From laboratory- to pilot-scale: moisture monitoring in fluidized bed granulation by a novel microwave sensor using multivariate calibration approaches

Recently, microwave resonance technology (MRT) sensor systems operating at four resonances instead of a single resonance frequency were established as a process analytical technology (PAT) tool for moisture monitoring. The additional resonance frequencies extend the technologies’ possible application range in pharmaceutical production processes remarkably towards higher moisture contents. In the present study, a novel multi-resonance MRT sensor was installed in a bottom-tangential-spray fluidized bed granulator in order to provide a proof-of-concept of the recently introduced technology in industrial pilot-scale equipment. The mounting position within the granulator was optimized to allow faster measurements and thereby even tighter process control. As the amount of data provided by using novel MRT sensor systems has increased manifold by the additional resonance frequencies and the accelerated measurement rate, it permitted to investigate the benefit of more sophisticated evaluation methods instead of the simple linear regression which is used in established single-resonance systems. Therefore, models for moisture prediction based on multiple linear regression (MLR), principal component regression (PCR), and partial least squares regression (PLS) were built and assessed. Correlation was strong (all R²?>?0.988) and predictive abilities were rather acceptable (all RMSE ≤0.5%) for all models over the whole granulation process up to 16% residual moisture. While PCR provided best predictive abilities, MLR proofed as a simple and valuable alternative without the need of chemometric data evaluation.     

Growth kinetics in particle coating by top-spray fluidized bed systems

The kinetics of growth for the coating of particles in top- spraying fluidized bed systems is reported. The results indicated that only a small amount of particles that visited the spraying region are coated at a time. It was also revealed that different particle sizes are not equally coated during the process. In a polydispersed particle distribution, smaller particles were found to receive more coating than their larger counterparts. This preferential coating, which was associated with a rapid decrease in the distribution variance, is more pronounced in the earlier parts of the process. When a narrower seed distribution was used, the preferential coating was reduced. A segregation factor, f_s, was introduced in the development of a growth kinetics model to represent the chance of each particle size visiting the coating region. The result for the distribution from the model clearly resembled the results obtained experimentally. For the top-spraying process, the segregation factor was found to be an exponentially decaying function of particle weight. For lactose particles coated with hydroxypropyl methyl cellulose, two different rates of growth were observed during the coating process.     

Hydrodynamics of a fluidized bed in the intertube space of staggered and in-line tube bundles

The article presents the results of the experimental investigation of the effect of the horizontal and vertical pitches of tubes on the hydrodynamics of a fluidized bed. A formula is presented for calculating the mean porosity of the bed in the intertube space of tube bundles with optimum arrangement.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 38, No. 5, pp. 829–835, May, 1980.     

Thermal regime of batch furnaces for heating metal in a fluidized bed

An analytical investigation is made of the temperature variation in a fluidized-bed furnace, and in a part with low thermal resistance being heated in it.     

Development of a robust calibration model for nonlinear in-line process data

A comparative study involving a global linear method (partial least squares), a local linear method (locally weighted regression), and a nonlinear method (neural networks) has been performed in order to implement a calibration model on an industrial process. The models were designed to predict the water content in a reactor during a distillation process, using in-line measurements from a near-infrared analyzer. Curved effects due to changes in temperature and variations between the different batches make the problem particularly challenging. The influence of spectral range selection and data preprocessing has been studied. With each calibration method, specific procedures have been applied to promote model robustness. In particular, the use of a monitoring set with neural networks does not always prevent overfitting. Therefore, we developed a model selection criterion based on the determination of the median of monitoring error over replicate trials. The back-propagation neural network models selected were found to outperform the other methods on independent test data.     

