Experiment No.

Batch & Continuous Distillation

Date Performed: February 12, 2013

Date Completed: February 12, 2013

Submitted by: Group 4

Members Ching, Hans Elstin E. Gildo, Peniel Jean A. Lam, Angelo W. Uy, Marc Louie T.

Submitted to: Nathaniel P. Dugos, PhD Chemical Engineering Department Gokongwei College of Engineering

Date Submitted: March 26, 2013

I.

Objectives 1. To investigate Rayleighs equation in describing differential distillation. 2. To determine the temperature and concentration profile in a differential distillation process. 3. To determine the concentration profile in a packed column operating under total reflux conditions at steady state. 4. To determine HETP and Kya of a packed column.

II.

Theory Distillation is a unit operation to separate the components of liquid mixture into individual (or groups) of components by vaporization. Volatile liquids are readily vaporized at low pressure and the boiling point of the more volatile components drive the distillation process. The components are separated based on their physical properties, specifically relative volatility, a tool used to express the magnitude of the equilibrium distribution:

Where y is the vapor composition, x is the liquid composition, a is the more volatile component and b is the less volatile component. There are two kinds of distillation: batch and continuous. Batch distillation has the advantage of being able to handle different mixtures simply by changing its operating conditions, but with higher energy requirements and needs to be processed on a per batch basis. On the other hand, in continuous distillation, as the name implies, feed is continuously supplied and distilled.

In differential distillation, at any given time, the concentrations may be related by material balance, with W the amount in the still at any time of concentration x: ( )( )

Integrating and considering the initial feed as F and concentration xF, we obtain Rayleighs equation: The Rayleigh equation can be simplified into various forms such as: 1. When Henrys Law applies, y=mx where m=H/P. This, however, is only applicable for dilute solutions, where partial pressure of the vapor is a linear function of composition. The integrated equation yields

2. If the relative volatility is assumed to be practically constant, and substituting the relative volatility equation and integrating, we obtain in terms of the individual components,

Where subscript 1 refers to initial amounts and subscript 2 refers to the final amounts found in the solution. If the assumptions above cannot be applied, then the integral is evaluated by graphical or numerical methods.

In a packed column distillation, the advantages include simpler design, ease of operation, and lower pressure drop. In this experiment, total reflux was chosen for better and simpler data collection. A packed column may be expressed in terms of the number and height of a transfer unit. If we base it on the mass transfer in the interfacial contact between the liquid and vapor around a differential volume element: ( )

Substituting and solving for Z,

)(

The NTU can be determined from the experimental data by plotting the equilibrium curve together with the concentrations collected. Since the column is operated at total reflux, the operating line coincides with the diagonal thus the driving force (y*-y) is the vertical line from the equilibrium curve to the operating line. One can plot 1/(y*y) versus y or x since y=x at total reflux. The area under the curve yields the NTU. Since the height of the packing is known, then the HTU is evaluated. To measure the vapor flow rate, one can use the heat or wattage of the heater to estimate the vapor generated at steady state:

III.

Setup

IV.

Summary of Procedures:

A. Preparation of a Calibration Curve 1. Prepare a 0, 10, 20, 30, 40, 50, 60, 70, 80, 90 (% v/v) ethanol solution. 2. Determine each refractive indices of the different ethanol solution by using a refractometer. 3. Plot the refractive indices to the ethanol solution. B. Batch or Differential Distillation Experiment 1. Setup the batch distillation apparatus. 2. Prepare a 10% (250 mL) ethanol solution 3. Heat the setup until the first drop then record the initial temperature reading alongside start the time. 4. Take every 10 mL of distillate until 100 mL and for every 10 mL record the time and temperature. 5. Determine the refractive index of every 10 mL sample by using a refractometer. C. Packed Column Distillation at Total Reflux Conditions Experiment 1. Setup the Packed Colmn Distillation and prepare the ethanol solution. 2. Heat the setup for at least 45 to 60 minutes and make sure that every outlet is closed. 3. Every after 10 minutes, record the 4 temperature reading and take a sample for every outlet then determine the refractive index of each sample. 4. Repeat the previous step until the refractive index stabilizes.
V. Data

