Temperature Characteristics of Pharmaceutical Powders During Microwave Drying

The internal temperature of wetted pharmaceutical powder samples dried in an experimental microwave system were monitored. In general, the temperature profile consisted of three distinct stages: short preheating stage, constant temperature period, and decreasing temperature phase. Approaching the end of the constant rate period, a local maximum in the temperature curve was observed. The development of the internal temperature profile was observed to be material dependent, with the dielectric, physical, and thermal properties of the powder and solvent being contributory factors. The characteristics were also dependent on bed dimensions (surface area and depth), with an increase in surface area and decrease in depth providing lower product temperatures. The surface temperature remained lower than the center temperature throughout the drying process, with the differential through the sample depth increasing on reducing the moisture content. A nonuniform temperature distribution developed across the sample cross section. Sample agitation was found to aid temperature leveling.     

Temperature Variations in Powder Beds during Combined Microwave-Convective Drying

The center temperature of wetted pharmaceutical powder samples dried under combined microwave-convective conditions in an experimental system (2.45 GHz, 90 W) was monitored. Introduction of convective air to the microwave system facilitated a reduction in the material temperature, with the extent of the decrease being dependent on the air temperature and velocity. In general, the variation in center temperature of a sample dried under microwave-convective conditions consisted of three distinct stages: a short “warming-up” period; a constant temperature stage, and a decreasing temperature phase. Towards the end of the constant-rate period, a local “peak” superimposed on the temperature curve was observed. The temperature history was found to be material dependant, with the dielectric, physical and thermal properties of the solvent and powder being contributory factors. The variation was also dependent on bed geometry (surface area and depth), with an increase in surface area and decrease in depth providing reduced product temperatures. The surface temperature remained lower than the center temperature throughout processing, with the gradient increasing on reducing the moisture content.     

Comparative Study of Microwave Sintering of Zinc Oxide at 2.45, 30, and 83 GHz

Temperature gradients that develop in ceramic materials during microwave heating are known to be strongly dependent on the applied microwave frequency. To gain a better understanding of this dependence, identical samples of ZnO powder compacts were microwave heated at three distinct widely separated frequencies of 2.45, 30, and 83 GHz and the core and surface temperatures were simultaneously monitored. At 2.45 GHz, the approximately uniform "volumetric" heating tends to raise the temperature of the sample as a whole, but the interior becomes hotter than the exterior because of heat loss from the surface. At 30 and 83 GHz, this interior to exterior temperature difference was found to be reversed, especially for high heating rates. This reversal resulted from increased energy deposition close to the sample's surface associated with reduced skin depth. A model for solving Maxwell's equations was incorporated into a newly developed two-dimensional (2-D) heat transport simulation code. The numerical simulations are in agreement with the experimental results. Simultaneous application of two or more widely separated frequencies is expected to allow electronic tailoring of the temperature profile during sintering.     

Vacuum Contact Drying Kinetics: An Experimental Parametric Study

Abstract

Vacuum contact drying kinetics of a model system consisting of nonporous glass beads and water has been experimentally measured on a laboratory scale. A methodology for determination of drying curves from experimental data in a statistically robust way has been developed. The effects of jacket temperature, head-space pressure, particle bed depth, vessel diameter, and particle size on drying rate during constant and falling rate periods have been studied. It was found that in the range of parameters investigated, drying rate does not depend on the means of realization of the driving force (by temperature or pressure); drying rate in the constant-rate period decreases with increasing bed depth while the overall heat-transfer rate increases due to increased surface area. A very strong dependence of drying rate and regime on particle size was observed; the constant-rate period disappeared for small particles.     

A New Approach to Modeling the Nucleation and Growth Kinetics of Tricalcium Silicate Hydration

The hydration kinetics of tricalcium silicate (C₃S), the main constituent of portland cement, were analyzed with a mathematical "boundary nucleation" model in which nucleation of the hydration product occurs only on internal boundaries corresponding to the C₃S particle surfaces. This model more closely approximates the C₃S hydration process than does the widely used Avrami nucleation and growth model. In particular, the boundary model accounts for the important effect of the C₃S powder surface area on the hydration kinetics. Both models were applied to isothermal calorimetry data from hydrating C₃S pastes in the temperature range of 10°–40°C. The boundary nucleation model provides a better fit to the early hydration rate peak than does the Avrami model, despite having one less varying parameter. The nucleation rate (per unit area) and the linear growth rate of the hydration product were calculated from the fitted values of the rate constants and the independently measured powder surface area. The growth rate follows a simple Arrhenius temperature dependence with a constant activation energy of 31.2 kJ/mol, while the activation energy associated with the nucleation rate increases with increasing temperature. The start of the nucleation and growth process coincides with the time of initial mixing, indicating that the initial slow reaction period known as the "induction period" is not a separate chemical process as has often been hypothesized.     

