Binary Distillation Experiments in Chemical Engineering, by Servilano Si. Ola Jr Seen ee EXPERIMENT D2 BINARY DISTILLATION INTRODUCTION Distillation is one of the most important but also the most energy intensive separation process that chemical engineers should be concerned about. Thus, a good understanding of the theories and application of this unit operation is essential in order to minimize energy consumption, There afe many types of distillation operations, depending on the process followed, the type of equipment and the number of volatile components present in the solution to be purified. In this laboratory exercise, only two types are investigated, one using the concept of a binary equilibrium relationship by operating a simple batch distillation set- ‘up and the other one using the concept of rate process by the use of a packed distillation column operated under total reflux conditions. The binary system applied is ethanol-water ‘where students will investigate the validity of the Rayleigh’s equation for batch distillation and how to evaluate the number of transfer units and the mass transfer coefficient from ‘experimental data obtained from a packed distillation column, OBJECTIVES ‘The experiment is composed of two parts with the following objectives: PART I. Batch or Differential Distillation 1. To investigate the applicability of the Rayleigh’s Equation to describe differential distillation. 2. To determine the temperature and concentration profile ina differential distillation process. tion in a Packed Column: PART IL Batch Rect 1. To determine the concentration profile in a Packed distillation column operating under total reflux conditions a steady stat. 2. To determine the HETP and Kya of « packed distillation column,Experiments in Chemical Engincering, 2% ed Binary Distilation byServlano $B. Ola, Jr — ‘THEORY Distillation is a unit operation used to separate, by vaporization, components of @ liquid mixture of miscible and volatile substances into individual components or, in some ceases, into groups of components (McCabe et al, 1993). A liquid can be classified as volatile when itis readily vaporized at a relatively low temperature. The boiling of the more ‘olaile components of the mixture drives the distillation process. When the vapor is cooled, the more volatile material condenses in a greater proportion than the less volatile material ‘The components are separated based on their physical properties, specifically, relative volatilities, Relative volatility, a tool used to express the magnitude of the ‘equilibrium distribution, is defined as wo where z= Relative volatility y= Vapor composition x= Liquid composition A= More volatile component B= Less volatile component ‘There are two types of distillation classified according to its mode of operation. ‘These are continuous and the batch distillation. In a batch sysfem, the column can handle different mixtures by simply changing its operating conditions. The main disadvantage to using this kind of system, however, is that the longer the components are exposed to high temperatures, the better the chances that the components are broken down via thermal degradation. Along with this, the energy requirements ate usually higher for a batch system, Conversely, continuous distillation, as the name implies, feed is continuously supplied and separated it into two or more products over some period. On the other hand, batch distillation involves the processing of a batch of feed at a given time and splitting it into products by selectively removing the more volatile fractions over time. A, Differential Distitation When a binary solution of volatile liquids is subjected to batch differential distillation, the concentration of the solution in the distillery still decreases in the more Volatile component as the boiling point of the solution inereases. The resulting vapor is allowed to condense through a condenser and collected (ogether as the distillate product,Experiments in Chemical Engineering, 2 ed. Binary Disitation by Serlano $8. Olah, Jr ‘The problem in this case is 10 relate the initial amount of feed together with its concentration and the amount of over-all distillate collected and its concentration ‘AC any given time, the concentrations may be related by material balance, Referring to Figure .1, if W is the amount in the still at any time of concentration x; a ‘more volatile component balance yields x wr=(w—dW\(x=dr)= ydW wx—wa-+xdW +Wax—dWax = yd War = (y—2)d Ww de Wye igure I: Disilation System Integrating, considering the initial feed as F and concentration xr, (ala % de 2 a ne w ‘This equation is referred to as Rayleigh’s Equation. The instantaneous liquid composition, x and the corresponding vapor composition, y are assumed t© be in ‘equilibrium with one another. Vapor Liguid Equilibria (VLE) data may be determined from Vapor Pressure-Temperature, Boiling Point Composition diagram or Equilibrium data, or X-y diagram for the binary system. “The Rayleigh Equation may be simplified to various forms such as: 1. If Henry's law applies, y = mx where m = H/P. The integrated equation yields Teas are 6) =|s this equation, however, is applicable only for dilute solutions, where the partial pressure of the vapor isa linear function of composition DeExperiments in Chemical Engineering, 2 ed Binary Distillation by Serllano $8. lato. Fr 2. Ihe relative volatili assumed practically constant then, un a (@.