Part I. Batch Distillation A. Calibration Data

EtOH Conc in Water 0 10 20 30 40 50 60 70 80 90 99

Refractive Index 1.3319 1.3345 1.3411 1.3455 1.3535 1.3571 1.3577 1.3595 1.3614 1.3615 1.3605

B. Calibration Curve of EtOH-Water System

Calibration Curve for EtOH-Water

1.37 1.365 1.36 1.355 1.35 1.345 1.34 1.335 1.33 1.325 Refractive Index

y = -4E-06x2 + 0.0007x + 1.3297 R = 0.9832

0 20 40 60 80 y = 0.0003x + 1.3356 Concentration of EtOH in Water (%v/v) R = 0.8758

100

C. Batch Distillation Data

Refractive Index Volume (mL) 10 20 30 40 50 60 70 80 90 100 Flask Distillate 1.3395 1.3625 1.3381 1.3614 1.3370 1.3611 1.3355 1.3611 1.3343 1.3587 1.3335 1.3550 1.3328 1.3484 1.3320 1.3397 1.3319 1.3350 1.3318 1.3330

Volume Fraction Flask Distillate (x) (y) 0.1535 0.8967 0.1296 0.8600 0.1114 0.8500 0.0872 0.8500 0.0684 0.6735 0.0561 0.5102 0.0455 0.3290 0.0335 0.1569 0.0320 0.0793 0.0305 0.0485

D. Plot of 1/(y-x)
60 50 40 1/(y-x) 30 20 10 0 0.0000 0.0500 x 0.1000 0.1500 0.2000

E. Area Calculation

Area under the curve A1 A2 A3 A4 A5 A6

b1

b2

h 0.0015 0.0015 0.0120 0.0106 0.0123 0.0663 Total

Area 0.0562 0.0220 0.0696 0.0304 0.0237 0.0993 0.3012

55.6728 21.1351 21.1351 8.1010 8.1010 3.5270 3.5270 2.2023 2.2023 1.6526 1.6526 1.3455

Part II. Continuous Distillation A. Data

Steady-State Values T y* RI 80.1 0.822 1.3451 81 0.794 1.3536 86.5 0.6735 1.3517 98 0.198 1.3342

y 0.258066 0.465004 0.410664 0.066826

1/(y*-y) 1.773258 3.039553 3.804653 7.623461 Total

Area 1.616965 1.219376 -1.58286 1.253479

VI. Results and Analysis The calibration curve of ethanol-water system is used to compute for the actual concentrations of Ethanol in water using the measured refractive indexes. Two models were used to maintain accuracy. For RI values that are more than 1.3603, the linear model is used. RI = 0.0003 (Concentration) + 1.3356 For values below, the more fitted quadratic curve is used: RI = -410-6(Concentration)2 + 0.0007(Concentration) + 1.3297 From the data obtained, it can be computed that the area under the batch distillation curve is 0.3012. This means that the term ln(F/W) is equal to 0.3012 and thus, the Feed to Residue Ratio is equal to 1.3415. As for the continuous distillation, the calculated number of transfer unit is 1.2535. Knowing that the height of the tower is 0.9 m, the height of a transfer unit, HTU would be 0.717 m. VI. Conclusions and Recommendations: The group was able to utilize the Rayleigh Equation for the determination of the Feed to Residue ration, which is 0.3012. For the continuous distillation, the height of a transfer unit was also computed as 0.717 m. The calibration curve of the system turns out to be an accurate fit for the data but care must be taken from determining the actual data. Appendix I. References Olao, S. (2007). Experiments in Chemical Engineering, 2nd Ed. De La Salle University Press. Geankoplis, C. J. (2003). Transport Processes and Separation Process Principles, 4th ed. New Jersey: Pearson Education, Inc.