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Distillation is a process in which a liquid or vapor mixture of two or more substances is

separated into its component fractions of desired purity, by the application and removal of heat.
From this experiment, we had study the separation split as function of reflux ratio. Moreover, we
can calculate the number of theoretical plates, by plotting the graph from the result given and
obtain. We started this experiment as we boiled the mixture of methanol-water first and then both
element would turn into vapor and then goes up to the top of the distillation column where there
are differences of boiling point between methanol and water. The water turns back into liquid
before it reaches the top of the distillation column and then it flows back to the bottom of
distillation column. This experiment had separated two liquid dilute together by boiling the
mixture of liquid which its element have different boiling point. The result of the experiment is
based on the reflux ratio of 1:1 and 2:1 after that the number of theoretical stages is calculated.
As conclusion the objective of the experiment is achieved.

 


Distillation is the most common separation technique which separate two or more liquid
compounds on the basis of boiling-point differences. The boiling point of a liquid is the
temperature at which the liquid and vapor phases are in equilibrium with each other at a specified
pressure. Therefore, the boiling point is the temperature at which the vapor pressure of the liquid
is equal to the applied pressure on the liquid. When a pure liquid is boiled at fixed pressure, the
temperature remains constant until all the liquid has vaporized. When a solution is boiled at fixed
pressure, the composition of the vapor usually differs from that of the liquid, and the change in
liquid composition during boiling changes the boiling point

Reflux refers to the liquid which is recycled back to the top of the column. The Reflux ratio is
also the quantity of liquid reflux per unit quantity of product removed from the process unit, such
as a distillation tower or extraction column. The condensed liquid that is removed from the
system is known as the distillate or top product.
The hottest tray is at the bottom of the column and the coolest tray is at the top. At steady state
conditions, the vapor and liquid on each tray is at equilibrium. Only the most volatile of the
vapors stays in gaseous form all the way to the top. The vapor at the top of the column then
passes into the water-cooled condenser, where it condenses into a liquid. The process continues
until all of the most volatile components in the liquid feed boil out of the mixture.

›

1.c To study the separation split as function of reflux ratio

2.c To calculate the number of theoretical plates.


!" # 

1.c Automated Distillation Pilot Plant

2.c Compress Air supply
3.c Methanol
4.c Water

°

Êetting the continuous distillation plant

1.c Valves
V2,V3,V5,V8,V9,V14,V15,V10,V11,V13,V12,V17,V20,V21,V22,V23,V24,V25,V26,
V28, and V29 is being shut off.
2.c Valves V1, V4, V6, V7, V16, V27, V19 and V18 are opened.
3.c All switches set to 0
4.c The plant connected to the electrical mains
5.c The reducer unit connected under the electrical board to the 6-bar compressed air unit and
the two reducers adjusted respecting the pressure reported under the label ( the reducer on
the left must be adjusted to 6 bar, the one on the right to 1.5 bar)
6.c The plant connected to the water system as in the provided diagram
7.c The water output connected to a waste pipe
8.c The switch AUTO-PC turned to $
9.c The AUTO-DIFF switch connected
10.cThe run switch checked is off
11.cThe ³Êtart´ pushbutton is pushed
12.cThe 2nd loop FIC1(controller no. 1) selected with pushbutton ÷
13.cThe control 2n loop FIC1 (controller no.1) is set to manual mode with pushbutton m


(red led on)
14.cThe control valve FV1 (FIC1) is opened and set the flow rate at
 ( select the
indication › with pushbutton   and increase or decrease the flow rate)
15.cThe set point adjusted ( push the button ° increase of decrease its value with at 
and set the 2nd loop FIC1 to automatic mode with push button m

