Design and mechanism of agglomeration of aspirin crystals in pure solvents

Agglomeration with improved flowability for platy crystals is desirable in pharmaceutical downstream processing. The formation of agglomerates in pure solvents without the aid of bridging liquids is a convenient and low-cost method compared with complex spherical crystallization. In this work, the adhesion free energies between aspirin crystals in six solvents were calculated using Lifshitz-van der Waals acid-base theory to screen suitable solvents for agglomeration. The maximum stirring rate for agglomeration was determined by adhesion forces and dispersion forces. Then the agglomerates of plate-shaped aspirin were successfully prepared in acetone, methanol, ethanol, 2-propanol, and ethylene glycol without additives by simple cooling crystallization. The interactions between solvent and crystal surfaces were also used to explain the outcomes. A feasible mechanism for the agglomeration process of platy crystals was elucidated, involving the adhesion of dominant crystal facets at the beginning. The effect of stirring rate, cooling rate, and initial supersaturation on agglomeration degree and particle size of aspirin agglomerates were studied. The obtained aspirin agglomerates under the optimal conditions exhibited a uniform particle size distribution, a high agglomeration degree, and superior flowability.     

Biopolymer-assisted synthesis of yttrium oxide nanoparticles

Yttrium oxide nanopowder was prepared by a novel technique using an alginate biopolymer as a precursor. The technique is based on thermal decomposition of an yttrium alginate gel, which is produced in the form of beads by ionic gelation between the yttrium solution and sodium alginate. The effect of post-annealing temperature on the particle size of the nanocrystals was investigated at various tempera- tures. The products were characterized using X-ray diffraction, scanning electron microscopy, and atomic force microscopy. The size of the nanocrystalline Y2O3 particles varied from 22.7 to 38.7 nm, depending on the annealing temperature and time. The grain size distribution （GSD） was also determined. The GSD became more non-symmetrical as the annealing temperature increased, and the width of the distributions for the powders produced using the alginate method was less affected by heat treatment. This alginate method was compared with the conventional glycine combustion method, on the basis of particle size. The particles obtained using the proposed technique were smaller than those obtained using the combustion method. Alginate-assisted thermal decomposition is therefore an easy and cost-effective method for preparing nanosized Y2O3 crystals.     

Modeling of the random packing of a loose layer of polydisperse spherical particles

A method for calculating the loose packing structure of polydisperse spherical particles with a predetermined size distribution function is proposed. The coordinates of the particle centers in the loose layer are determined as the result of random fall of single spheres on a substrate under the action of gravity, assuming the inelastic collision of the spheres and considering the force of their adhesive interaction, and also assuming that the motion of one sphere on the surface of the other is pure slip. Numerical simulation is used to obtain the pattern of arrangement of polydisperse spherical particles in the loose powder layer, whose porosity depends on the particle size distribution function. The results are compared with experimental data.     

TAILORING OF PORE SIZE IN MESOPOROUS SILICA WITH STEARIC ACID AND PVP

Mesoporous silica was prepared using tetrathoxysilane （TEOS）, cetadecyltrimethylammonium bromide （CTAB）, aqueous ammonia, acetone and water as silica source, template agent, precipitator and solvent respectively. Stearic acid and polyvinylpyrrolidone （PVP） were employed as additional templates to tailor the pore size in the resultant porous silica. BET, SAXRD and SEM analyses were used to characterize the surface area, pore size, pore structure, pore regularity and morphology of the sample. BET measurement results showed that PVP could increase the surface area but diminish the pore size while stearic acid could decrease the surface area but enlarge the pore size. SAXRD analysis indicated that more additional template introduction gave rise to less order-structured products. All these various results could be attributed to the differently modified CTAB micelles involving stearic acid and PVP addition.     

Controlled preparation and characterization of nano-sized hexagonal Mg（OH）2 flame retardant

Nano-sized hexagonal magnesium hydroxide （Mg（OH）2） with good dispersibility was synthesized by a double injection-hydrothermal method, utilizing polyvinylpyrrolidone （PVP） as an additive and with optimized processing parameters. SEM and BET analysis showed that the mean particle size and specific surface area of the Mg（OH）2 particles were 174 nm and 50.77 m^2/g, respectively. The FT-IR spectra and the XRD patterns showed that PVP was adsorbed on the surface of the Mg（OH）2 crystal, thus effectively limiting particle agglomeration and hindering crystal growth along the （1 01 ） plane. TGA showed a decrease in the decomposition temperature and an increase in the weight loss of the Mg（OH）2 particles due to addition of PV/.     

