The modified outflow funnel — A device to assess the flow characteristics of powders

Flow regulators are added to solid pharmaceutical formulations to improve the flow properties of powder mixtures. During the blending process the glidants adsorb successively at the surface of the host particles and thus lead to a reduction of attractive forces. A large variety of flow additives based on silicon dioxide is commercially available, but not all glidants are just as well suited for each technological problem or each cohesive bulk powder. To assess the improvement of the flowability parameters caused by a glidant a classification system and an adequate measuring device is needed. We would like to present a new measuring device to evaluate the flow enhancing potency of glidants. The modified outflow funnel features a stirrer that acts in the region of bulk arches obstructing the outflow process of a cohesive powder. By destruction of the bulk arches powder outflow is enabled and the time needed for emanation can be measured as a parameter of the flow properties. In addition other measuring parameters like the force needed to destroy the bulk arches are capable to evaluate the flowability of the powder mixture. Binary powder mixtures consisting of corn starch and flow regulator were blended in a Turbula® mixer for a defined period of time. The flow regulators were represented by fumed silica and a selection of various types of SIPERNAT^® precipitated silica provided by Evonik Degussa GmbH, Hanau, Germany. Flowability parameters of the mixtures were characterized with a modified outflow funnel, Hausner Ratio and a shear tester.     

Powder flowability and density ratios: the impact of granules packing

The propensity of powders to flow under given circumstances (flowability) affects a large number of industrial applications. A single, reliable and widely applicable flowability test does not exist, because of the variety of both granular materials and influence of handling on the measurements results. Here we critically examined the results provided by Hausner's method, based on apparent densities ratio, with several granular materials. Major limitations appeared to be the achievement and measurement of a dense packing condition, provided by the tapped density in the Hausner's ratio. After a detailed discussion of standard and modified techniques to measure bulk density, we eventually suggest a new flowability criterion based on a novel technique to determine a high packing density. The proposed criterion is more sensitive to differences in flowability, as quantified by the repose angle. In order to investigate also the domain of cohesive powders, we developed a novel procedure to measure the repose angle of such powders. Eventually, the new criterion was able to account consistently for free-flowing and cohesive powders. It also stimulates the discussion on subtle issues involved in the determination and use of elementary powder's properties.     

煤粉的流动性测试及评价方法研究

采用休止角法、HR（Hausner Ratio）法、Carr流动性指数法、Jenike法和质量流率法等方法实验研究了不同粒径的羊肠湾煤粉、北宿煤粉和田坝煤粉的流动性,对五种方法进行了比较与分析。结果表明：煤粉粒径越小,流动性越差,当粒径小于约75 μm时,改变煤粉粒径对流动性改善效果显著;相似粒径下三种煤粉流动性存在差异,北宿煤粉流动性最差;各种方法对煤粉流动性趋势关系的描述具有良好的一致性;在40kPa的预压缩应力,煤粉流动指数值ffc超出了传统的ffc与流动性关系范围。     

高含量β-胡萝卜素微胶囊干粉流动性的考察及其影响因素

The flowability of five kinds of microencapsulation powders,with differentβ-carotene contents and by two alternative particle-forming technologies i.e.spray-drying and starch-catching beadlet technology,was meas- ured.The actual flow properties of the five powders were compared based on bin-flow test,and three flow indexes (Hausner ratio,repose angle and flow index)were measured.It was found that the repose angle is the most suitable index to reflect the flowability of these powders for the particle properties would not be altered due to compaction or tapping during the measuring process.Particle size and particle size distribution play most important roles in the flowability of these granular materials,which was also influenced by other factors like shape,surface texture,sur- face roughness,etc.Microcapsules with wall material of gelatin and a layer of modified starch absorbed on the sur- face showed excellent flowabilities and good mechanical properties,and they are favorable for tabletting to supply β-carotene.     