Multiway methods to explore and model NIR data from a batch process

Multiway methods are tested for their ability to explore and model near-infrared (NIR) spectra from a pharmaceutical batch process. The study reveals that blocking of data having a nonlinear behaviour into higher-order array can improve the predictive ability. The variation in each control point is independently modelled and N-way techniques overcome the nonlinearity problem. Important issues as variable selection and how to fill in for missing values have been discussed. Variable selection was shown to be essential to be able to perform multiway modelling. For spectra not yet monitored, use of mean spectra from calibration set gave close to the best results. Decomposing the spectra by N-way techniques gave additional information about the chemical system. To support the results simulated data sets were used.     

Optimization and characterization of direct coating for ibuprofen particles using a composite fluidized bed

Ibuprofen particles (mean particle size, 27 μm and melting point, 76 °C) as core materials were directly coated with a water-soluble polymer. The primary particles were preserved using a composite fluidized bed with a dispersing mechanism at the bottom of the fluidized bed apparatus. Coated primary particles were obtained under the following 3 conditions: (1) Setting the spray air flow rate at 10 L/min from the initial to 2% coating, (2) adding the low-viscosity water-soluble polymer macrogol 6000 to the hypromellose coating solution, and (3) changing the spray air flow rate to 15 L/min from 2% coating. The particles obtained were confirmed to be coated primary particles by scanning electron microscopy of their cross sections prepared by the cryo-focused ion beam method. The dissolution test showed a marked improvement in the solubility of ibuprofen from the coated primary particles compared with that of a physical mixture. In conclusion, the optimization of the direct coating process made it possible to undertake primary particle coating of a raw material that has a low melting point and a particle size of not more than 50 μm. Primary particle coating contributes to improvements in the physicochemical properties of drugs.     

Mathematical modeling of the heat-transfer process and solid particles in a fluidized bed

The authors formulate a two-concentration model of particle mixing in a fluidized bed, accounting for particle inertia.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 42, No. 2, pp. 251–259, February, 1982.     

The dynamic analysis of a small fluidized bed combustor

The dynamic characteristics of a small fluidized bed combustor for coal were examined analytically and experimentally.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 25, No. 3, pp. 476–484, September, 1973.We would like to thank J. J. Henderson, of the Faculty of Electronics and Electrical Engineering of Birmingham University, for his advice and assistance in this work.     

Filtration of nano-particles by a gas-solid fluidized bed

The filtration of 80 nm SiO2 and Al(2)O(3) particles in a gas stream using fluidized beds was studied. Silica sand and activated carbon (A.C.) were adopted as bed materials to filtrate 80 nm SiO2 and Al(2)O(3) particles. The collected particles were elutriated from the fluidized bed, so the filtration was a dynamic process and the variations of the removal efficiency with time were studied. Experimental results showed that the filtrations of 80 nm SiO2 and Al(2)O(3) particles with a bed material of silica sand were not dynamic processes but the filtration by A.C. was. The removal efficiencies for SiO2 and Al(2)O(3) particles using silica sand as bed material were held steady and found to be equal, between 86 and 93%. A.C. is considered to be more efficient than silica sand because it has a high specific surface area. However, the experimental data yield conflicting results. The removal efficiency of Al(2)O(3) particles fell from 92% initially to 80% at the end of test-a little lower than that obtained by filtration using silica sand. A higher voidage of A.C. than silica sand weakens the removal of nanoparticles since the diffusion mechanism dominates. The removal efficiency of SiO2 by A.C. decayed from 83 to 40% with time passed. The huge differences between the filtration efficiency of SiO2 and that of Al(2)O(3) particles by A.C. was associated with the extensive segregation of SiO2 and A.C. particles, which caused more SiO2 particles to move to the top of the bed, where they were elutriated. The weak inter-particle force for SiO2 decreased the removal efficiency also.     

Instability in a granular bed fluidized by a gas flow

Stability in fluidization is considered in an approach in which the granular bed is considered as a structureless element with a definite working response, and the boundary to the stability region in parameter space is examined.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 31, No. 3, pp. 410–417, September, 1976.     

Probability analysis of the motion of particles in a fluidized bed

The velocity and acceleration of particles moving in a fluidized bed are analyzed by means of histograms and random functions.     

