Scribd
Upload
24 views3 pages

Batch Distillation Experiment Guide

Uploaded by

mudit
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
24 views3 pages

Batch Distillation Experiment Guide

Uploaded by

mudit
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

INDIAN INSTITUTE OF TECHNOLOGY KANPUR

Department of Chemical Engineering


Unit Operation Lab

Experiments Name: Batch Distillation

1. Scope:
When a liquid is to be separated into its components batch distillationis especially us
eful for small amount of material . A given batch distillation unitmay be used to
process many different mixtures. When there are several compounds (N) in the feed, one
batch column will suffice to separate all of them whereas N-1 continuous stills will be
required. When solids are present, batch distillation is moreconvenient than the
continuous one.

2. Objective:
(a) To observe the operation of batch distillation
(b) To determine the number o theoretical plates; to obtain an overall heat Balance.

3. Theory & Formulae:


In batch distillation, a batch of liquid is charged in the still and heated, and when
vaporshave reached the condensing system a portion of the condensed distillate is returned as
reflux. As top product take off is carried out , the material in the still becomes poorer in the
more volatile component (s) ,hence as the distillation proceeds the reflux ratio must be
increased to maintain the top-product quality, or sacrifice in sharpness of separation must be
made.
If the column is operated with a given mixture at total reflux, the
Fenske Underwood equation can be used to calculate theoretical plates for a binary
separation.
x p (1 − x s )
log
x s (1 − x p )
N +1 = (1)
log 

Where, α = Relative volatility


N = Theoretical plates
xp = Product concentration .
xs = Final still concentration ,mole fraction.

If the column is operated at a fixed know reflux ratio, then the product concentration varies
during the cycle. The variation of product concentration with amount of liquid remaining in
the still is given by
1
xs
S1 dxs
ln = 
S 2 x s ( x p − xs ) (2)
2

Where, S1= initial batch charge, moles


S2=residue in kettle at the end, moles
Relation betweenxp&xs can be obtained from X-Y diagram by plottingenriching section
operating line of slope determines by the fixed (L/V)ratio, with the lower terminus starting
with the initial still concentration and final line terminating with xs2. Based upon the
fixed no. of plates a relation between xp&xs can be calculated by the above procedure.
Equations (2) can then be integrated to give curves showing product and still composition
as functions of the percent of charge distilled.
(refer Perry’s Chemical Engineering Handbook,6th edition pg.13-82 to 13-85)

4. Materials and Apparatus:


The binary system used in the distillation experiment is ethanol-water. Analysis is carried out
by refractometer. The calibration curve of refractive index vs percent ethanol (0-100 %) must
be obtained at room temperature before hand. The reflux ratio can be adjusted by timer.
Other apparatus include sample bottles, thermometers or thermocouples.

5. Procedure:
5.1 Obtain the calibration curve for refractive index vs percent ethanol.
5.2 Charge a known amount of ethanol and water (50-50%) mixture in the still and start
heating.
5.3 Operate under total reflux (keeping the timer off) until steady state is reached obtained
distillate and bottoms (xp, xs) samples.
5.4 Take the necessary data – refractive index and specific gravityof reflux and residue,
cooling water rate, reflux rate and temperatureof inlet and outlet water stream in order
to be able to obtained a heat balance.
5.5 Record the weight (or volume) distilled vs time and record the weight of the still
sample.
5.6 Operate under a known fixed reflux ratio (say 5:1). Obtain samples at various times and
measure total amount of distillate collected.
5.7 Obtain RI and Specific Gravity of both Distillate collected and RI of bottoms.
5.8 Record the temperature of bottoms and distillate for heat balance.
5.8 Repeattherun at other known reflux ratio.