Vacuum Contact Drying Kinetics: An Experimental Parametric Study

Vacuum contact drying kinetics of a model system consisting of nonporous glass beads and water has been experimentally measured on a laboratory scale. A methodology for determination of drying curves from experimental data in a statistically robust way has been developed. The effects of jacket temperature, head-space pressure, particle bed depth, vessel diameter, and particle size on drying rate during constant and falling rate periods have been studied. It was found that in the range of parameters investigated, drying rate does not depend on the means of realization of the driving force (by temperature or pressure); drying rate in the constant-rate period decreases with increasing bed depth while the overall heat-transfer rate increases due to increased surface area. A very strong dependence of drying rate and regime on particle size was observed; the constant-rate period disappeared for small particles.     

Microwave-convective drying characteristics of pharmaceutical powders

Common pharmaceutical excipients and active ingredients, wetted with specific solvents, were dried in a combined microwave-convective system (2.45 GHz, 90 W). The drying curves showed a constant drying rate period, followed by two falling rate periods. Cross-flow air velocity had little effect on solvent evaporation rate in the initial stages; however, an increase in drying rate was observed during the falling rate period. Increasing air temperature increased the drying rate throughout the entire process, with reductions in drying time of up to 78% being observed. Average and maximum sample temperatures were found to decrease on addition of air-flow, the extent of which was dependent on material and operating conditions.     

水泥-石灰石粉体系抗碳化效应研究*

探讨石灰石粉比表面积、矿物掺合料、早强剂、防水物质及CO₂捕收剂对水泥-石灰石粉体系强度和碳化深度的影响。实验发现,硅灰替代20 kg/m³石灰石粉时28 d抗压强度达最高,为40 MPa,比空白高6 MPa,高比表面积(750 m³/kg)石灰石粉次之,为37 MPa,比空白高4 MPa,防水物质和过量硝酸钙会降低混凝土强度;掺入0.3%防水石蜡乳液可使体系碳化深度降至最低,达11 mm,比空白降低13 mm,掺入0.8%硝酸铁次之,碳化深度为13 mm,比空白降低11 mm,矿物掺合料替代石灰石粉不会有效降低碳化深度。因此可适度引入铁离子、防水组分或较高比表面积石灰石粉来提高该体系抗碳化性能。     

Microwave-Vacuum Drying Kinetics of Pharmaceutical Powders

Abstract

The drying kinetics (maximum drying rate, drying constants) and center temperature of selected powder (aspirin, paracetamol, lactose, and maize starch)–solvent (water, ethanol, methanol, and acetone) systems were monitored during microwave-vacuum drying. An experimental microwave-vacuum system (650 W and 2.45 GHz) operated at 61–81 kPa was used. The drying rate profile did not vary with the powder–solvent system; an initial warming-up period was followed by a constant-rate stage and two falling-rate periods. However, the drying kinetics were found to be both powder and solvent dependent, with the drying times for acetone-, ethanol-, and methanol-wetted materials being considerably shorter (up to 89.8%) than those of samples containing water. Although the general form of the temperature profile (short warming-up period, constant-rate stage, and decreasing temperature phase) was similar for all systems, the maximum temperatures varied quite significantly with solvent type, ranging from highest to lowest in the order water-ethanol-methanol-acetone. For most powder–solvent systems, reduced operating pressure facilitated increased drying rates and thus shorter drying times.     

Synthesis of nanocrystalline ZnO–NiO mixed metal oxide powder by homogeneous precipitation method

Nanocrystalline ZnO–NiO mixed metal oxide powder has been successfully prepared via a simple homogeneous precipitation method in short time. The nanocrystalline sample was obtained at low calcination temperature (350 °C). Specific surface area, crystallite size and optical band gap of the samples depend on calcination temperature. The synthesized samples were characterized by means of powder X-ray diffraction, thermal gravimetric analysis, Fourier transform infrared spectroscopy, diffuse reflectance spectroscopy, surface area measurements, scanning electron microscopy coupled with energy dispersive X-ray analysis, transmission electron microscopy and magnetic measurements. The synthesized powder samples have been tested for their catalytic reduction of 4-nitrophenol to 4-aminophenol in the presence of sodium borohydride.     

Characterization of the First Falling Rate Period During Drying of a Porous Material

This study deals with the evolution of the surface state and its influence on the drying of porous media. Surface temperature and saturation values are obtained using optical metrology. Analysis of the experimental results allows discussion of the apparition of constant drying rate period and to characterize the transition to the falling rate period. A mathematical model is developed to account for these observations and experimental results for some physical properties of a model material. It allows determination of the internal profile of moisture and the penetration of the drying front during the falling rate period.     