Modification of interparticle forces for nanoparticles using atomic layer deposition

Silica and titania nanoparticles were individually coated with ultrathin alumina films using atomic layer deposition (ALD) in a fluidized bed reactor. The effect of the coating on interparticle forces was studied. Coated particles showed increased interactions which impacted their flowability. This behavior was attributed to modifications of the Hamaker coefficient and the size of nanoparticles. Stronger interparticle forces translated into a larger mean aggregate size during fluidization, which increased the minimum fluidization velocity. A lower bed expansion was observed for coated particles due to enhanced interparticle forces that increased the cohesive strength of the bed. Increased cohesiveness of coated powders was also determined through angle of repose and Hausner index measurements. The dispersability of nanopowders was studied through sedimentation and z-potential analysis. The optimum dispersion conditions and isoelectric point of nanoparticle suspensions changed due to the surface modification. A novel atomic force microscope (AFM) technique was used to directly measure interactions between nanoparticles dispersed on a flat substrate and the tip of an AFM cantilever. Both Van der Waals and electrostatic interactions were detected during these measurements. Long and short range interactions were modified by the surface coating.     

Flowability of moist pharmaceutical powders

The effect of moisture content on four pharmaceutical powders (an active pharmaceutical ingredient (API), Aspartame, Hydroxypropyl Methylcellulose (HPMC), and Respitose ML001) has been investigated. The API and Respitose powders were found to be nonhygroscopic and were tested at their native moisture contents only. The Aspartame was tested at moisture contents of 0%, 2%, 5%, and 8% and the HPMC was also tested at moisture contents of 0%, 2%, 5%, and 10%. Powder flowability was measured using the Jenike shear index, the Hausner Ratio, the Carr Index, and the static and dynamic angles of repose. The flowability of Aspartame increased with an increase in moisture content, which is attributed to the formation of large, round agglomerates. The flowability of HPMC decreased with an increase in moisture content, attributed to the increasing strength of liquid bridges. The Jenike shear index was the only flowability indicator to capture this complex behaviour.     

Influence of a lipid phase on steam jet agglomeration of maltodextrin powders

The contribution of an oil phase to the agglomeration mechanisms of food powders was evaluated. Maltodextrin (DE 10), palm oil stearin and two palm oil oleins (up to 25% dry mass) were used as food models. Granulation runs were carried out in a pilot plant steam jet agglomerator. The powders containing oleins were more cohesive than those with stearin and the presence of oil changed the agglomeration mechanisms. The size increase mechanism of pure maltodextrin powder was controlled by surface plasticization and agglomerates with suitable instant properties were obtained. Small amount of oil degenerated drastically the rate of dispersion in water of the powders and their agglomerates but the average size and the mechanical resistance of the agglomerates increased when the oil content of the powders increased. SEM micrographs of agglomerates indicated that higher lipid content in the powders produced compact granules, favoring sinkability but hindering their disintegration. Agglomeration enhanced considerably the flowability of the particles containing oil. The dispersion behavior of the powders with higher lipid content could be correlated with the Hausner Number. A pre-agglomeration step favored the blend of the more cohesive powders producing larger and more resistant agglomerates.     

Measuring the flow properties of small powder samples using an avalanche tester

The feasibility of using a small-scale avalanche tester to measure the flow properties of pharmaceutical lactose powders was examined. The modes of behavior observed in larger systems were displayed and showed a clear distinction between angular, free-flowing particles and more spherical particles of similar flow characteristics. Angular Lactohale LH100 particles showed slumping behavior at a rotational frequency of 0.33 Hz that disappeared at higher frequencies. Spherical lactose powder with a similar flow function to LH100 only showed rolling behavior under the same conditions, as did more cohesive powders LH200 and LH300. Further investigation of the LH100 data using fast Fourier analysis showed that the slumping frequency was one tenth of the rotational frequency.     