干水材料对瓦斯爆燃抑制的实验研究

为了研制绿色环保高效的抑爆剂，以疏水型气相二氧化硅和去离子水为原料，采用机械搅拌法制备具有“固包液”结构的干水材料。利用20 L近球形爆炸装置测试干水材料对瓦斯爆燃的抑制效果。实验结果表明:当添加的干水材料较少（2 g和3 g）时，干水材料对瓦斯爆燃产生促进效果；当添加的干水材料大于4 g时，对瓦斯爆燃有抑制效果。通过研究不同粒径的干水材料对瓦斯爆燃的影响，发现干水材料的粒径对瓦斯爆燃最大压力的影响较小，但显著影响最大爆燃压力上升速率；对比不同类型改性干水材料对瓦斯爆燃的抑制效果，综合比较得出抑制效果由强到弱顺序为:尿素改性干水材料、磷酸二氢铵改性干水材料、聚磷酸铵改性干水材料、普通干水材料。     

砂岩球体法向恢复系数实验研究

法向恢复系数是岩崩块石运动分析的关键参数,其取值直接决定了块石的运动轨迹。本文中采用自行设计的碰撞实验装置和声频采样技术,测定了砂岩球体碰撞的法向恢复系数,研究了粒径、碰撞速度、含水状态和板的弹性特性4个因素对恢复系数的影响。结果表明:砂岩球体法向恢复系数存在复杂的尺寸效应,恢复系数随粒径的增大先增大后减小;碰撞过程中存在的黏弹性耗能机理和弹塑性损伤耗能机理共同作用产生了复杂的尺寸效应;受砂岩非均质特性的作用,粒径较小时,恢复系数的速度效应较明显(随速度增大而增大),粒径较大时速度对恢复系数的影响消失;砂岩饱和使黏弹性耗能和弹塑性损伤耗能增加,使恢复系数比风干时低;等效弹性模量对恢复系数的影响较大,等效弹性模量越大,法向恢复系数越小。     

Size segregation and particle velocity fluctuations in settling concentrated suspensions

We investigate the sedimentation of concentrated suspensions at low Reynolds numbers to study collective particle effects on local particle velocity fluctuations and size segregation effects. Experiments are carried out with polymethylmetacrylate (PMMA) spheres of two different mean diameters (190 and 25 μm) suspended in a hydrophobic index-matched fluid. Spatial repartitions of both small and large spheres and velocity fluctuations of particles are measured using fluorescently labelled PMMA spheres and a particle image velocimetry method. We also report measurements of the interstitial fluid pressure during settling. Experiments show that size segregation effects can occur during the sedimentation of concentrated suspensions of either quasi-monodisperse or bidisperse spheres. Size segregation is correlated to the organisation of the sedimentation velocity field into vortex-like structures of finite size. A loss of size segregation together with a significant decrease of the fluid pressure gradient in the bulk suspension is observed when the size of vortex-like structures gets on the order of the container size. However, the emergence of channels through the settling zone prevents a complete loss of size segregation in very concentrated suspensions.     

Evaporation of thin liquid droplets on heated surfaces

We carry out combined experimental and theoretical studies of liquid droplet evaporation on heated surfaces in a closed container filled with saturated vapor. The droplets are deposited on an electrically heated thin stainless steel foil. The evolution of droplet shapes is studied by optical methods simultaneously with high-resolution foil temperature measurements using thermochromic liquid crystals. A mathematical model is developed based on the assumptions that the droplet surface has uniform mean curvature and the contact line is pinned during evaporation. Both the dynamics of liquid–vapor interface and the temperature profiles at the foil are shown to be in good agreement with the experimental data.     