A fryer design with constant specific surface area

The specific surface area (surface area/volume) of a traditional frying vessel with a rectangular profile increases as the oil level decreases. In order to maintain a constant specific surface area of frying oil regardless of oil consumption, a special fryer was designed and constructed. The specific surface area of a frying vessel having a linear-inclined profile (Valentine batch fryer) deviated from a constant value by a maximum of 7.5%. The specific surface area of a frying vessel with an exponentially curved profile maintained a constant specific surface area even though the oil level varied.     

In-situ infrared thermographic analysis during dehydrogenationof cyclohexane over carbon-supported Pt catalysts using spray-pulsed reactor

Infrared thermography, a tool used for screening of active catalytic materials generally during the exothermic reactions has been used for thermal imaging during strong endothermic reaction of dehydrogenation of cyclohexane on Pt catalyst supported on active carbon cloth (CFF-1500s) sheets. A spray-pulsed mode was used for injection of atomized cyclohexane and to create alternate wet and dry condition on catalyst surface. The simultaneous product gas analysis and recording of the temperature profile of the catalyst surface using an IR camera was carried out. The production rate of hydrogen via endothermic dehydrogenation reaction is greatly dependent on the temperature of the catalyst surface. The observed change in the temperature profile at wet and dry conditions with varying pulse-injection frequency and corresponding product gas analysis reveals that the spray-pulse mode is useful in improving the catalyst activity. Further the reaction conditions were optimized using thermal profile data.Rajesh B. Biniwale-On deputation from NEERI, Nagpur India.     

Sintering Kinetics at Isothermal Shrinkage: Effect of Specific Surface Area on the Initial Sintering Stage of Fine Zirconia Powder

The isothermal shrinkage behaviors of fine zirconia powders (containing 2.8–2.9 mol% Y₂O₃) with specific surface areas of about 6 and 16 m²/g were investigated to clarify the effect of specific surface area on the initial sintering stage. The shrinkage of powder compact was measured under constant temperatures in the range of 1000°–1100°C. The increase in specific surface area enhanced the densification rate with increasing temperature. The values of activation energy ( Q ) and frequency-factor term (β₀) of diffusion at initial sintering were estimated by applying the sintering-rate equation to the isothermal shrinkage data. The Q of diffusion changes little but the β₀ increases with the increase in specific surface area. It is therefore concluded that the increase in the specific surface area of fine zirconia powder enhances the shrinkage rate because of an increase in the β₀ at the initial stage of sintering.     

Evaporation and Diffusion Transport Properties and Mechanical Properties of Alginate Dried Film

The effects of alginate concentration and drying temperature on drying kinetics/characteristics of alginate solution and mechanical property of formed solid films were examined. Solid films were fabricated through thin-layer drying of 1 to 4%w/w sodium alginate solution at 40, 60, and 80°C using the solvent-evaporation method. The water weight loss profile of alginate solution undergoing drying was recorded with time. The polymer weight of all solid films was kept constant. The plasticity of films was evaluated using thermomechanical analyzer. The findings indicated that both constant rate and falling rate periods existed during drying of dilute alginate solution or at low drying temperature since both surface and core waters were available for drying. The falling rate period dominated in drying of an alginate solution of high polymer concentration and at high drying temperatures with internal diffusion being the governing transport phenomenon for water. In the latter, an exponential relationship between water content and drying time was obtained. The drying process of 4%w/w alginate solution at 60 and 80°C was relatively simple as there was only a single drying stage, viz. the falling rate period requiring no consideration of critical moisture content. The drying rate was faster than those obtained from the dilute alginate solution or conducted at low temperature, such as 40°C. The plasticity attributes of films prepared from 4%w/w alginate solution can be modulated to a degree similar to films prepared from dilute alginate solution or dried at low temperature via changing the drying temperature between 60 and 80°C.     

Powder metallurgy magnesium composite with magnesium silicide in using rice husk silica particles

By using the solid-state reaction of rice husk silica particles with magnesium powder, P/M magnesium based composites dispersed with the magnesium silicide (Mg₂Si) and magnesium oxide (MgO) were fabricated. High-purity silica particles were originated from rice husks, one of the major agricultural wastes, via the citric acid leaching treatment and combustion in air. The effects of the silica particle characteristics such as size, crystalline and porous structures, on the reactivity of silica and magnesium to synthesize Mg₂Si intermetallics were discussed. As the results by DTA and XRD analysis, finer silica particles were more effective for the solid-state reaction at low temperature due to the increase of their surface area contacted with magnesium powder. Amorphous silica was also more useful for this reaction than the crystalline one. The reactivity of rice husk silica was superior to that of the conventional mineral silica particles not only because of its amorphous structure but also the larger specific surface area due to their pore structures. In the case of the green compact of the elemental mixture of silica particles and Mg powder, the silica particle size was not effective on the reactivity because the coarse particles were fractured into fine ones by cold compaction. The distribution of Mg₂Si intermetallics of magnesium powder composites consolidated by SPS process was investigated by XRD and SEM-EDS analysis. When the sintering temperature was over the exothermic temperature of the mixture in the DTA profile, the synthesis of Mg₂Si completely occurred during sintering. The sinterability of the elemental mixture powder was improved when employing the amorphous rice husk silica particles. The density and hardness of their composites sintered over the ignition temperature of the DTA profile were remarkably high because of the good densification by the high reactivity and the distribution of Mg₂Si hard compounds.     