细粉下料过程的气固流体动力学作用分析

细颗粒粉体下料时受气固流体力学作用在料仓出口附近形成逆压力梯度,使得粉体下料流率实验值远低于理论预测值。而且该压力梯度力直接测量较困难,对模型修正和发展提出了挑战。以玻璃微珠、流化催化裂化（FCC）催化剂颗粒、褐煤和聚氯乙烯（PVC）颗粒为实验材料,首先开展粉体静力学与动力学测试,借助休止角（AOR）、豪斯纳比（HR）和卡尔流动指数（CFI）多个粉体流动性判据综合分析不同粉体的流动特性;在分析粉体料仓出口附近气固流动特征的基础上,结合Jenike流动与不流动判据,将作用在细颗粒粉体上的逆压力梯度力引入到拱应力平衡方程;进一步,提出了利用迭代算法获得逆压力梯度力的方法,实现了对逆压力梯度力与粉体料仓下料流率的预测。建立的粉体下料流率模型考虑了气固流体动力学作用对粉体下料流动的影响,有效改善了传统模型对细粉体流率预测偏高的问题,模型预测偏差从60%以上降低至±20%。     

The effect of surface modification of aluminum powder on its flowability, combustion and reactivity

Surface modification of aluminum powders for the purpose of flow improvement was performed and several samples were prepared. Correlations between the flowability and reactivity for these powders as well as for the initial untreated aluminum powder were established. The powders were characterized using Scanning Electron Microscope (SEM), particle size distribution, angle of repose flowability test, Constant Volume Explosion (CVE) combustion test, and Thermo-Gravimetric Analysis (TGA). The surface modification of micron-sized aluminum powders was done by: (1) dry coating nano-particles of silica, titania and carbon black onto the surface of spherical aluminum powders and (2) chemically and physically altering the surface properties of the same powders with methyltrichlorosilane. All surface modifications improved flowability of the powders. CVE measurements indicate that powders with an improved flowability exhibit improved combustion characteristics if the powder treatment does not add an inert component to aluminum. The TGA results do not show significant differences in the reactivity of various powders. Based on combined flowability and CVE characteristics, the silane modified material gave the best results followed by the powders dry coated with carbon, titania and silica, respectively.     

水泥粉体流动行为及其与不同材质库壁粘附性研究

水泥粉体流动性与其储存、输送、给料、混合等操作密切相关。通过休止角、内摩擦角、粘聚力和无侧限抗压强度测试方法,研究了含水率对水泥粉体流动性的影响,对比了水泥粉体与砂浆、钢、涂料、防腐卷材四种壁面材料的壁摩擦角和附着力。结果表明:随着水泥粉体含水率增加,休止角、粘聚力和无侧限抗压强度增加,水泥粉体流动性变差。松散堆积水泥粉体随着放置时间增加,由于水泥水化引起颗粒尺寸增加造成流动性变好。固结应力增加,无侧限抗压强度明显增大,导致水泥粉体流动性变差。水泥粉体在不同壁面材料的粘聚力均随着含水率的增加而增大,在水泥库内表面涂覆涂料和防腐卷材均可以起到降低水泥粉体与壁面的摩擦力和附着力的作用。     

Hot melt granulation of coarse pharmaceutical powders in a spouted bed

The hot melt granulation of a coarse pharmaceutical powder in a top spray spouted bed is described. The substrate was lactose-polyvinylpyrrolidone particles containing or not acetaminophen as a drug model. Polyethylene glycol (MW, 4000) used as binder was atomized onto the bed by a two-fluid spray nozzle. The granulation experiments followed a 2³ factorial design with triplicates at the center point and were carried out by varying the spray nozzle vertical position, the atomizing air flow rate and the binder feed rate. Granules were evaluated by their pharmacotechnical properties like size distribution, bulk and tapped densities, Carr index, Hausner ratio and tableting characteristics. Analysis of variance showed that granule sizes were affected by the PEG feed rate and atomizing air pressure at the significance levels of 1.0 and 5.0%, respectively, but spray nozzle distance to the substrate bed was not significant. The spray conditions also affected granule flow and consolidation properties, measured by the Carr index and Hausner ratio. Measured densities, Carr indexes and Hausner ratios proved that granules flowability and consolidation properties are adequate for pharmaceutical processing and tableting. Tablets prepared with acetaminophen-containing granules showed good properties and adequate release profiles in in vitro dissolution tests. The results indicate the suitability of spouted beds for the hot melt granulation of pharmaceutical coarse powders.     

