Ministry of Higher Education and Scientific Research

Technical University in the North Region

Technical College in Kirkuk / Engineering
Department / Fuel and Energy

KIRKUK OIL TRAINING INSTITUTE

Laboratory Unit Operation

'Continuous Distillation Unite '

2017/ December / 18
Thursday at 9:00 AM

PRPARED BY
SARAH WALEED A.SATTAR
►The purpose of experiment:-
to separate the mixture into its component parts, or fractions, based on the
Differences in volatilities and boiling point.

►The theory of experiment :-

Continuous distillation, a form of distillation, is an ongoing separation in
which a mixture is continuously (without interruption) fed into the process
and separated fractions are removed continuously as output streams.
Distillation is the separation or partial separation of a liquid feed mixture
into components or fractions by selective boiling (or evaporation) and
condensation. The process produces at least two output fractions. These
fractions include at least one volatile distillate fraction, which has boiled and
been separately captured as a vapor condensed to a liquid, and practically
always a bottoms (or residuum) fraction, which is the least volatile residue
that has not been separately captured as a condensed vapor .

►The feed stock of experiment:

1- Ethanol (B.P=78 C , 50%)
2- Water ( B.P=100C , 50%)

►The product from experiment :-

1- The Distillate Ethanol.
2- The Water (residual material )

► EQUIPMENT OF THE CYCLE:-

• bottom boiler (3L), borosilicate glass execution.
• Quartz-sheathed electrical heater, P = 1600 W, code J1.
• Borosilicate glass distillation column, with 7 bubble plates, code C1.
• Reflux head and overhead condenser, borosilicate glass execution,code E1.
• Solenoid valves for the reflux ratio control, code EV1.
• borosilicate glass feed tank(5L), code D1.
• distillate collection tank(1L), borosilicate glass execution, code D2.
• bottom product collection tank(2L), borosilicate glass execution,code D3.
• Tube-tube heat exchangers E2, E3 and E4, stainless steel AISI 304execution.
• Feeding pump, Teflon head, 0-8.5 l/h, adjustable with signal 4-20 mA, code G1.
• Rotary blade vacuum pump, flow 4 m3/h, code G2.
• 6 double RTDs Pt 100, stainless steel sheath in AISI 316, code TI1,TI2, TI3,
TI4, TI5 and TI6 .
• electronic temperature indicators(6), range 0-199°C.
• timers (2) for the reflux ratio control.
• (15A) Resistor unit for the power Electrical control of the J1 .
• Cold trap, stainless steel AISI 304 execution, code S1.
• Connection lines and valves in stainless steel AISI 304-316 .
• Vacuum meter, range (0-1 bar), stainless steel execution in AISI 304, code PI2.
• Variable area electronic flow meter, range 20-250 l/h, output signal
4-20 mA, stainless steel AISI 304 execution, code FI1
• Pneumatic control valve, Cv = 0.32, stainless steel execution in
AISI 316, code FV1
• Pneumatic control valve, Cv = 0.32 stainless steel execution in
AISI 316, code PV1
• (2) Electro pneumatic converters 4-20 mA/ 0.2-1 bar
• Residual pressure electronic transmitter, range 0 - 1000 mbar,
output signal 4-20 mA, code PT1
• Digital microprocessor controller, PID type, input-output signals 4-20 mA

►The procedure of experiment:-

- There are more than one case to operate the device the two of them is
(Automatically way and handily way(under atmospheric temperature ).
In the KOT we learn who to operate distillation column by Automatically way.
In the first we full the D1 tank with mixture form (Ethanol and Water)
50% percentage to both , and then we close the (v2) valve to pass the mixture
To (G1)pump which drives the mixture in the form of batches (meals) as a result
of its frequency movement to send it to (E2 )where we get the initial heating of
the mixture. In the other way (J1)the heater (1600W) heating the distillation
tower and (C1) became Immersed in water.
each tray has 2 conduits, one on each side, called ‘down comers’. Liquid falls through the
down comers by gravity from one tray to the one below it. The flow across each plate is
shown in the above diagram on the right. A weir on the tray ensures that there is always
some liquid (holdup) on the tray and is designed such that the holdup is at a suitable height,
e.g. such that the bubble caps are covered by liquid.

Being lighter, vapor flows up the column and is forced to pass through the liquid, via the
openings on each tray. The area allowed for the passage of vapour on each tray is called
the active tray area. As the hotter vapour passes through the liquid on the tray above, it
transfers heat to the liquid. This continuous contacting between vapour and liquid occurs on
each tray in the column and brings about the separation between low boiling point
components and those with higher boiling points.