Homogeneous precipitation of α-phase Co–Ni hydroxides hexagonal platelets

This paper describes the synthesis of α-phase Co–Ni hydroxides hexagonal platelets through homogeneous precipitation, using hexamethylenetetramine (HMT) or urea as a hydrolytic agent. In the CoCl₂–NiCl₂–HMT system, pure α-phase can be synthesized at the concentrations of both metal ions higher than 20 mM, while in the CoCl₂–NiCl₂–urea system, the formation of pure α-phase is independent of the concentrations of the metal ions. When using HMT, monodisperse hexagonal platelets of α-phase Co–Ni hydroxides can be produced in the presence of polyvinylpyrrolidone (PVP). Cyclic voltammogram curve of the hexagonal platelets prepared with HMT demonstrates electrochemical performance superior to that of urea.     

Measuring evaporation of micro-fuel droplets using magnified DIH and DPIV

This paper details the use of magnified digital in-line holography (MDIH) and digital particle image velocimetry (DPIV) to measure the evaporation rates of fuel micro-droplets undergoing heating. The technique can be used to measure instantaneous evaporation along an individual droplet trajectory, or if applied to a series of droplets, the average evaporation over a number of successive measurement locations. The advantage of this technique over traditional optical techniques is greater spatial resolution and depth of field for the high magnification factors used. An application of the technique to the evaporation measurement of diesel fuel droplets ranging from 10 to 90 μm is presented. Results reveal that similar to larger droplets, temperature plays the dominant role in evaporation processes, with little sensitivity to initial droplet size found for a peak reactor temperature of 660 K.     

Size-dependent cellular uptake and sustained drug release of PLGA particles

Poly (lactic-co-glycolic) acid (PLGA) particles have become a commonly used drug delivery strategy in the pharmaceutical industry. In this work, we aim to investigate the size-dependent cellular internalization of PLGA particles and its effects on sustained drug release. We prepared three different-sized particles using PLGA (200, 500 and 2000 nm) ranging from submicrometer to micrometer. Dexamethasone (DEX) with excellent anti-inflammatory properties was used as a model drug to prepare DEX-loaded PLGA particles (DPs). We comprehensively investigated the encapsulation efficiency, cellular uptake and in vitro drug release profile. Pharmacodynamic assessment revealed that, in the lipopolysaccharide (LPS)-induced RAW 264.7 cells model, 500 nm DPs showed sustained anti-inflammatory efficacy. This work provides important information for designing PLGA-based drug delivery systems for biomedical applications.     

Directional Wave Propagation in a Highly Nonlinear Square Packing of Spheres

We studied the dynamic response of a two-dimensional square packing of uncompressed stainless steel spheres excited by impulsive loadings. We developed a new experimental measurement technique, employing miniature tri-axial accelerometers, to determine the stress wave properties in the array resulting from both an in-plane and out-of-plane impact. Results from our numerical simulations, based on a discrete particle model, were in good agreement with the experimental results. We observed that the impulsive excitations were resolved into solitary waves traveling only through initially excited chains. The observed solitary waves were determined to have similar (Hertzian) properties to the extensively studied solitary waves supported by an uncompressed, uniform, one-dimensional chain of spheres. The highly directional response of this system could be used as a basis to design granular crystals with predetermined wave propagation paths capable of mitigating stress wave energy.     

On the use of quartz crystals in dynamic stress and force transducers

An important consideration in determining the veracity of data obtained from X-cut quartz crystals used to measure nominally one-dimensional load states is the role which spatial nonuniformity of the normal stress distribution on the crystal will play in determining the transducer output signal. This role was found to be minor both for crystals located 0.74 mm below a surface subjected to impact by spherical steel strikers and for 25.4-mm-diam crystals positioned in a 12.7-mm-diam Hopkinson bar through which a longitudinal wave was travelling. Load transducers utilizing two crystals to eliminate undesirable signals arising from bending of the crystal were also studied by attaching these devices to plates and subjecting them to dynamic loading by steel spheres. While bending effects were successfully eliminated, it was found that the method of transducer attachment may give rise to additional unwanted signals associated with other modes of crystal deformation.     