采用表面凝胶化技术制备超疏水性涂膜

采用表面凝胶化技术制备了超疏水性涂膜.在醇溶性氟化聚合物溶液中,在水量不足的酸性条件下,掺杂聚四氟乙烯(PTFE),得到了杂化复合溶胶.涂敷后,以表面凝胶化技术为手段,在涂层表面形成了微米和纳米相结合的阶层结构膜.TEM和XPS证实了凝胶化只在膜表面发生,SEM和AFM观察到膜表面的形貌与天然荷叶表面极其相似.该方法制备的涂膜对水的接触角高达155°,并具有良好的力学性能,可用于制备超疏水性功能化膜材料.     

Properties of thin TiN films deposited onto stainless steel by an in-line dry coating process

A new coil-coating pilot plant, capable of utilizing ion plating, sputtering and plasma-assisted chemical vapor deposition (PACVD) processes, independently or in series, was developed and optimum conditions for TiN, TiC, Al_xO_y, SiO_x and Cr coating were established. This paper is mostly concerned with the results of characterization (conducted in parallel by the authors′ two institutions) of TiN films deposited by ion plating or sputtering onto type-304 stainless steel strips. In particular, the dependence of the basic properties such as chemical composition, structure, adhesion, and color on the coating process are discussed with respect to anti-corrosion, anti-wear, and decorative applications. TiN coatings with a very attractive gold coloration were obtained; they performed well in wear testing, but did not show satisfactory corrosion resistance. However, it was found that the latter can be improved significantly by depositing a SiO_x, top layer by PACVD above the TiN coating. Thus the in-line dry coating processes are capable of producing highly functional steel surfaces with decorative color and high corrosion resistance.     

Engineering methods of analysis of devices with a vibrationally fluidized bed

A linear rheological model is worked out for the forced oscillations of a granulated bed in a vibration facility, including the working chamber, the associated gas chambers, and the gas distributing grating. Results of the analysis are compared with experimental data.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 6, No. 6, pp. 907–913, June, 1991.     

致密SiC包覆层低温流化床化学气相沉积制备及形成机制

一般致密SiC材料的制备需要极高的温度,而降低制备温度一直是SiC制备领域的重要研究方向。采用流化床化学气相沉积法,在球形二氧化锆陶瓷颗粒上制备了厚度为几十微米的SiC包覆层。通过对不同温度SiC包覆层的显微形貌及微观结构变化规律研究,给出了沉积效率变化规律,发现低温产物富硅,而高温产物富碳。对不同氩气含量的实验研究发现,氩气的加入可以促进沉积反应向富碳方向移动,从而可以在显著降低温度的条件下制备出致密SiC包覆层。综合实验结果给出了流化床化学气相沉积方法在不同温度及氩气浓度条件下制备SiC的物相分布图。      

The effective thermal diffusivity of a bed fluidized by vibration

Measurements are reported for the horizontal component of the effective thermal diffusivity of a bed in a vessel of diameter 20 cm with vibrations of 16–30 Hz and amplitude 2–6 mm.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 20, No. 2, pp. 274–280, February, 1971.     

Thermal stability and flammability studies of coated polymer powders using a plasma fluidized bed process

In this work, the thermal stability of organosilicon coatings, polyamide-6 powders and polyamide-6 clay nanocomposite powders coated with organosilicon are studied. The coatings were obtained from polymerization of 1.1.3.3-tetramethyldisiloxane (TMDS) monomer doped with oxygen using a cold remote nitrogen plasma (CRNP) process. A fluidized bed reactor using CRNP assisted polymerization was used to coat the polymer powders. The effect of oxygen addition to TMDS on the thermal stability was investigated. Oxygen addition to TMDS promotes the formation of more thermally stable coated polymers. In the case of the polyamide-6 clay nanocomposite, the Limiting Oxygen Index values were much improved. This shows that the deposits are effective fire retardant coatings.