Continuous process for production of hydrogenated nitrile butadiene rubber using a Kenics® KMX static mixer reactor

A continuous process for hydrogenating nitrile butadiene rubber (NBR) was developed and its performance was experimentally investigated. A Kenics® KMX static mixer (SM) is used in the process as a gas–liquid reactor in which gaseous hydrogen reacts with NBR in an organic solution catalyzed by an organometallic complex such as an osmium complex catalyst. The Kenics® KMX SM was designed with 24 mixing elements with 3.81 cm diameter and arranged such that the angle between two neighboring elements is 90°. The internal structure of each element is open blade with the blades being convexly curved. The dimensions of the SM reactor are: 3.81 cm ID 80 S and 123 cm length and was operated cocurrently with vertical upflow. The NBR solutions of different concentrations (0.418 and 0.837 mol/L with respect to [C?C]) were hydrogenated by using different concentrations of the osmium catalyst solution at various residence times. The reactions were conducted at a constant temperature of 138°C and at a constant pressure of 3.5 MPa. From the experimental results, it is observed that a conversion and/or degree of hydrogenation above 95% was achieved in a single pass from the designed continuous process. This is the first continuous process for HNBR production that gives conversions above 95% till date. Optimum catalyst concentration for a given mean residence time to achieve conversions above 95% were obtained. Finally, a mechanistic model for the SM reactor performance with respect to hydrogenation of NBR was proposed and validated with the obtained experimental results. © 2009 American Institute of Chemical Engineers AIChE J, 2009     

Liquid phase residence time distribution for gas–liquid flow in Kenics static mixer

The residence time distribution (RTD) of the liquid phase for co-current gas–liquid upflow in a Kenics static mixer (KSM) with air/water and air/non-Newtonian fluid systems was investigated. The effect of liquid and gas superficial velocities on liquid holdup and Peclet number was studied. Experiments were conducted in three KSMs of diameter 2.54 cm with 16 elements and 5.08 cm diameter with 8 and 16 elements, respectively, of constant L_e/D_e = 1.5 for different liquid and gas velocities. A correlation was developed for Peclet number, in terms of generalized liquid Reynolds number, gas Froude number and liquid Galileo number, where as for liquid holdup, a correlation was developed as a function of gas Reynolds number. The axial dispersion model was found to be in good agreement with the experimental data.     

Residence Time and Concentration Distribution in a Kenics Static Mixer

Static mixers, often referred to as motionless mixers, are in-line mixing devices that consist of mixing elements inserted into a length of pipe. Most of the experimental works in this field have concentrated on establishing design guidelines and pressure drop correlations. Due to experimental difficulties, few articles have been published on the investigation of the flow and mixing mechanisms. In this work, a Kenics KMX static mixer was utilized to study concentration and residence time distribution (RTD) and effect of Reynolds number on mixing. The static mixer had six mixing elements arranged in-line along the length of the tube, and the angle between two neighboring elements was 90°. The length of the mixer was 0.98 m with internal and external diameters of 5.0 cm and 6.0 cm, respectively. The main continuous fluid was water, and NaCl solution was used as a tracer. All experiments were conducted with three replications at three Reynolds numbers, Re = 1188.71, 1584.95, and 1981.19. A dispersion model was used to model the RTD data. The experimental results were compared with the model results and reasonable agreement was achieved.     

Turbulent liquid–liquid dispersion in SMV static mixer at high dispersed phase concentration

The aim of this paper is to investigate the influence of physico-chemical parameters on liquid–liquid dispersion at high dispersed phase concentration in Sulzer SMV™ mixer. Four different oil-in-water systems involving two different surfactants are used in order to evaluate the effect of interfacial tension, densities and viscosities ratio on mean droplets size diameters. Moreover the influence of the dispersed phase concentration on the pressure drop as well as on the droplet size distribution is investigated. Two different droplets size distribution analysis techniques are used in order to compare the resulting Sauter mean diameters. The comparison between residence time in the mixer and surfactants adsorption kinetics leads to take into account the evolution of the interfacial tension between both phases at short times. Finally experimental results are correlated as a function of dimensionless Reynolds and Weber numbers.     

