wight, degree of substitution, and grouping distribution on the cellulose chain of the cellulose ether suspension agent (all of which affect interfacial tension) is important for the PVC manufacturer.     

Drop coalescence processes in suspension polymerization of vinyl chloride

A tracer dye technique was used to investigate the effect of turbulence intensity, stirring time, and the type and concentration of the suspending agent, partially hydrolyzed poly(vinyl acetate) (PVA), on the coalescence rate of vinyl chloride monomer (VCM) droplets in an agitated liquid–liquid dispersion. It was found that the extent of coalescence rises slowly with mixing time, is roughly proportional to the agitation speed, and decreases sharply when the concentration of stabilizer is increased. Coalescence rate depended on the degree of hydrolysis of the stabilizer. The method of addition of initiator during VC suspension polymerization was also studied and its effects on the polymerization conversion and final PVC particles' properties were determined. It was found that the polymerization reaction occurs more uniformly in all the VCM droplets when the initiator was predissolved in the VCM prior to reaction compared with the case when the initiator was predispersed in the continuous water phase. Also, for the same reaction time, the conversion was higher in the former case. During polymerization, the concentration of PVA in the aqueous phase decreased substantially and the porosity of the polymer particles was reduced. © 1996 John Wiley & Sons, Inc.     

Influence of the plate-type continuous micro-separator dimensions on the efficiency of demulsification of oil-in-water emulsion

The objective of this article is to find the optimal dimensions of rectangular plate-type micro-separators in order to enhance the continuous separation of immiscible liquids. The main structure of the separators contains two plates: a hydrophobic (PTFE) upper plate and a hydrophilic (stainless steel) bottom plate which formed the contact surfaces for the fluids in the channel. The devices have two outlets, one for the aqueous phase and the other for the organic phase enabling the continuous separation and withdrawal of the separated phases. Demulsification has been carried out using Shellsol/water emulsion in the presence of a non-ionic surfactant (Tween 80). The separation efficiency is investigated as a function of micro-separator sizes, channel depths, flow rates and plate configurations. The major parameter that controls the destabilization mechanism is the ratio between the droplet size and the channel depth. When the size of the dispersed droplets remains smaller than the height of the separator (channel depths: 25–100 μm), creaming is the main demulsification mechanism. Creaming refers to the migration of the dispersed phase of an emulsion, under the influence of buoyancy. The particles float upwards and rise to the top due to the difference in the densities of the particles and the medium. The separation efficiency depends mainly on the residence time of the liquid/liquid mixture in the device regardless of the separator dimensions and channel heights. The separation rate is limited by the removal of the cream layer, formed at the top of the upper plate, from the separator. When the size of the dispersed droplets is larger than the depth of the separator (channel height of 9 μm), the separation performance and mechanism become different. The coalescence of the dispersed droplets occurs by passing through the device. The comparison of the data corresponding to creaming and coalescence phenomena emphasizes that the coalescence greatly enhance and accelerate the separation action. The phase separation in the micro-coalescer takes place considerably faster than in the micro-separators.     

Influence of process conditions on the mean size of PLGA nanoparticles

Investigation was carried out to determine the influence of process conditions on the volume mean size of PLGA nanoparticles intended as drug delivery vehicle for an injection formula of protein type therapeutic agent. Nanoparticles were produced by double emulsion-solvent evaporation method to encapsulate bovine serum albumin into the PLGA matrix material. At first aqueous BSA solution was dispersed by sonication into an organic phase composed of dichloromethane as solvent and dissolved PLGA. This first emulsion was dispersed in a second aqueous phase containing PVA emulsifier. Solid nanoparticles were obtained by evaporating the dichloromethane from the droplets. Size distribution of particles was determined by dynamic light scattering. It was found that volume mean particle size was influenced by several process variables, such as PVA concentration in the external phase, PLGA concentration in the organic phase, BSA concentration in the inner phase, volume ratio of the external and intermediate phases, and the time of sonication during the second emulsification. To elucidate their effects a 5-factorial 3-level experimental design and statistical analysis were carried out. Relationship between the mean particle size and process parameters was proposed.     

Mechanism of suspension polymerization of uniform monomer droplets prepared by glass membrane (Shirasu Porous Glass) emulsification technique

The mechanism of the unique suspension polymerization of uniform monomer droplets, without coalescence and breakup during the polymerization, was investigated using styrene (S) as a monomer mixed with water‐insoluble hexadecane (HD). The glass membrane (Shirasu Porous Glass, SPG) emulsification technique was employed for the preparation of uniform droplets. Depending on the pore sizes of the SPG membranes (1.0, 1.4, and 2.9 μm), polymer particles of an average diameter ranging from 5.6 to 20.9 μm were obtained with the coefficient of variation (CV) being close to 10%. The role of HD was to prevent the degradation of the droplets by the molecular diffusion process. Sodium nitrite was added in the aqueous phase to kill the radicals desorbed from the droplets (polymer particles), thereby suppressing the secondary nucleation of smaller particles. Each droplet behaved as an isolated locus of polymerization. With the presence of HD, the initial polymerization rate was proportional to 0.24th power of the benzoil peroxide (BPO) concentration. This peculiar behavior as compared with the ordinary suspension polymerization was explained by introducing the assumption that each droplet was composed of isolated compartments (cells) in which active polymeric radicals were dissolved in an S‐rich phase and surrounded by a rather incompatible S/HD (continuous) phase. The average number of radicals in the droplet increased initially due to the separate existence of polymeric radicals in compartments. As the polymerization progressed, the HD‐rich phase gradually separated, eventually forming macrodomains, which were visible by an optical microscope. The phase separation allowed polystyrene chains to dissolve in a more favorable S phase, and the homogeneous bulk polymerization kinetics took over, resulting in a gradual decrease of the average number of radicals in the droplet until the increase of viscosity induced the gel effect. When no HD was present in the droplets, the polymerization proceeded in accordance with the bulk mechanism except for the initial retardation by the entry of inhibiting radicals generated from sodium nitrite in the aqueous phase. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 1025–1043, 2000     

Synthesis of Lithium-Cobalt Oxide Nanoparticles by Flame Spray Pyrolysis

Crystalline LiCoO2nanoparticles were synthesized from an aqueous solution of acetate compounds of lithium and cobalt by a flame spray pyrolysis, and characterized by TEM, XRD, and BET method. We investigated the evolution of LiCoO2nanoparticles from liquid droplets sprayed along the flame and observed disintegration of aqueous precursor droplets about 10μm into smaller fragments around 50 nm in the high temperature flame, as well as decomposition/oxidation of the precursor and coalescence/coagulation. We also examined effects of process variables such as molar concentrations of the precursors and flow rates of combustible gases on the particle size and crystal structure. The average particle diameter increased with an increase in the molar concentration of the precursor. Raising the maximum flame temperature by controlling the gas flow rates also led to an increase in the average diameter of the particles. The crystalline nanoparticles synthesized were nearly spherical, and their average primary particle diameters ranged from 11 to 35 nm.