Accurate analysis of multicomponent fuel spray evaporation in turbulent flow

The aim of this paper is to perform an accurate analysis of the evaporation of single component and binary mixture fuels sprays in a hot weakly turbulent pipe flow by means of experimental measurement and numerical simulation. This gives a deeper insight into the relationship between fuel composition and spray evaporation. The turbulence intensity in the test section is equal to 10%, and the integral length scale is three orders of magnitude larger than the droplet size while the turbulence microscale (Kolmogorov scales) is of same order as the droplet diameter. The spray produced by means of a calibrated droplet generator was injected in a gas flow electrically preheated. N-nonane, isopropanol, and their mixtures were used in the tests. The generalized scattering imaging technique was applied to simultaneously determine size, velocity, and spatial location of the droplets carried by the turbulent flow in the quartz tube. The spray evaporation was computed using a Lagrangian particle solver coupled to a gas-phase solver. Computations of spray mean diameter and droplet size distributions at different locations along the pipe compare very favorably with the measurement results. This combined research tool enabled further investigation concerning the influencing parameters upon the evaporation process such as the turbulence, droplet internal mixing, and liquid-phase thermophysical properties.     

Detonation waves in trinitrotoluene

Fabry-Perot, ORVIS, and VISAR laser interferometry are used to obtain nanosecond time resolved particle velocity histories of the free surfaces of copper and tantalum discs accelerated by detonating trinitrotoluene (TNT) charges and of the interfaces between TNT detonation products and lithium fluoride crystals. TNT detonation reaction zone profiles are measured for self-sustaining detonation and piston supported overdriven (supracompressed) waves. The experimental records are compared to particle velocity histories calculated using very finely zoned meshes of the exact dimensions with the DYNA2D hydrodynamic code. The Ignition and Growth reactive flow model, which is based on the Zeldovich-von Neumann-D?ring (ZND) theory of detonation, yields excellent agreement with the experimental records for TNT using an unreacted von Neumann spike pressure of 25 GPa, a reaction rate law which releases 90% of the chemical energy within 80 ns and the remaining 10% over an additional 200 ns, and a reaction product equation of state fit to cylinder test data assuming a Chapman-Jouguet pressure of 19 GPa. The late time energy release is attributed to diffusion controlled solid carbon particle formation. Received 26 July 1997 / Accepted 29 December 1997     

爆轰法合成纳米CeO粉末*2

爆轰合成过程中采用Ce(NO₃)₃·6H₂O制备的可爆药剂,并利用X射线衍射仪(XRD)和透射电子显微镜(TEM)对合成的纳米CeO₂粉末进行了检测,研究了起爆方式对于合成产物结晶化度、粒径和形貌的影响。结果表明,采用Ce(NO₃)₃·6H₂O制备的可爆药剂,可以合成立方晶系的球形纳米CeO₂; 提高可爆药剂的爆速,可有效降低纳米CeO₂的粒径,得到球形化更好的纳米粒子。     

Coating of finely dispersed particles by two-fluid nozzle

Particle coatings are used extensively to generate dispersed solids with well-defined properties, e.g., to protect active ingredients, with most coating processes using core particles of a diameter larger than 200 μm. This work contributes to the development of a coating process for fine dispersed particles (diameter less than 50 μm) by combining two particle-formulation processes, namely, coating and spray drying. The feasibility of the operation is based on and demonstrated by the innovative application of a two-fluid nozzle. Experiments were conducted by using glass particles as core particles and sodium benzoate as the coating agent. The coating of finely dispersed particles is achieved by the spraying of particles and coating solution as a homogeneous suspension. The aim is to create droplets with only one contained particle at the nozzle outlet. After evaporation of the water in the droplet, a thin solid film is built on the particle surface. The suspension viscosity was measured and compared with empirical equations from the literature. The liquid-film thickness on the particle surface was calculated to predict the building of a uniform coating layer or agglomerates. In this study, the feasibility of pneumatic transport through the nozzle and an investigation of the process were illustrated. The agglomeration fraction and degree of coating of the particle surface were analyzed optically by scanning electron microscopy. In this way, the influence of different processes and suspension parameters on the product quality were determined.     

Controllable precipitation of naproxen micro-particles with different morphologies

A simple precipitation method was proposed to prepare naproxen micro-particles with different controllable morphologies, using capillary video microscopy to study the precipitation process. Different particle shapes were obtained including spherical, platelet-like, stick-like, needle-like, and butterfly-like, all in the micro-size range. It was found that the sizes and morphologies of the formed naproxen particles were sensitive to the nature and concentration of the added surfactant, and depended significantly on processing conditions such as temperature, stirring speed, and initial drug concentration. In addition, precipitation with different surfactant types and concentrations would not affect the crystal microstructure of the formed naproxen particles.