THE EFFECT OF THE REFLUX RATIO

Olvar Andrés Pedraza, Juan Pablo González Yunda.

UNISABANA Universidad de La Sabana Código SNIES 1711, Campus del Puente del Común,
Km. 7, Autopista Norte de Bogotá. Chía, Cundinamarca, Colombia. Ingeniería Química. Facultad
de Ingeniería.
Laboratorio de operaciones de separación y nuevas tecnologías.

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1. Objectives.

General objective

Determine the effect of the reflux ratio in the power consumption and in the concentration of
ethanol produced when a reflux ratio of 2(L0/D) min is used and a 0.77 mol% of ethanol in the
distillate is desired.
Specific objectives
1. Using a concentration curve determine the alcohol concentration of the samples taken.
2. Analyze the behavior of the distillate composition by varying the reflux rate.
3. Determine the overall efficiency of the distillation column to be Used.

2. Introduction

Thermodynamic equilibrium of the ethanol-water mixture.

To determine the thermodynamic equilibrium, environmental conditions must be taken into
account, since in this case they will affect my process. The pressure in Bogotá that are above sea
level or at 760 mmHg.

Fig 1. Diagram x and ethanol-water

3. Materials and equipment.

 Beakers.
 Syringes.
 Ethanol.
 Water.
 UOP3CC colum.
 Refractometer.

4.Security conditions.
For this practice, the equipment called UOP3CC will be used, which allows the study of batch and
continuous distillation, the operation of the packed or plate column, operation at atmospheric or
vacuum pressure, azeotropic distillation and manual control, PID, PLC or computer process, the
operation of this tower requires various recommendations in order to avoid accidents, the most
important are listed below:

 Fluids: The equipment works with highly flammable substances.

 Temperature: The equipment works in high temperature conditions, so do not modify or
alter any part of the equipment while it is in operation.
 Storage: Flammable substances must be stored properly.
 Fire: Keep equipment and any flammable material required for use away from flame, very
high temperatures and sources of sparks.
 Electrical hazards: The equipment used must be connected to a current source of equal
frequency, otherwise, it may suffer electric shock or damage the equipment.
 Operation: Users must be informed of the correct procedure in case of an emergency. It is
the duty of the user to know and study the manual before the operation of the equipment,
besides being always under the supervision of his supervisor
 Chemicals: Vapors can be generated due to the toxic substances used. Work in well
ventilated areas.
5. Procedures
Concentration curve:

With the help of a test tube, place the quantity of ethanol indicated in table 1 on 8
1 volumetric balls of 10mL.

Bring each ball to capacity with distilled water.

2

Homogenize the mixture.

3

Using the breathalyzer, measure the refractive index of each prepared sample.
4

Record the data obtained in the results table 1.

5

Volumetric Ball Ethanol (mL)

1 1,5
2 3
3 4,5
4 6
5 75
6 90
7 10
8 0

Table 1. Amount of the calibration curve solutions.

VOLUMETRIC REFRACTIVE
FLASK INDEX
1
2
3
4
5
6
7
8

Table 1. Refractive indices of the concentration curve

At the end of the process of preparation and measurement of refractive indices, the molar fraction
data versus the refractive index will be plotted, in theory from this, a graph like the one shown
below should be obtained.
Illustration 1. Theoretical graph of molar fraction vs refractive index [2]

Efficiency of the column

1 In a bucket, add 5 L of ethanol and 5 L of water to obtain a 50% v / v solution of ethanol / water.

2 Through the filler cap, add the 10 L of prepared mixture to the reboiler

3 Turn off the reflux ratio timer on the console to configure the equipment to operate at full reflux.

Set the heat controller high and then reduce the heat as the reflux is introduced to provide constant
4 bubbling throughout the plate and total reflux.
5 Leave the device for 30 minutes to reach equilibrium conditions.

6 Actuate valve V3 so that all condensate is diverted to a measuring cylinder.

7 Take a small discard sample of 5 to 10 ml in an alternative container.

Divert the condensate into the measuring cylinder and use the stopwatch to measure 5 minutes to
8 collect a certain amount.