CFD simulation and experimental measurement of gas holdup and liquid interstitial velocity in internal loop airlift reactor

This paper documents experiments and CFD simulations of the hydrodynamics of our two-phase (water, air) laboratory internal loop airlift reactor (40 l). The experiments and simulations were aimed at obtaining global flow characteristics (gas holdup and liquid interstitial velocity in the riser and in the downcomer) in our particular airlift configurations. The experiments and simulations were done for three different riser tubes with variable length and diameter. Gas (air) superficial velocities in riser were in range from 1 to 7.5 cm/s. Up to three circulation regimes were experimentally observed (no bubbles in downcomer, bubbles in downcomer but not circulating, and finally the circulating regime). The primary goal was to test our CFD simulation setup using only standard closures for interphase forces and turbulence, and assuming constant bubble size is able to capture global characteristics of the flow for our experimental airlift configurations for the three circulation regimes, and if the simulation setup could be later used for obtaining the global characteristic for modified geometries of our original airlift design or for different fluids. The CFD simulations were done in commercial code Fluent 6.3 using algebraic slip mixture multiphase model. The secondary goal was to test the sensitivity of the simulation results to different closures for the drag coefficient and the resulting bubble slip velocity and also for the turbulence. In addition to the simulations done in Fluent, simulation results using different code (CFX 12.1) and different model (full Euler–Euler) are also presented in this paper. The experimental measurements of liquid interstitial velocity in the riser and in the downcomer were done by evaluating the response to the injection of a sulphuric acid solution measured with pH probes. The gas holdup in the riser and downcomer was measured with the U-tube manometer. The results showed that the simulation setup works quite well when there are no bubbles present in the downcomer, and that the sensitivity to the drag closure is rather low in this case. The agreement was getting worse with the increase of gas holdup in the downcomer. The use of different multiphase model in the different code (CFX) gave almost the same results as the Fluent simulations.     

Gas/liquid dispersions with a SMX static mixer in the laminar regime

A Sulzer SMX mixer was used to disperse gas into viscous, Newtonian and non-Newtonian fluids. The investigation covered the effect of the dispersed phase volume fraction, the viscosity of the continuous phase, the mixer length and the power draw. The flow regime was kept laminar in all the experiments. The dispersion of gas was carried out with gas concentrations between 1% and 7% in volume. Using the “process viscosity” concept, it was possible to collapse all the measured sizes on a single master curve by using the energy consumption in the mixer as the common variable between the experiments. Comparison was made with a Kenics mixer. The SMX mixer was found to be better adapted to the dispersion task due to its internal structure.     

Fluidization behavior in a circulating slugging fluidized bed reactor. Part I: Residence time and residence time distribution of polyethylene solids

Square nosed slugging fluidization behavior in a circulating fluidized bed riser using a polyethylene powder with a very wide particle size distribution was studied. In square nosed slugging fluidization the extent of mixing of particles of different size depends on the riser diameter, gas velocity, hold up and solids flux in the riser. Depending on the operating conditions the particle residence time distribution of a riser in the slugging fluidization regime can vary from that of a plug flow reactor to that of a well-mixed system.Higher gas velocities cause shorter particle residence times because of a significant decrease in the hold-up of particles in the riser at higher gas velocities. A higher solids flux also shortens the average residence time. Both influences have been quantified for a given polyethylene-air system.Residence time and residence time distribution were determined for different particle size and the influence of gas velocity, solids flux, hold up and riser diameter was studied. When comparing data from segregation and residence time experiments it is clear that segregation data can predict the spread in residence time as a function of overall residence time, particle size and gas velocity. The differential velocity between small and large particles found in the segregation experiments can predict the spread in residence time as found in the residence time distribution experiments with a powder with a broad particle size distribution. Raining of particles through the slugs was studied as a function of plug length, gas velocity and pulse length. It was found that raining is not the determining mechanism for segregation of particles.     