—Dev substituting this in Equation 3 and integrating gives 0) or in erms of the individual component B, ayn o Subscript 1 refers to the initial amounts and subscript 2 refers to the final amounts found in the solution. The amount of distillate may be determined by material balance together with its composition, IF the above assumptions could not be applied, the best way to evaluate the integral of Equation 2 is by graphical or numerical methods. The graphical method is shown in Figure 2. Graphically, plot —— versus x at diferent stages ofthe experiment y to relate the amount distilled at anytime with composition and temperature by geting the urea under the curve and comparing this ara and composition wih the experimental data obtained. The validity of the simplified equation may also be compared with the experimental data Area = In w Figure 2: Graphical MethodExperiments in Chemical Engineering, 2" ed. Binary Distitlaion by Servillano SB Olah Ir B. Packed Colum Distillation ‘The use of a packed column in distillation is becoming more popular due to its case of operation, lower pressure drop and simpler design configuration. Packed Column distillation is based on rate processes as distinguished from equilibrium stage process typical of a plate column. The packed distillation column in the laboratory is operated on a batch process at total reflux conditions. Although, the system could be modified to ‘operate at specified reflux condition, Total reflux is used for better and simpler data collection and treatment. ‘The performance of a packed distillation column may be expressed in terms of, the number and height of a transfer unit which may derived from the mass transfer equation. If we consider an interfacial contact between the liquid and vapor around the differential element of volume as shown in Figure 3, ay, (y= ysdz. imerface bby material balance, aN, = Vd¥ = Vay substituting, and solving for Z, @ igure 3 %nterfacal Contact HTU (NTU) 6) ‘The NTU may be determined from the experimental data by plotting the equilibrium curve together with the concentrations collected Figure 4: Total Reflux Condiion D-13Experiments in Chemical by Semillano SB. Olah, Jr Engineering, 2" ed Binary Distillation Under total reflux, the operating line coincides with the diagonal, thus, the driving force (y"-y) i the vertical line from the equilibrium curve to the operating line as L shown in Figure 4 Several values of those may be obtained and plotted as —"— versus Yor x, since x = y at total reflux. Area = NTU Figur 8: Sobing for NTO. ‘The area under the curve in Figure will yield the NTU. Since the height of the packing is known, the HTU is evaluated. To calculate for the Ky, in Equation 8, the vapor flow rate must be known. However, since it was not measured in the experiment, the heat or wattage of the heater may be used to estimate the vapor generated at steady state, that is Vv 0 © of Solution is obtained from the diameter ofthe column, thus (1) HTExperiments in Chemical Engineering, 2* ed. Binary Disitaion by Serulano SB. Ola, Ie :QUIPMENT. |A. Actual Equipment ey ee Control System igure 6 Laboratory Distillation Column 1B. Equipment Description ‘The equipment contains a 4-inch bubble cap batch distillation column which may be ‘operated under total or partial reflux conditions. Also used in this experiment is & distillation column packed with glass beads for total reflux operations. As for the determination of the refractive index, a refractometer was used,Binary Distillation Experiments in Chemical Engineering, 2” ed by Serna $B. Ola. Je PROC URE A. Preparation of Calibration Curve 1 2. Use the ref 3._ Plot the refractive index versus ethanol concentration. B, Batch or Differential Distillation Experiment 1. Setup Make 10% ethanol solution (25 ml pure ethanol and 225 ml water). 3. Heat the setup until the first drop of condensate is collected. Record the initial temperature reading and start the time. 4. For every 10 ml of condensate collected, record the corresponding time and temperature. Using a refractometer, determine the refractive index of the saruples collected Repeat steps 4 and 5 ‘until you have at least six runs or until 60 to 70% of the solution is distilled. c batch distillation apparatus, ©. Packed Column Distillation at Total Reflux Conditions Experiment NOTE: The distillation column used for this part of the experiment will be operated at total reflux conditions. The setup has 4 exit points, namely outlet 4 located at the topmost part, outlet 2 and 3 located at the middle part and outlet | atthe bottom, 1. Pour into flask 1 L pure ethanol and 9 L water. 2. Check the distillation setup and make sure that there is no distillate collected by closing outlet 4 or the topmost part. Open such outlet only when needed, 3. Collect at least 0.5 ml sample of the ethanol-water solution from outlet 1 and determine its refractive index. 4, Heat the setup for at least 45 t0 60 minutes. Make sure, however, tha all outlets, are closed. 5. Every after 5 minutes, record the temperature reading and collect at least 0.5 ml sample from the four exit points or outlet. Then, determine their respective refractive indices. (6. Repeat step 5 until the refractive index per outlet stabilizes. 7. Return the excess samples collected per outlet to the main flask. D-16Experiments in Chemical Engineering, 2% ed by Serllano SB. Ol Binary Disilation DATA SHEET ‘Concentration of C:H,OH-H,0 (ev) Refractive Index B, Batch Distillation Volume (ml) Ist drop Temperature (°C) Refractive Index 10 20 30 40 30 0 70. 80 90 100 C. Packed Column Distilat (minutes) Refractive Index ‘Thermometer ‘Outlet 1] Outlet 2 =EExperiments in Chemical Engineering, 2" ed. Binary Distilation by Serilano SB. Ola, J After 20 minutes After 30 minutes ‘Time when steady state was achieved: ANALYSES AND CALCULATIONS. 1. Plot the calibration curve as refractive index versus ethanol concentration, Derive & correlation equation for refractive index as a function of concentration ‘Comment on the usefulness of this correlation. What is the range of concentration that generates the smallest and largest deviation? 3. For Batch Distillation, plot the theoretical ratio of FAW and the experimental ratio FAW versus the concentration of the residue. Describe the results. Is there good agreement between the experimental results with those obtained by Rayleigh’s ‘equation? 4, Compare the experimental amount of (otal distillate collected with the theoretical resulls using the graphical method of solution and using the average relative volatility during the entire differential distillation process. Tabulate and indicate the percent deviation, 5. For Batch Rectification, determine the theoretical number of stages based on the concentration of the solutions at the re-boiler and the condenser for the bubble-cap distillation column, Based on the results, determine the over-all plate efficiency. 6. Plot the actual concentrations of the liquid obtained from each plate using the xy equilibrium diagram and analyze the results, 7. For the packed column, determine the theoretical number of transfer units. Based on the measured height of the packed column, determine the mass transfer coefficient and the HETP. D-18