And through the( F11) we add water to measure the water flow rate at 250m/s the
water pass through the moved ball part to (E1)the top and reflex to maintain the
tower temperature , the light condense product outed from it and enters to heat
exchanger (E3)than we open the (V7)valve to strong the top production
in(D2)(that distillate and have low B.P and falls by ethanol).

In The end of process the water enters to heat exchanger E4 and Pour into the
bottom strong tank (D3) .

►Laboratory work on the device :-

The distillation device used generally consists of a column Distillation consists of seven
layers with inverted cups ,The single cup bubble is made of glass, The borosilicate is 2 m
high and 5 cm diameter.
Enter the article Feeder at the second layer of the tower and a glass top capacitor
To prepare the cooling needed to condense the rising steam to the top of the tower
Using tap water supplied by an external pump. The boiling boiler is located at the bottom of
the 3-liter tower Of borosilicate glass contains an electric heater envelope Its quartz thermal
capacity is (1600watts) as maximum for purpose Heat processing required for distillation
process in a tube A slug is next to the boiling boiler as the liquid is heated Located through
convection. Liquid level in The boiler controls it by controlling the level with survival
The pressure is constant in the boiling boiler and the output tank Lower. The tower also
contains an electromagnetic valve To control the ratio of the refractive fluid by dividing the
distillate to Liquid refer to the tower and tower overhead.
Dominates this The LED is used as a temporary timer A fixed time to open the valve and
convert the distillate to the output The tower has a specific time to close the valve and turns
distilled into liquid Check out the tower.
 The tower also has a feeding pump Pumping pumps are pumped at a rate of
Flow is between (0-8.4 L/hr) . It has a tower Distillation used on three tanks is a feeding tank
Cylindrical volume of (5L) is made of borosilicate glass And a cylindrical upper cylinder of
(1L) volume It is made of borosilicate glass and tank of the lower diameter Cylindrical shape
of (2L) size made of glass Borosilicate.
The tower contains a range of heat exchangers The double tube is made of stainless steel
Used for the purpose of heating and cooling the products as they are used for lifting
The temperature of the feeder is located down the tower next to the boiler Re-boiling as it is
connected to the boiler from the top Bottom and inside an open tube from top to pull distilled
The underside of the underside of the tower and its turn is dominant Controls the fluid level
in the Boiler Boiler within Limit required.
The second is used to cool the top output of the tower It is located after the return valve and
the third is used to cool the output Bottom of the tower.
The temperature is measured by six Sensors distributed throughout the tower. These sensors
Related to digital temperature measurements ranging from (199-0) Placed on the control
panel. It has a distillation tower On the refrigerant flow rate is between (0-250 L / hr) and
antenna control valve to control Cooling water flow rate for condensate and heat exchangers
And electric-to-air signal converters.
The control system consists of a personal calculator Computer and a connection between the
device and the computer (interface) which consists of an analog signal adapter to
Analog to Digital (ADC) (digital signal ), DAC (and vice versa)
It receives a signal connection from the dual-thermal (Thermocouple) and turns it into a
digital signal and sends it to The computer that has the control program is processed
An action within the control and signalling program Signal Exit the computer through the
connection unit to turn it off To an analogy signal, this signal can be projected on
Control valve, electric heater or feeding pump Discharge pump.
The control computer is equipped with Eng. (Pilot) To turn on the device that has many
windows And tools, through which the program can choose the layout of any
Variable with time and observation response can also be selected The control loop is
required and the switching mode is automatic To manual mode and vice versa, and the
program stores data And save them to the computer within a special file that includes
Variables in and out of the program, including all Time and date.
This device is equipped with (Multi-Loop PID) as shown below:
1-The first loop :-
Used to regulate the flow rate of cooling water supplied to the device by
Dominant and at a flow rate ranging from (0-250 L / h ).
2 –The second Loop 2:-
It is used to regulate the pressure of the tower by controlling and at a rate of (0 -1000 mbar).
3-The third loop 3 :-
Used to control the amount of nutrients by controlling the number Pulse injection pump.
4-The forth loop 4:-
is used to control the heating capacity fitted to the electric heater.

►Discussion :-

1- Why pump(G1)made from Teflon ?

TO prevent the calcification, it is frequency movement that make mix. Flowing
looks like batches (meals).

2- The change temperature amount to distillation process ?

Its depending on the components of the material, the higher the volatile material,
the lower the temperature.

3- Thermal gradient along the distillation tower ?

For the separation process the heat must be below the tower higher than the heat
of the highest tower.

4- thermal gradient of the ethanol concentration along the distillation tower ?

Whenever temperature increases mean that the amount of alcohol less because
the boiling point of it is 78 C.

