MT303 Batch Distillation

Group B1(b) 09002061 09d02019 09d02022 09002059 Puneet Singla (report) Amruta Rokade (report) Tarun Gangwar (ppt) K Sri Vivek (presentation)

Date of submission: 10-08-2011 Date of presentation: 17-08-2011

AIM : To determine the height equivalent to number of theoretical stages and the number of transfer units for a packed column. MOTIVATION : Distillation is the most widely used separation technique in the chemical and petroleum industry and is performed in either tray or packed columns . It is a very frequent separation process in the pharmaceutical industry and in wastewater treatment units. Batch distillation is an unsteady state operation usually carried out in a batch still to which a column equivalent to a number of equilibrium stages is attached and packings are used . Many industries use distillation for critical separations in making useful products. When running under reflux condition the efficiency of the distillation process greatly increases. Hence, it is essential to determine the number of stages required for a particular output concentration to design a distillation column

THEORY: Distillation is commonly used in separating and purifying liquids in industry. Its operation is based on differences in boiling points between the components being separated. When the relative volatility between the components being separated is high, distillation tends to be cheaper than other separation methods. In this experiment, methanol and ethanol are separated using a three stage distillation column. A batch will be prepared in the heating coil reboiler prior to the start of the lab period. The column will be started up under total reflux conditions, and then distillate product will be drawn off. By operating the column under different conditions, its performance can be characterized. Control of the column throughout experimentation will be achieved using a computerized control system. Sample compositions will be determined using refractive index. We calculate the number of stages by two different methods a) Fenske's equation:

Nmin = number of theoretical stages at total reflux, av = average relative volatility.

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b) The graphical McCabe-Thiele Method can be used to determine the number of ideal stages and feed tray location. To do this, you make a plot showing the equilibrium curve, feed line, and operating lines for the rectifying and stripping sections (all on the same axis), and then find answers by graphical construction.

EXPERIMENTAL PROCEDURE :

Prepare a calibration chart of refractive index (RI) vs.mole fractions of components Methanol and Ethanol.

Fill approximately 2/3rd volume of the reboiler with a mixture Methanol and Ethanol.

When the top and the bottom temperatures become steady (based on two successive readings taken at 10 min time interval) it indicates that the system has attained steady state and the samples may be withdrawn.

Start water circulation through the Condenser andSwitch on the heating mantle and all control panels and allow the temperature in the distillation to rise.

2 to 4 ml of top sample is collected in a test-tube after purging oft some quantity. The test-tube should be immediately closed to avoid losses. Determine the RI of the sample.

Count the number of actual plates in the column

Calculation Procedure:

Mole fraction of methanol in feed as well as in reflux is obtained using calibration graph

The corresponding Ya values are obtained using vapour-liquid equilibrium data

The average volatility is calculated using equation 2 and number of plates is calculated by Fenskesequation

McCabe-Thiele graph also gives the number of theoretical plates and HETP is calculated using both the methods using relation given in equation 3.

NTU is calculated using equation 5 and using the value, HTU is obtained by equation 4

Calculations:
S NO. 1 2 3 4 5 6 Volume Of Methanol 0 2 4 6 8 10 Volume Of Ethanol 10 8 6 4 2 0 Mole Fraction Of Ethanol 1 0.734893 0.50969 0.316011 0.14767 0 Mole Fraction Of Methanol 0 0.265107 0.49031 0.683989 0.85233 1 Refractive Index 1.3581 1.3552 1.3464 1.3401 1.3339 1.327

Table 1

Calibration Chart
1.365 1.36 1.355 Refractive Index 1.35 1.345 1.34 1.335 1.33 1.325 0 0.2 0.4 0.6 Mole Fraction of Methanol 0.8 1 1.2 y = -0.032x + 1.361 R = 0.9695

Figure 1

S NO. 1 2 3 4 5 6

Volume Of Methanol 0 2 4 6 8 10

Volume Of Ethanol 10 8 6 4 2 0
Table 2

Mole Fraction Of Ethanol 1 0.734893 0.50969 0.316011 0.14767 0

Mole Fraction Of Methanol 0 0.265107 0.49031 0.683989 0.85233 1

Refractive Index 1.3581 1.3552 1.3464 1.3401 1.3339 1.327

Reboiler temp(C) 69 73

Tzone1(C) 77 76

Tzone2(C) 64 64
Table 3

Tzone3(C) 63 64

RI Liq 1.3456 1.3490

RI Vap 1.3277 1.3277

1.Fenskes Equation
We calculated Nm from

avg = 1.69

Xd = 0.997 Xw = 0.365
Therefore Nm = 11.14

Mc Cabe Thiele Method

Figure 2 We used the equation: y=kx/(1+(k-1)x) to draw the VLE graph. Where k is the relative volatility, found using Antoines equation for saturated pressure of methanol and ethanol (at 68o C). From the graph we find that the number of stages is 10 . From
fenskes equation HETP = 2.4/11 = 0.218

Mccabe thiele method HETP = 2.4/10 = 0.24

NTU Calculation:

yB = Xw = 0.365 yD = Xd = 0.997 Again we use trapezoidal integration approximation to calculate the integral. We randomly select five point between yB and yD and extrapolate respective y* terms from the VLE graph we drew. We therefore got this table of values : x 0.365 0.3500 0.4800 0.5900 0.7100 0.8400 0.997 Table 4 Therefore upon integration, using trapezoidal integral approximation, we get NTU = 9.4684. Also, we know NTSM = 4 (given) Therefore, HTU = 1/NTSM = 0.25 And Z = HTU * NTU Y 0.3917 0.4842 0.6168 0.7150 0.8102 0.9015 0.9964 1/(y*-x) 8.1963 7.4491 7.3104 7.9978 9.9789 16.2549 50.7563

We therefore calculate Z = 2.36m It was given that Z ~ 2m, therefore, we see good correlation between experimental and known data.
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Precautions and Sources of Error 1. The test-tube should be immediately closed to avoid losses. 2. The RI meter should be properly cleaned prior to measuring RI of a sample. 3. There might be some error in the temperature measurement of the different zones. Zero errors, if any should be taken into account. 4. Before taking the sample, some amount should be purged in order to get rid of any impurity

Results and Discussion: Batch Distillation : We calculated the theoretical number of stages using Fenskes equation 11. Knowing that the actual number of stages was 13 Using McCabe-Thiele method, the number of theoretical stages for a similar plate column distillation unit is 10. We also calculated NTU to be 9.4684, and using this calculated height of the column to be 2.36m (which is very close to the actual value of ~2m). Conclusions : Through the experiment we find that both the graphical method and the analytical method for calculating the number of theoretical plates needed for the distillation are almost the same. Since the value of the relative volatility of the mixture is greater than one at both the ends, this implies that thermodynamically, the mixture does not form an azeotrope and hence the components can be separated. From the asymptotic behaviour of the graph of 1/(y-y*) versus mole fraction of y, it is evident that the area of the graph would increase as y increases to a greater separation. This means that NTU increases as the selectivity during the separation increases. This makes it clear that it becomes harder and harder to separate two streams as the purity of the separated streams increases.