Effect of fiber length distribution on gas holdup in a cocurrent air-water-fiber bubble column

An experimental investigation is reported on the effect of fiber length distribution on gas holdup in a cocurrent air-water-fiber bubble column. Different combinations of 1 and 3 mm Rayon fibers are used to simulate different fiber length distributions. At a constant total fiber mass fraction, gas holdup generally decreases with increasing mass fraction of the 3 mm Rayon fiber while other conditions remain constant. Crowding factors estimated using four different methods (N_c=N_c,A, , N_c,L, and N_c,M) and the parameters and are tested on their performance to quantify the overall effects of fiber mass fraction and fiber length and its distribution on gas holdup. and provide the best characterization of the fiber effects on gas holdup in the cocurrent air-water-fiber bubble column. The crowding factor estimated using the model-based average fiber length (N_c,M) also provides a good characterization and is better than the other crowding factor definitions.     

SK静态混合器内各截面停留时间分布实验研究

采用脉冲示踪法对SK静态混合器内各截面的停留时间进行了实验测试,比较了流量对各截面停留时间分布的影响.结果表明:在同一截面上,随着流量增加,平均停留时间减小,停留时间分布密度曲线变得高而窄;在相同流量下,沿着轴线方向,平均停留时间增大,量纲一方差减小,流体流动趋向于活塞流.同一截面上,随着流量增加应答峰初期的斜率较陡,...     

Single and two-phase flows in a horizontal pipe with a Kenics static mixer: Effect of pressure drop on mixing

Single and two-phase flows pressure drops through a Kenics static mixer were investigated, for liquid and gas Reynolds numbers ranging from 8110 < Re_L < 18 940 to 1730 < Re_G < 8680, respectively. New friction factor correlations were established for single and two-phase flows, showing better agreement than those available in the literature. Dissipated energy and characteristic time constants were estimated from experimental data. For instance, a dissipated energy with a maximum value of 510 W/kg was calculated in two-phase flow with the drift-flux model. The dispersed phase reduced the characteristic mixing times and its influence was more important than the continuous phase for all the characteristic mixing time investigated. Furthermore, the macroscopic characteristic mixing time was shown to be the governing mixing process for almost all gas and liquid flow rates explored.     

Residence time distribution and dispersion of gas phase in a wet gas scrubbing system

Residence time distribution (RTD) of exhaust gas in a wet scrubbing system was investigated for application to the removal of SO _x , NO _x or dust included in exhaust gas. The mixing of gas phase in the wet scrubbing system was also examined by considering the axial dispersion coefficient of gas phase. Effects of gas amount (velocity), liquid amount (velocity) and solid floating materials on the residence time distribution (RTD) and axial dispersion coefficient of exhaust gas were discussed. The addition of solid floating materials could change the RTD and thus dispersion of exhaust gas in the scrubbing system. The mean residence time and axial dispersion coefficient of exhaust gas were well correlated in terms of operating variables.     

Drop breakage model in static mixers at low and intermediate Reynolds number

Drop break-up process for the flow of liquid-liquid dispersion in a static mixer has been investigated. Two new theoretical models for the drop break-up at low and intermediate Reynolds number for variant viscosity ratio of the dispersed phase to the continuous phase have been developed assuming that the flow through the static mixer elements is analogous to the flow through porous media. This concept has recently been established by Morançais et al. (Chem. Eng. Commun. 179 (1999) 77) and Legrand et al. (Chem. Eng. Res. Des. 79 (2001) 949). The boundary-layer shear force concept has been applied to predict the drop break-up at low Reynolds number and at intermediate Reynolds number, the effect of inertia on the drop break-up has been considered. The predicted drop sizes are in reasonable agreement with experimental results.     