Sintering Behavior of Fine Aluminum Nitride Powder Synthesized from Aluminum Polynuclear Complexes

The sintering behavior of fine AIN powder synthesized from an aluminum polynuclear complex was investigated. The focus of this work was to investigate the densification behavior of the AIN powder with different particle sizes (specific surface area: 3.2–22.8 m²/g). The AIN powder was synthesized from basic aluminum chloride and glucose mixed in a water solution. This powder was divided into two groups: one with 2 wt% Y₂O₃ added as the sintering aid and the other without such an additive. The AIN powder investigated possessed favorable densification potential. The density of the AIN powder with a surface area of 16.6 m²/g and without additives attained theoretical density at 1700°C. Adding Y₂O₃ further decreased the sintering temperature required for full densification to 1600°C. It is speculated that low-temperature sintering of our fine AIN powder with Y₂O₃ proceeds in two steps: in the initial stage, sintering proceeds predominantly through interdiffusion between yttrium aluminates formed on the AIN powder surface; in the second stage, the densification may occur by the interdiffusion between solid phases formed by a reaction between the yttrium aluminates and AIN. To investigate the effect of oxygen on sintering, the content of oxygen in AIN powder was varied while the particle size was kept constant. In this study, the difference in surface oxygen content scarcely affected the sintering behavior of fine AIN powder.     

Observation of initial deposition process of electroless nickel plating by quartz crystal microbalance method and microscopy

The initial deposition process of electroless nickel plating was investigated by combining a quartz crystal microbalance (QCM) method with microscopy. The authors found an anomalous deposition rate in the initial deposition and four stages were noted: an induction period before the initiation of deposition, an acceleration period with an increase in the deposition rate, a deceleration period with a decrease in the deposition rate and a stationary period at a constant deposition rate. The practical surface area of the deposits increased until the deposits became continuous and reached a constant value. On the other hand, the deposition rate per unit practical surface area decreased monotonously as the deposition proceeded. As a result, an anomalous initial deposition rate was observed. The four periods also appeared in the deposition when the catalyzation process was repeated 4 times. In this case, the number of grains at the initial stage was greater, and nucleation still continued until the deposits became continuous. The initial deposits, therefore, became continuous at lower thickness.     

超声波辅助插层-剥离法制备煤系高岭土微粉的研究

我国煤系高岭土储量丰富,为满足造纸、纺织等行业个性化的需求,通常要对其进行深加工。以山西朔州煤系高岭土为原料,分别在恒温磁力搅拌和超声波作用下探究了煤系高岭土/二甲基亚砜(DMSO)插层复合物制备的最佳条件,在插层复合物的基础上对煤系高岭土进行超声辅助剥离,制备得到高岭土微粉,并利用XRD、SEM、BET、TG-DSC等方法分析表征样品。正交实验结果表明在磁力搅拌条件下DMSO用量、插层时间以及插层温度均对插层率具有一定的影响,引入超声波有利于高岭土插层率的提升。插层复合物经超声辅助剥离后晶粒厚度明显减小,高岭土片层状结构大体上呈现碎片化,仅保留少部分大的片状结构,其边缘碎化,整体上也出现碎裂的趋势。剥离样品的比表面积和孔径均大幅度增加,为硬质高岭土的剥离和超微细粉体的制备提供了新的思路。     

Simulation of thermal and electric field evolution during spark plasma sintering

Finite element simulations have been conducted to determine the temperature distribution (both in radial and axial direction), heat and electric flux-field in the powder compact/die/punch assembly during the spark plasma sintering (SPS) process. A thermal–electrical coupled model with temperature dependent thermal and electrical properties is implemented. The simulation studies were conducted using both ABAQUS and MATLAB and a range of power input, varying thermal conductivity of powder compact were considered. Also, the effect of time variation on both thermal and electric field evolution was assessed. During SPS, the heat transmission pattern and the temperature difference between the specimen center and the die surface depend on thermal conductivity of the powder compact, time of sintering and power input. The simulation results also revealed that the temperature gradient across the powder compact/graphite die wall is higher for conditions of higher power input and/or powder compact with lower thermal conductivity.