9 Maintain the liquid level in the condensate feed tube.

Partially open valve V3 and drain the condensate (in a separate measuring cylinder) from the reflux
10 system until a constant flow is obtained.

11 Start collecting samples and time at the same time, and collect a considerable amount.

12 Repeat the measurements 3 times.

13 Measure the refractive index of each sample with the breathalyzer and record it in the results table 2.

14 Following a similar procedure, take a sample from the bottom through V2.

15 Repeat this procedure every ten minutes until five samples are obtained from the top and bottom.

16 Record the temperatures T8 and T1 to calculate the average column temperature.

17 Repeat this procedure for several different boiling rates to cover the column's operating range.
In order to determine the overall efficiency of the column, it is necessary to know the number of
theoretical plates of the column given that:
N Theorists
E 0= ∗100 (1)
N Actual

Where N means number of dishes and E0 overall efficiency. To calculate the number of theoretical
plates you can apply the Fenske formula, which says:

n+1=
log ⁡[ ( XA
XB ) d(
XB
XA )
b]
(2)
log (∝ AB ) av
Where:

 n = number of theotic dishes

 Xa = molar fraction of the most volatile component.
 Xb = molar fraction of the least volatile component.
 d and b = indicate distillate and funds respectively.
 αav= It is the average relative volatility, this is calculated as follows α av¿ √ ∝d∗∝b (3)

For example for a sample where

(XA)d=0,75
(XB)d=0,25
(XA)b=0,43
(XA)b=0,57
αav=1,25

n+1=
log ⁡[ ( 0,75 d
0,57
0,25 ) ( 0,43 ) = 6,2
b]

log ( 1,25 )
n= 5,2

Boiling rate Refractive index X volatile X volatile Temperatures

component in the component in the 1 and 8
distillate funds
 Table 2. Data for the determination of column efficiency.

Separation of the mixture of ethanol water to different flow rates

In a bucket, add 5 L of ethanol and 5 L of water to obtain a 50% v / v solution of ethanol / water.
1

Through the filler cap, add the 10 L of prepared mixture to the reboiler
2

Turn off the reflux ratio timer on the console to configure the equipment to operate at full reflux.
3

Leave the device for 15 minutes to reach equilibrium conditions

4

Set the reflux controller with the desired values, shown in table 2.
5

Turn on the reflux valve (on the control panel).

6

Actuate valve V3 so that all condensate is diverted to a measuring cylinder.

7

Take a small discard sample of 5 to 10 ml in an alternative container.

8
Divert the condensate into the measuring cylinder and use the stopwatch to measure 5 minutes to collect a
9 certain amount.

Maintain the liquid level in the condensate feed tube

10
Partially open valve V3 and drain the condensate (in a separate measuring cylinder) from the reflux system until a
11 constant flow is obtained.

Start collecting samples and time at the same time, and collect a considerable amount.
12
Record the refractive index for the sample taken above. Similarly and preferably at the same time, take a sample
13 from the bottom through valve V2.

Repeat this procedure every ten minutes until five samples are obtained from the top and bottom.
14

Record the temperatures T8 and T1 to calculate the average column temperature.

15

16 Repeat this procedure for different reflux rates.

Reflux Rate mL / min Reflux Rate mL / min Time

Tabla 3. Datos recolectados con los cambios de reflujo.

With the data obtained in the last table, the analysis of how and why the compositions of the most
volatile component change during separation will be performed if the reflux is changed.
All the numbers indicated in the procedures that refer to parts of equipment are according to the
following illustration:
Illustration 2. Guidance map of the team for the development of the procedures.
REFERERENCES
[1] Armfield (2012).  continuous distillation column instruction manual uop3cc from http:// /uop3cc
%20manual%20-%20distillation.pdf/.
[2] Bench.(2010). continuous distillation column instruction manual. armfield instruction manual,
(31).