Physicochemical Characterization of Whole Egg Powder Microencapsulated by Spray Drying

Physical characterization and oxidative stability of egg powder microencapsulated by spray drying were studied in this work. The wall material (gelatin, lactose, pullulan, and their mixtures) and liquid egg mixtures were prepared by homogenization at 22,000 rpm for 60 s. The spray drying was carried out at pilot-scale spray dryer (Niro Mobile Minor, Søborg, Denmark). The spray-dried egg powders were analyzed for moisture content, water activity, peroxide value, total cholesterol oxidation products (TCOPs), particle properties, and bulk properties. Using gelatin as wall material resulted in a significant increase in the moisture content and water activity of egg powder during storage and it improved flowability. Egg powders containing pullulan as wall material showed a fibrous structure and had the lowest bulk density. Adding lactose as wall material increased the oxidative stability, which was indicated with lowest peroxide value and TCOPs level of egg powder.     

Aerosolisation behaviour of micronised and supercritically-processed powders

Comparative analysis of salmeterol xinafoate (SX) powders was carried out to define the aerodynamic properties and mechanism of particle dispersion relevant to the use of these materials in dry powder inhalation drug delivery. Particle sizing methodology was evaluated using laser diffraction, time-of-flight and Andersen cascade impactor measurements combined with electron microscopy and surface area determination. Particle interactions, assessed on the basis of powder bulk density and inverse gas chromatography surface energy measurements, were compared with the aerodynamic forces generated by a dry-powder dispersion device. The supercritically produced material showed by a factor of seven reduced tensile strength of the aggregates and indicated a two-fold increase of fine particle fraction deposited in a cascade impactor when blended with lactose. This effect was explained by the reduced particle aggregation at low differential air pressures and flow rates. A relatively small value of aerodynamic stress required to disperse supercritically produced particles in comparison to micronized material comes from: (a) lower bulk density (loose aggregate structure), (b) larger volume mean diameter, (c) larger aerodynamic shape factor and (d) smaller specific free energy of S-SX particles, in this order of priority. It is shown that aggregation between primary drug particles is important for SX/lactose formulations because such aggregates survive the pre-separation impactor stage.     

Synthesis of nanograined zirconium diboride microsphere powder feedstock via emulsification of suspensions

Ceramic nanograined materials have desirable characteristics compared to their macroparticle counterparts but are rarely used in industrial applications due to issues with poor handleability and health hazards. Due to interparticle forces that become more dominant as the particle size decreases, it is difficult to use nanomaterials to fill dies, spread on surfaces, or flow through hoppers found in various manufacturing processes. Here we report a scalable gelcasting solution and unique emulsification process to create microspheres composed of nanoscale powders to enhance the flowability and handleability of nanomaterials. The gelcasting solution and emulsification process can be used with any nanoparticle composition that can be suspended in a liquid phase. This paper reports the effects of various parameters on zirconium diboride microsphere formation, such as surfactant content and mixing conditions. The microspheres maintain the nano-scale characteristics of the powder but improve its flowability by using cross-linked polyvinyl alcohol to combine irregularly shaped zirconium diboride nanoparticles with a particle diameter of 60 nm into larger spherical particles with a d₅₀～25 μm. This hierarchical feedstock engineering design combine the positive characteristics of materials across both length scales and improve the flowability of the feedstock from a Hausner Ratio of 1.56 to 1.19. The materials produced using this technique can be used in thermal plasma spray, die filling for hot pressing or spark plasma sintering, and binder jet printing applications.     