5- The effect of change in Reflex quantity on the efficiency of the separation

process?
Whenever the reflex ratio has increased the recurrent increased efficiency of the
process and working to maintain the heat of the tower.

6- How we can control to the temperature of the column ?

By heater and quantity of the reflux .
7- Operating problems are possible in the tower distillation and treatment
Methods?

A) FLOODING:-
A phenomenon that the liquid level rise in the pipe layer where the course of the
descent of the liquid is not enough to drain fluid to down ,so thus make to
accumulate fluid in it and the liquid level rises to the top of the tower , also the
liquid can come out from the top. get as a result of high-vapour flow.
TO treatment this problems :-
1- We Reduce the temperature heated and thus reduce evaporation rates.
2- We Reduce flow of liquid by reducing the amount of material entering
and quantity.

B) WEEPING :-
A phenomenon that drops out of the liquid through the holes for the exit of
vapour.
They occur when the velocity of the liquid and its pressure are higher than the
steam, and this phenomenon reduces the efficiency of the layer and appears in
the layer holes
And Solved by raising evaporation rates.

C) ENTRAINMENT :-
A phenomenon that carries liquid droplets with high fumes.
They occur as a result of high vapour velocity.
AND treatment by reduction vapour speed is handled by controlling vapour
boiler work.
►Calculations
*relation between mole fraction for ethanol & density

Ethanol 0% 10% 20% 30% 40% 46% 50% 60% 70% 80% 90% 100%
Concentration
Relative 0.99 0.98 0.96 0.95 0.93 0.92 0.91 0.89 0.86 0.84 0.81 0.78
density

*equilibrium data for ethanol-water:

X 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Y 0.527 0.656 0.713 0.746 0.771 0.799 0.799 0.858 0.912 1

Xf=ethanol concentration in feed

Xd= ethanol concentration in overhead product(distillate)
Xw= ethanol concentration in bottom product(waste)
1.we take a sample from distillate and measure the density ( ρ ) and from mole fraction-density relation table
we take out( xd)
2. take a sample from waste and measure the density ( ρ ) and from mole fraction-density relation table we
take out( xw)
3.drawing equilibrium curve[x-y]from equilibrium data and draw 45 line.
4.calculate reflux value from below law:

L STOP TIME
𝑅= =
D 𝑆𝑇𝐴𝑅𝑇 TIME
NOTE:

*START TIME :is the time when the reflux valve is opened i.e. the light condensed
substance comes out to distillate tank.
*STOP TIME: is the time when the reflux valve is closed i.e. the light condensed substance
returned to distillation column.
5.determine the points[xd,xd],[xw,xw]&[xf,xf]and the point [0,xd/(R+1)] on the drawing.
6.draw top operationg line through the point[xd,xd] and the point [0,xd/(R+1)].
7.draw q-line by drawing vertical line from the point [xf,xf] to cut top operating line at
specific point for example (a).
8.draw bottom operating line from (a)point and the point [xw,xw].
9.draw number of stages between top & bottom operating line and the equilibrium curve.
10.calculate number of theoretical stages:

Number of plates=number of stages-1

number of theoretical plates
11.calculate separation efficiency= *100
number of actual plates
Xf= 0.6
Xd=0.8
Xw=0.02
Stope time= 10 sec , Start time = 4 sec
Type of feed= 90◦

= 7𝐧𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐭𝐡𝐞𝐨𝐫𝐞𝐭𝐢𝐜𝐚𝐥 𝐩𝐥𝐚𝐭𝐞𝐬

L 10 sec
𝑅= =
D 4 𝑠𝑒𝑐
R= 2.5
Xd/ R+1 = 0.8 /2.5+1 = 0.228

Number of stage =4
Number of plat= 4-1 =3
𝐧𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐭𝐡𝐞𝐨𝐫𝐞𝐭𝐢𝐜𝐚𝐥 𝐩𝐥𝐚𝐭𝐞𝐬
separation efficiency = *100
𝐧𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐚𝐜𝐭𝐮𝐚𝐥 𝐩𝐥𝐚𝐭𝐞𝐬

= 3/7 *100 = 43%

►Diagram :-
OPERATIONAL UNITS LABORATORY

Continuous Distillation Unit __mode: UDCA/EV

PSV1

V11
TI5 PI2
FC1 TI6
FT1
E1 V10
FI1
S EV1 PT1
V6
H2O PI1
D1
TI4 D1 PC1
FV1

E3
V1
PV1
V12
V2
V8 V7
TI3
D2
G1
V9 V13
V14
TI2 E4
D3
J1 H2O
V15

C1 E2

S1
TI1
V5
V3 V4 V16
G2