6. Results:
6.1 Plot calibration curve and equilibrium data for ethanol water system at 1.013 x 102
KN/m2total pressure.
6.2 Find number of theoretical stages using Fenske-Underhood equation and compare with
actual number of stages.
6.3 Set up material and energy balance equations.
6.4 Make a heat balance for the total reflux run and determine the % heat loss.
6.5 Plot moles of liquid remaining in the still vs distillate composition (s2vsxp) and compare
with results obtained from equation (2).
6.6 Comment on the sieve plates in the column.
6.7 Obtain a material balance on the last run and determine the % ethanol loss. Account for
all the ethanol.
7. Questions:
7.1 While setting up the equations, negligible column hold up is assumed. What happens if
the hold up is not actually negligible?
7.2 Can a packed column be used instead of sieve plate or bubble plate column for any
separation?
7.3 What must be done to maintain the distillate quality in a batch distillation column?
7.4 How will you set up the performance equation for the still if the assumption of constant
rate of distillate is not valid?
8. References:
8.1 Fenske, [Link]. 24, 482, (1932)
8.2 Smoker & Rose, Trans [Link]. 36, 285 (1940)
8.3 M. Van Winkle, “Distillation”, McGrow Hill Book Co. New York, (1967)
8.4 Perry’s Chemical Engineering Handbook,6th edition, Editors:[Link] and Don
Green.

Common questions

Powered by AI

To establish a material balance for the last run, measure the mass of the initial charge, the mass of the distillate collected, and the residue in the still. Subtract the mass of the collected distillate and residue from the initial charge to determine the unaccounted ethanol, indicating percentage loss. Calibration data from refractive index measurements will aid in quantifying ethanol concentrations accurately .

The suitability of packed columns versus sieve plate columns depends on several factors, including the feed composition, desired separation efficiency, and operational flexibility. Packed columns are often preferred for their lower pressure drop and efficiency in handling smaller liquid loads, while sieve plate columns may provide better performance for large-scale operations requiring precise control of the liquid-vapor contact .

When the constant rate of distillate assumption is invalid, the performance equation should account for variable distillation rates by incorporating time-dependent variables such as distillate flow rates and changing reflux ratios. This requires integrating additional data on concentration profiles and adjusting the model to reflect real-time distillation dynamics to maintain accuracy in predictions .

Batch distillation is advantageous for small quantities because it allows the processing of different mixtures in a single unit, unlike continuous distillation which would require multiple stills for different components. Additionally, batch distillation is more convenient in the presence of solids as it can accommodate variations in feed composition and can be adapted for processing without significant modifications .

In batch distillation at total reflux, the Fenske equation can be applied to calculate the number of theoretical plates needed for binary separation. It requires parameters such as relative volatility (α), the product concentration (xp), and the final still concentration (xs). The equation helps in determining the efficiency of the separation process under these conditions.

Observations on sieve plates should focus on aspects such as liquid distribution, plate weeping or flooding, and pressure drop across the column. Analyzing these factors helps in evaluating their performance and efficiency in vapor-liquid contact. Observations provide insights into whether the column is operating within optimal parameters or requires adjustments .

The refractive index calibration curve is significant as it correlates the refractive index to the ethanol concentration in the distillate. This curve is essential in analyzing the distillation process because it provides a straightforward method to determine the percentage of ethanol in collected samples. Accurate measurements from the curve ensure proper assessment of distillation progress and final product composition .

Adjusting the reflux ratio is essential to maintain distillate quality as the composition of the liquid in the still changes over time, becoming poorer in the more volatile components. Increasing the reflux ratio helps maintain a high separation efficiency and desired product quality, otherwise sharpness in separation might be sacrificed .

Assuming negligible column hold-up simplifies calculations, as the liquid hold-up is considered not to affect material balances significantly. If this assumption is inaccurate, it could impact the calculated number of theoretical plates, as hold-up can alter the vapor-liquid equilibrium and affect separation efficiency, leading to deviations from expected performance .

Integrating equation (2) involves using initial and final values of the liquid remaining to derive curves that map product and still compositions against the percentage of the batch charge distilled. These insights help understand how separation progresses over time, allowing for adjustments in process parameters to optimize efficiency and product quality .

You might also like