Physical and flow properties of pecan shells—Particle size and moisture effects

Pecan shells are the byproduct of the processing of pecans for human consumption. The potential use of these shells for bioenergy and other value-added applications requires information on the physical and flow properties. These properties are needed for the design of storage, processing and handling equipment. The effects of particle size and moisture content on bulk density, particle density, tap density, compressibility, angle of repose, cohesion, angle of internal friction and flowability were quantified in this study. Equilibrium moisture relations for the shells were also determined at temperatures ranging from 10 to 50 °C. The densities (bulk, particle and tap) significantly decreased and compressibility significantly increased with increases in particle size and moisture content. Increasing the moisture content reduced its flowability from free flowing (flow index of 15.77) at a moisture content of 4.2% (w.b.) to cohesive (flow index 3.14) at a moisture content of 24.6% (w.b.). The cohesive strength of pecan shells also increased with particle size (0.58 to 1.14 kPa) and with moisture content (0.36 to 1.69 kPa). An average angle of internal friction of 41.28° was obtained and was not significantly affected by moisture content and particle size. The angles of repose of pecan shells varied from 33.1 degrees to 46.3 degrees. The equilibrium moisture relation curves for the shells were sigmoidal in shape and showed that pecan shells should be stored at moisture contents of less than 18.03% (w.b.) to minimize microbial activity. The equilibrium moisture relation curves were best predicted by the modified Henderson equation.     

Effect of powder properties on discharge characteristics of cohesive carbonaceous fuel powders from a top discharge blow tank at high pressure

Abstract

Discharge experiments of two cohesive carbonaceous fuel powders (anthracite coal and petroleum coke) were carried out in a top discharge blow tank experimental system with design pressure up to 6.4?MPa. The effects of powder properties (particle size and powder category) on the discharge characteristics (including solid discharge rate, solids loading ratio, and discharge stability) from the top discharge blow tank at high pressure were investigated. Meanwhile, shear tests with a ShearTrac II shear tester were performed to investigate the flowability of these two cohesive powders. The results indicate that there exists a near-linear relationship between major consolidation stress and flow function (FF). As particle size decreases, the values of FF decrease and powder flowability becomes worse. However, as particle size decreases, the particle suspension velocity decreases correspondingly, and the gas permeability becomes worse and gas maintain ability becomes better, which contribute to higher solid discharge rate and better discharge stability, whereas solids loading ratio may have opposite variation tendency. Compared to petroleum coke with similar particle size, anthracite coal has better flowability and can obtain higher solid discharge rate and solids loading ratio, as well as better discharge stability. During the discharge processes of petroleum coke, it was found that as the number of discharge experiment increases, the discharge stability decreases correspondingly. After petroleum coke being discharged continuously for 4–6 times, the discharge process could not start again, adhesion phenomena of petroleum coke to the wall of conveying pipelines could be observed.     

Glass transition and the flowability and caking of powders containing amorphous lactose

Many powders contain amorphous components, such as amorphous lactose in milk powders, which when given sufficient conditions of temperature and water content, will mobilise as a high viscosity flow making the particles sticky. This can lead to increased cohesiveness, powder caking and increased adhesion to surfaces. The transition from the glassy state is established by increasing the powder temperature to above its glass transition temperature which can be measured using differential scanning calorimetry. Exposing milk powder to over 10-20 °C above the lactose glass transition makes the powder more sticky, rendering it a lot more cohesive and also increases its adhesion to a stainless steel surface. This glass transition induced stickiness is time-dependent. Over time, crystallisation can take place converting the amorphous lactose into crystalline lactose. Furthermore, the caking behaviour of powders depends on the amount of component present in the amorphous state. Finally, this work presents an approach for applying the measured relationship between the glass transition and water content for predicting caking problems with powders containing amorphous components.     

Spectral analysis of force fluctuations during probe penetration into cohesive powders

We investigate force fluctuations during probe penetration into cohesive powders consisting of ∼ 5 μm lactose particles with varying surface properties prepared by spray drying. The results obtained for the more cohesive powders were remarkably similar to those previously reported for orders of magnitude larger noncohesive particles. For the less cohesive powders, the spectral densities were instead found to exhibit two distinct power-law regions. Furthermore, the spectra were found to be independent of the geometry of the penetrating probe and dimensions of the die cavity. These findings suggest that the response is dominated by particle aggregate or agglomerate movement for the more cohesive powders, whereas the behaviour of the less cohesive ones is consistent with a response dominated by relatively weak force chains, with the fluctuations resulting from the recurring creation and collapse of jammed states being damped for length scales > 0.1 mm.