 (green led on)
16.cWait until the container of the preheating resistor J1 is filled by turning on the pump G1.
17.cThe set point were adjust at 55 oC(push the button °)
18.cÊet the control loop TIC1 to automatic mode with pushbutton M/A/C (green led on)
select the 1st loop (TIC1) of controller no.1.
19.cThe resistor J1 were set to 1.
20.cThe boiler of column C1 were filled with a binary mixture (methanol-water) until the
electrical resistor J2 is completely plunged by switch the pump G1 to the position 1.
21.cThe pump G1 switched off to 0 when the boiler C1 is filled.
22.cAt 2nd loop of controller no.2 with the indication Out with pushbutton Ind the value is set
at 30.
23.cThe switch of the resistor J2 set to 1.
24.cThe mixture is taken to the boiling point.
25.cLet the column to total reflux for about 5 minutes (until the temperature TI6 is not
stabilized).
26.cTo select the reflux ratio (1:1), set the timer ³ÊTART´ at 2 sec and the timer ³ÊTOP´ at
20 sec.
27.cÊet switch ³Reflux´ to 1
28.cTo change the reflux ratio, select different times of the timers
 29.cThe temperatures, along the column, give the composition in different positions of the
column.
30.cTake the temperature at TI3 and TI6 at first drop of the distillate at the distillate product
tank D4.

Halting the Plant

1.c The switch of the pre-heating resistor J1 set to 0

2.c The pump G1 stopped
3.c The column exhausted
4.c The switch of the heating resistor J2 set to 0
5.c The ³Reflux´ switch set to 0
6.c After about 3-5 minutes close the water inlet to the top condenser (take the output of the
control loop FIC1 to 0)
7.c The container of the distillate D4 is exhausted
8.c The tank D2 is exhausted
9.c The tank of the high boiling D3 is exhaust
10.cThe water to the top condenser is closed













?%

?&%'?((

#    ?%

Feed (liter / hour) 6.9769

Xf (fraction) 0.3

TI3 (ÛC) 84.3

TI6 (ÛC) 64.1

?&%'?(

#    ?%

Feed (liter / hour) 6.9769

Xf (fraction) 0.3

TI3 (ÛC) 85.1

TI6 (ÛC) 63.4

#    )%

XD 0.59

XB 0.105

D (liter / hour) 36.8

B (liter / hour) 18.1

à 

BAÊIC DIÊTILLATION EQUIPMENT AND OPERATION

Main Components of Distillation Columns Distillation columns are made up of several

components, each of which is used either to tranfer heat energy or enhance materail transfer. A
typical distillation contains several major components:

1.c a vertical shell where the separation of liquid components is carried out
2.c column internals such as trays/plates and/or packings which are used to enhance
component separations
3.c a reboiler to provide the necessary vaporisation for the distillation process
4.c a condenser to cool and condense the vapour leaving the top of the column
5.c a reflux drum to hold the condensed vapour from the top of the column so that liquid

(reflux) can be recycled back to the column The vertical shell houses the column internals and
together with the condenser and reboiler, constitute a distillation column. A schematic of a
typical distillation unit with a single feed and two product streams is shown below:

Basic Operation and Terminology

The liquid mixture that is to be processed is known as the feed and this is introduced usually
somewhere near the middle of the column to a tray known as the feed tray. The feed tray divides
the column into a top (enriching or rectification) section and a bottom (stripping) section. The
feed flows down the column where it is collected at the bottom in the reboiler.
Heat is supplied to the reboiler to generate vapour. The source of heat input can be any suitable
fluid, although in most chemical plants this is normally steam. In refineries, the heating source
may be the output streams of other columns. The vapour raised in the reboiler is re-introduced
into the unit at the bottom of the column. The liquid removed from the reboiler is known as the
bottoms product or simply, bottoms.

The vapour moves up the column, and as it exits the top of the unit, it is cooled by a condenser.
The condensed liquid is stored in a holding vessel known as the reflux drum. Êome of this liquid
is recycled back to the top of the column and this is called the reflux. The condensed liquid that
is removed from the system is known as the distillate or top product.

Thus, there are internal flows of vapour and liquid within the column as well as external flows of
feeds and product streams, into and out of the column.

 % 

We can study the separation split as function of reflux ratio and we can also calculate the number
of theoretical plates

?& 

 c Jacqueline I. Kroschwitz and Arza Êeidel (2004). Kirk-Othmer Encyclopedia of Chemical

Technology (5th ed.). Hoboken, NJ: Wiley-Interscience. Retrieved on March 13, 2011
from K

 
 
2 c Perry, Robert H. and Green, Don W. (1984). °erry's Chemical Engineers' Handbook, 6th
Edition. McGraw-Hill. 
Ô c Kister, Henry Z. (1992). àistillation àesign, 1st Edition. McGraw-Hill. Retrieved on
March 13,2011.