Numerical study on gas and liquid slugs for Taylor flow in a T-junction microchannel

The rapid development of microfabrication techniques creates new opportunities for applications of microchannel reactor technology in chemical reaction engineering. The extremely large surface-to-volume ratio and the short transport path in microchannels enhance heat and mass transfer dramatically, and hence provide many potential opportunities in chemical process development and intensification. Multiphase reactions involving gas/liquid reactants with a solid as a catalyst are ubiquitous in chemical and pharmaceutical industries. The hydrodynamics of the flow affects the reactor performance significantly; therefore it plays a prominent role in reactor design. For gas/liquid two-phase flow in a microchannel, the Taylor slug flow regime is the most commonly encountered flow pattern. The present study deals with the numerical simulation of the Taylor flow in a microchannel, particularly on gas and liquid slugs. A T-junction empty microchannel with varying cross-sectional width (0.25, 0.5, 0.75, 1, 2 and 3 mm) served as the model micro-reactor, and a finite volume based commercial computational fluid dynamics (CFD) package, FLUENT, was adopted for the numerical simulation. The gas and liquid slug lengths at various operating and fluid conditions were obtained and found to be in good agreement with the literature data. Several correlations in the T-junction microchannel were developed based on the simulation results. The slug flows for other geometries and inlet conditions were also studied.     

Tomography measurements of gas holdup in rotating foam reactors with Newtonian, non-Newtonian and foaming liquids

Rotating solid foam reactors have already proven to show high mass transfer rates and to be a potential alternative to slurry reactors. The rotation of a foam block stirrer results in a high mass transfer and in the development of different reactor sections showing specific hydrodynamics and gas holdup distributions. In order to optimize the reactor system the hydrodynamics in a lab scale reactor are studied using γ-ray tomography, a powerful method to measure the gas holdup in three-phase reactors. The influence of liquid properties, such as viscosity and surface tension, and the rotational speed on the gas/liquid distribution in the different reactor sections is investigated. Especially the viscosity has a strong effect on the entrapment of gas bubbles in the foam block structure, while the surface tension is the dominant parameter in the outer reactor section. The influence of these parameters on the inset of foaming and the collapse of the gas/liquid dispersion is investigated. Conclusions on the mass transfer performance are drawn and recommendations for further optimizations of the reactor design and the operational conditions depending on the liquid properties are developed.     

Effects of internals on phase holdup and backmixing in a slightlyexpanded-bed reactor with gas-liquid concurrent upflow

Five different internals were designed, and their effects on phase holdup and backmixing were investigated in a gas-liquid concurrent upflow reactor where the spherical alumina packing particles of three diameters (3.0, 4.5 and 6.0 mm) were slightly expanded under the conditions of varied superficial gas velocities (6.77×10^-2-3.61×10^-1 m·s^-1) and superficial liquid velocities (9.47×10^-4-2.17×10^-3 m·s^-1). The experimental results show that the gas holdup increases with the superficial gas velocity and particle size, opposite to the variational trend of liquid holdup. When an internal component is installed amid the upflow reactor, a higher gas holdup, a less liquid holdup and a larger Peclet number characterizing the weaker backmixing are obtained compared to those in the bed without internals under the same operating conditions. Additionally, the minimal backmixing is observed in the reactor equipped with the internals with a novel multi-step design. Finally, empirical correlations were proposed for estimating gas holdup, liquid holdup and Peclet number with the relative deviations within 11%, 12% and 25%, respectively.     

Computation of system turbulences and dispersion coefficients in circulating fluidized bed downer using CFD simulation

In this study, the Eulerian computational fluid dynamics model with the kinetic theory of granular flow model was effectively used to compute the system turbulences and dispersion coefficients in a circulating fluidized bed (CFB) downer. In addition, the obtained model was used to simulate all the system velocities.     

Mass transfer in bubble column for industrial conditions—effects of organic medium, gas and liquid flow rates and column design

Most of available gas-liquid mass transfer data in bubble column have been obtained in aqueous media and in liquid batch conditions, contrary to industrial chemical reactor conditions. This work provides new data more relevant for industrial conditions, including comparison of water and organic media, effects of large liquid and gas velocities, perforated plates and sparger hole diameter.The usual dynamic O₂ methods for mass transfer investigation were not convenient in this work (cyclohexane, liquid circulation). Steady-state mass transfer of CO₂ in an absorption-desorption loop has been quantified by IR spectrometry. Using a simple RTD characterization, mass transfer efficiency and k_La have been calculated in a wide range of experimental conditions.Due to large column height and gas velocity, mass transfer efficiency is high, ranging between 40% and 90%. k_La values stand between 0.015 and and depend mainly on superficial gas velocity. No significant effects of column design and media have been shown. At last, using both global and local hydrodynamics data, mass transfer connection with hydrodynamics has been investigated through k_La/ε_G and k_La/a.     

