This action might not be possible to undo. Are you sure you want to continue?
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. distillation tends to be cheaper than other separation methods. 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. It is a very frequent separation process in the pharmaceutical industry and in wastewater treatment units. In this experiment. 2 . Hence. MOTIVATION : Distillation is the most widely used separation technique in the chemical and petroleum industry and is performed in either tray or packed columns . By operating the column under different conditions. A batch will be prepared in the heating coil reboiler prior to the start of the lab period. Many industries use distillation for critical separations in making useful products. and then distillate product will be drawn off. methanol and ethanol are separated using a three stage distillation column. Control of the column throughout experimentation will be achieved using a computerized control system. 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 . When running under reflux condition the efficiency of the distillation process greatly increases. The column will be started up under total reflux conditions. Its operation is based on differences in boiling points between the components being separated. Sample compositions will be determined using refractive index. αav = average relative volatility. When the relative volatility between the components being separated is high. its performance can be characterized. We calculate the number of stages by two different methods a) Fenske's equation: Nmin = number of theoretical stages at total reflux.
Fill approximately 2/3rd volume of the reboiler with a mixture Methanol and Ethanol. feed line. To do this.b) The graphical McCabe-Thiele Method can be used to determine the number of ideal stages and feed tray location. The test-tube should be immediately closed to avoid losses. EXPERIMENTAL PROCEDURE : Prepare a calibration chart of refractive index (RI) vs. 2 to 4 ml of top sample is collected in a test-tube after purging oft some quantity.mole fractions of components Methanol and Ethanol. Start water circulation through the Condenser andSwitch on the heating mantle and all control panels and allow the temperature in the distillation to rise. 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. and operating lines for the rectifying and stripping sections (all on the same axis). you make a plot showing the equilibrium curve. and then find answers by graphical construction. Count the number of actual plates in the column 3 . Determine the RI of the sample.
NTU is calculated using equation 5 and using the value.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 Fenske’sequation McCabe-Thiele graph also gives the number of theoretical plates and HETP is calculated using both the methods using relation given in equation 3. HTU is obtained by equation 4 4 .
8 1 1.365 1.325 0 0.4 0.14767 0 Mole Fraction Of Methanol 0 0. 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 0.36 1.683989 0.734893 0.2 y = -0.032x + 1.Calculations: S NO.361 R² = 0.345 1.85233 1 Refractive Index 1.35 1.3581 1.2 0.335 1.34 1.50969 0.3552 1.3464 1.355 Refractive Index 1.327 Table 1 Calibration Chart 1.6 Mole Fraction of Methanol 0.3339 1.9695 Figure 1 5 .265107 0.33 1.49031 0.3401 1.316011 0.
3456 1.50969 0.3490 RI Vap 1.734893 0.S NO.265107 0.3552 1.49031 0.3581 1.Fenske’s Equation We calculated Nm from αavg = 1.3401 1.365 Therefore Nm = 11.3339 1.69 Xd = 0.14 6 .14767 0 Mole Fraction Of Methanol 0 0.327 Reboiler temp(C) 69 73 Tzone1(C) 77 76 Tzone2(C) 64 64 Table 3 Tzone3(C) 63 64 RI Liq 1.85233 1 Refractive Index 1.3277 1.683989 0.3277 1. 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 0.997 Xw = 0.3464 1.316011 0.
218 Mccabe thiele method HETP = 2. From the graph we find that the number of stages is 10 . From fenske’s equation HETP = 2.4/11 = 0.Mc Cabe Thiele Method Figure 2 We used the equation: y=kx/(1+(k-1)x) to draw the VLE graph.24 7 . Where k is the relative volatility.4/10 = 0. found using Antoine’s equation for saturated pressure of methanol and ethanol (at 68o C).
4800 0.9978 9. We therefore got this table of values : x 0. we get NTU = 9. using trapezoidal integral approximation.9964 1/(y*-x) 8. We randomly select five point between yB and yD and extrapolate respective y* terms from the VLE graph we drew.3104 7.8400 0.4842 0.NTU Calculation: yB = Xw = 0.365 0. we see good correlation between experimental and known data. 8 . Also.365 yD = Xd = 0.7150 0.9789 16.4684. therefore.2549 50.6168 0.3917 0. HTU = 1/NTSM = 0.997 Again we use trapezoidal integration approximation to calculate the integral.3500 0.36m It was given that Z ~ 2m.8102 0.7100 0.1963 7.7563 We therefore calculate Z = 2.9015 0.5900 0.997 Table 4 Therefore upon integration.4491 7.25 And Z = HTU * NTU Y 0. we know NTSM = 4 (given) Therefore.
Before taking the sample. Since the value of the relative volatility of the mixture is greater than one at both the ends. Knowing that the actual number of stages was 13 Using McCabe-Thiele method. This means that NTU increases as the selectivity during the separation increases. 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 Fenske’s equation – 11. Zero errors.4684. the number of theoretical stages for a similar plate column distillation unit is 10. This makes it clear that it becomes harder and harder to separate two streams as the purity of the separated streams increases. We also calculated NTU to be 9. the mixture does not form an azeotrope and hence the components can be separated. 4. The test-tube should be immediately closed to avoid losses. it is evident that the area of the graph would increase as y increases to a greater separation. 9 . 2. if any should be taken into account.Precautions and Sources of Error 1. and using this calculated height of the column to be 2.36m (which is very close to the actual value of ~2m). this implies that thermodynamically. The RI meter should be properly cleaned prior to measuring RI of a sample. 3. From the asymptotic behaviour of the graph of 1/(y-y*) versus mole fraction of y. 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. There might be some error in the temperature measurement of the different zones.