Name: Crezl Y.

Montebon ID No: 2008-0072

Date: September 16, 2013 Subject: ChE 157

EXPERIMENT 1: Running a Distillation Column at Total Reflux ABSTRACT

The objectives of this experiment are: (1) to be able to run a distillation at total reflux and (2) learn in the process the specifications of the column and the available data that is generated by the simulation. The experiment was performed in a simulation lab using the software AZprocede. In the simulation, the reboiler was filled up to 90% and was heated to boiling. As the level of the reflux drum reached to 25%, cascade mode was applied and total reflux was set. Then, the set-up was allowed to reach steady-state. As the set-up was just acquiring steady-state, the reboiler temperature, molar fraction of component A in the reboiler and reflux drum was also recorded with respect to time. These were plotted with respect time using MS excel.
I. INTRODUCTION II. METHODOLOGY

The separation process known as distillation is a method for separating the various components of a liquid solution which depends upon the distribution of these components between a vapor phase and a liquid phase. All components are present in both phases. The vapor phase is created from the liquid phase by vaporization at the boiling point. Continuous distillation works using the principles of distillation, but it is particularly useful in dealing with large volumes of industrial chemicals by allowing distillation to happen without interruption. It is important especially in the petroleum industry, where it is used to refine crude oil. Distillation column can also run in total reflux. The total reflux condition represents operation with no product removal. The entire overhead vapor is condensed and returned as reflux. Consequently, the reflux ratio (L/D) is infinite. This, in turn, makes the operating lines the 45 degree line (prove it to yourself by setting D=0, and noticing that consequently L=V). With the operating lines on the diagonal, they are as far as they can get from the equilibrium curve, so if the number of plates are stepped off using the diagonal and the equilibrium curve, the number of theoretical stages will be a minimum. Total reflux simulation will be performed by the proponent.

The program that was used in the simulation was AZprocede. First, the reboiler was filled up to 90% by opening the valve in feed area to 100% and let it flow until the mass of the feed is only 1797.7 kg. Next, the mixture was heated to boiling by opening the valve to 70%, which enables the entry of steam. As soon as the mixture boils, the valve opening was reduced to 25%. Then, the level of the reflux drum was let to reach 25%, then the valve in the reflux was changed to cascade mode and total reflux was set. Then, mixture was gradually fed to the reboiler, in order for the reach 60% level. After these parameters were reached, the set-up was allowed to reach steady-state. The boiler temperature, molar fraction of component A in the bottom and distillate was also recorded with respect to time. As soon as it reached the steady-state, the simulation was stopped and the reflux drum, together with the bottom, was drained. The whole simulation has been captured using Camtasia for ease of access and review of the whole experiment after it was complete.

III.

DATA AND COMPUTATION

Temp 90 70 50 0 200 400 Time (sec) 600 800

Fig 1. Temperature vs. time plot

Reboiler Mole Fraction of A (%) 150 100 50 0 0 200 400 Time (sec) 600 800 Reflux

Fig 2. Molar fraction of component A vs. time plot

Fig 3. McCabe-Thiele at steady-state IV. DISCUSSION

As soon as the data were gathered, the temperature, molar fraction of A in the reboiler and reflux drum vs time was plotted using MS

Excel. As shown in Fig 1, as expected, the temperature gradually increases as the time passed. In here, the molar concentration of A in the reboiler decreases as time passes by (see Fig. 2). This means that the composition in the reboiler contains more of the less volatile component, which is propanol that has a boiling point of 97C 98C. In further details, at the start of the set-up, the composition in the reboiler contains 65% isopropyl alcohol, which has a boiling point of 82.6C, therefore the sample in the reboiler will boil at a temperature close to 82.6. The boiling temperature at the start is at 86.4C. As the distillation proceeds, gradual amount of isopropyl alcohol was separated to the mixture, leaving large amount of propanol in the reboiler. This resulted to an increase of the boiling temperature and as the steady-state is finally attained, the final composition in the reboiler is 30.8% isopropyl alcohol which resulted to a boiling temperature of 93.0C. This value is much closer to the boiling point of propanol. From Figure 2, we can also see that the decrease in the mole fraction of component A is subsequently equal to the fraction of component A that has been added into the reflux drum. This can be proven by applying mass balance with repect to component A. Furthermore, this will continue until it reaches a relative volatility () equal to 1. Relative volatility defines the mixture if it can still be separated. When = 1, no separation is possible: both component A and component B are equally volatile. They will vaporize together when heated. It also means that equilibrium has reached; the net transfer rate from vapour to liquid is exactly balanced by the transfer rate from liquid to vapour. We can say that steady-state can be attained when = 1, or equilibrium is reached. To determine if it really reached equilibrium, we can set = 1, then by using the formula of relative volatility which is: ( ) ( ) Rearranging the equation, we get an equation of a line, which is y = x, the graph of this line is the 45 line. As seen in figure 3, all of the plate touches the 45 line; therefore, all plates have already reached its equilibrium. Moreover, in the simulation, where the cascade loop was implemented, the valve in the heating steam was reduced to 25%. This was

Temp (C)

done in order to prevent flooding. Since the more steam that will be introduced to the reboiler, the more vapor that will be formed which could increase the pressure drop in the distillation column. And as soon as the pressure drop in the distillation column reached to its maximum capacity, the vapor phase can now lift the liquid phase which will eventually cause flooding. Furthermore, when the level in the reboiler was at 25%, cascade made was set. This was done to improve control system performance over single-loop control whenever either: (1) Disturbances affect a measurable intermediate or secondary process output that directly affects the primary process output that we wish to control; or (2) the gain of the secondary process, including the actuator, is nonlinear. V. CONCLUSION The AZprocede program used in the simulation of the total-reflux distillation is a very big help for the students. They can learn a lot concerning the whole set-up of a distillation column along with its process flows and process control features. The students can also determine and assess factors that affects a distillation process. VI. REFERENCES McCabe, W. L., Smith J. C., and Harriott, P., Unit Operations of Chemical Engineering, 6th ed., McGraw Hill Company, New York, 2001 Perry, R. H., Green, D., Maloney, J. O., Perrys Chemical Engineers Handbook, 6th Ed, McGraw Hill Company, 1985 http://www.wisegeek.com/what-iscontinuous-distillation.htm