Evaluation of pseudohomogeneous models for heat transfer in packed beds with gas flow and gas-liquid cocurrent downflow and upflow

Several pseudohomogeneous models are used by researchers in the study of heat transfer in packed beds. In this work, five of the most used pseudohomogeneous models (to one, two and three parameters) are analyzed, for gas and gas-liquid flow configurations. The models were evaluated concerning the following aspects: (a) the fitting between calculated and measured temperatures, (b) the values of thermal parameters, (c) their confidence intervals, (d) the quality of the estimation of the thermal parameters by analysis of their Box biases, and (e) the nonlinear dependence of the calculated temperatures on the thermal parameters (using the curvature measures of Bates and Watts). It was observed, particularly in gas-liquid flow, that the fittings between calculated and measured temperature profiles are better for models in which a wall heat transfer coefficient is incorporated to consider the convective resistance at the bed wall. It was also noted that the values of the thermal parameters fitted from the pseudohomogeneous models may be very different at identical operational conditions. The effective axial thermal conductivity may be neglected in the modeling because its estimation does not affect the residual functions. Besides, the estimation of k_a is tricky because it depends on the initial guess and also because the parameter is extremely sensitive to changes in the operational conditions. The confidence intervals for the parameters depend on the model and are also affected by the experimental conditions. The estimation of the parameters was adequate for the k_r-h_W and k_r-k_a models and the curvatures measures were satisfactory only for models in which h_W was not incorporated.     

An analysis of liquid CO2 drop formation with and without hydrate formation in static mixers

The formation process of CO₂ drops in various types of Kenics Static Mixers was analyzed from the perspective of energy dissipation in the mixer, focusing on the formation of drop surfaces. Experimental studies on CO₂ drop formation were conducted under varying temperatures, pressure, and flow rates, with and without hydrate formation. Analysis of the CO₂ drop size and distribution at several locations within the static mixer was conducted, as of pressure drop in the mixer, to determine dissipation energies. In all the experimental conditions, by considering the surface energy for hydrate formation, the energy required for the formation of CO₂ drops correlated well with total energy dissipation by mixer flow, which is represented by a pressure drop along the mixer. This process has important applications to the formation of liquid CO₂ for ocean disposal as a countermeasure to global warming. © 2010 American Institute of Chemical Engineers AIChE J, 2010     

Effect of gas expansion on the velocity of individual Taylor bubbles rising in vertical columns with water: Experimental studies at atmospheric pressure and under vacuum

This study was designed to determine the effect of gas expansion on the velocity of Taylor bubbles rising individually in a vertical column of water. This experimental study was conducted at atmospheric pressure or under vacuum (33.3 and ) using three different acrylic columns with internal diameters of 0.022, 0.032, and 0.052 m, and more than 4.0 m high. A non-intrusive optical method was used to measure velocity and length of Taylor bubbles at five different locations along the columns. The operating conditions used correspond to inertial controlled regime.In experiments performed under vacuum, there is considerable gas expansion during the rise of Taylor bubbles, particularly when they approach the liquid free surface where the pressure drop (due to the hydrostatic pressure) is of the order of magnitude of the absolute pressure. The liquid ahead of the bubble is displaced upward by an amount proportional to the gas expansion resulting in increased bubble velocity. The calculated Reynolds number suggests a laminar regime in the liquid ahead of the bubble. However, the experimentally determined velocity coefficient C for each column was much smaller than 2, which would be expected for laminar flow. The value of C obtained ranges from 1.13±0.09, for the narrowest column, to 1.40±0.24, for the widest column. This suggests that a fully developed laminar flow in the liquid ahead of the bubble is never achieved due to continuous bubble expansion at a variable rate, regardless of column height.The velocity coefficient C can be used to calculate the contribution of liquid motion to bubble velocity. Subtracting this contribution from the measured bubble velocity defines a constant value which is nearly identical to the bubble rise velocity measured in the same column operated as a constant volume system (two ends closed) where gas expansion is absent.