Polytechnic University of Puerto Rico

Chemical Engineering Department

CHE 5113-26

D E T E R M I N ATI O N O F TH E O R E T IC A L S TAG E S AN D TH E
OVERALL EFFICIENCY IN A
D I S T I LL ATI O N C O LU M N IN F U N C T I O N O F M I X T U R E
C O M P O SI T I O N S , F E E D P O SI T I O N , R E F L U X R ATI O , F E E D F L O W
R ATE AN D P O W E R

Wig b erto Re yes 6 63 3 9

Luz M. Surez 51641
Suheily Rivera 53923
L i n Y. M o r a l e s 5 2 3 5 6

Agenda

Objectives
Theory
Equipment

Schematic Diagram of Apparatus

Procedure
Data
Calculations
Safety

Objectives
Determinate the variation with boil-up rate of pressure drop over the distillation

column.
To use a Density Meter to determine mixture compositions.
Determination of the overall column efficiency.
Carry out a distillation at constant reflux ratio, varying top and bottom compositions

with time.
Investigate the steady state distillation of a binary mixture under continuous

operation.
Investigate the effect of varying the feed position under continuous operation.

Theory
Distillation is a process in which a liquid or vapour mixture of

two or more substances is separated into its component fractions

of desired purity, by the application and removal of heat

Theory
Types of Distillation Process

Flash Vaporization - is a single-stage

operation where in a liquid mixture is
partially vaporized, the vapor is allowed to
come to equilibrium with the residual
liquid, and the resulting vapor and liquid
phases are separated and removed from the
apparatus. It may be batch or continuous.

Theory
Types of Distillation Process

Differential Distillation - a feed mixture

of a given composition is placed in a
single stage separator and heated to
boiling. The vapor is collected and
condensed

to

composition of the

distillate.

The

remaining liquid

and the distillate are functions of time.

Theory
Types of Distillation Process

Continuous Rectification: Binary Systems - is a multistage,

countercurrent distillation operation. For a binary solution it is
possible by this method to separate the solution into its components,
recovering each in any state of purity desired.

Theory
Mc-Cabe-Thiele Method for trayed towers.

Estimates:

The number of equilibrium stages

The amount of reflux required

Assumptions:

The two components have equal and constant molar latent heats of vaporization.

Sensible enthalpy changes and heat of mixing are negligible compared to latent heats of
vaporization.

Heat losses are negligible.

The pressure is uniform throughout the column (negligible pressure drop).

Theory
Mc-Cabe-Thiele Method for trayed towers.

Theory

Rectifying Section

The material balance is:

(1)
(2)

For constant molar overflow:

Then:
(3)
*Equation 3 is the operation line for the rectification section

Theory
Rectifying Section

Reflux Ratio is the liquid entering the top stage, Lo, and its ratio to the
distillate rate.
(4)

if L0 is constant:
(5)
Since:
(6)
(7)

(8)

Theory
Rectifying Section

Combining equations 3, 7 and 8:

(9)

*Equation 9 is the most useful

form of the operation line for
the rectification section

Theory
Stripping Section

The material balance is:

(10)
(11)

*Equation 11 is the operation line for the

stripping section

Theory

Stripping Section

Boil-up ratio is the vapor rate leaving the reboiler and its ratio to the
bottoms product rate.
(12)

Since:
(13)

(14)

Theory
Stripping Section

Combining equations 11, 12 and 14:

(15)

*Equation 15 is the operation line

for the stripping section

Theory
The point of intersection of the two operating lines will help

locate the exhausting-section operating line.

Subtracting equations of operating lines of stripping and rectifying sections

will give:
(16)

The locus of intersection of operating lines(the q-line) is given by:

(17)

Theory
q-line

Theory
Equilibrium Data
Figure of Equilibrium Line for Ethanol/Water Mixture

Theory
To calculate the number of theoretical plates for a given

separation at total reflux, Fenske developed the following

formula:
(18)
Where:
n = number of theoretical plates
xA = mole fraction of more volatile component
xB = mole fraction of least volatile component
ABav = average relative volatility
(19)
Subscripts d, b indicate distillate and bottom respectively

Theory
The efficiency is given by:

(20)

Equipment
Diagram of UOP3CC Console

Schematic Diagram of Apparatus

Procedure
Perform the tower at total reflux.

Prepares the batch

Pump is calibrated

Adjust the power for start evaluating the pressure drop and the

boil up rate.

Will work at different power

Reading was taken of the pressure drop
Reading was taken of the boil up rate
Only for 0.5 KW sample was taken of xB and xD.

Procedure
For continuous distillation
Varying the reflux rate

RR=5:1
RR=9:3
Varying the power
Power = 0.5 KW
Power =0.9 KW
Varying the feed position
Feed Position; middle
Feed Position; bottom
Varying the flow rate
Flow rate = 1.0 L/h
Flow rate = 2.0 L/h
Varying the feed composition
Feed composition; 0.5 ethanol and 0.5 water
Feed composition; 0.7 ethanol and 0.3 water

Data
Variation of Column Pressure Drop

Calibration of the pump

@Total Reflux
Setting
20
40
60
80

Volume
(mL)

Time (s)

Power
(KW)
0.50
0.75
1.00
1.25
1.50
1.75

Volume
(mL)

Time
(s)

Pressure
Drop
(mm H2O)

Degree of
Foaming
On Trays

Data
@Total Reflux
RR

Power
(KW)

Feed
Position

Total
Reflux

0.50

_____

Flow
Rate
(L/hr)

xf

xd

xb

Volume
(mL)

Time
(s)

P
(mm H2O)

T1-T14

xd

xb

Volume
(mL)

Time
(s)

P
(mm H2O)

T1-T14

_____ ___

Variation of Reflux Ratio

RR

Power
(KW)

Feed
Position

Flow
Rate
(L/hr)

xf

5:1

0.50

Middle

2.0

0.5

9:3

0.50

Middle

2.0

0.5

Data
Variation of Power
RR

Power
(KW)

Feed
Position

Flow
Rate
(L/hr)

xf

5:1

0.50

Middle

2.0

0.5

5:1
0.90 Middle
Variation Feed Position

2.0

0.5

RR

Power
(KW)

Feed
Position

Flow
Rate
(L/hr)

xf

5:1

0.50

Middle

2.0

0.5

5:1

0.50

Bottom

2.0

0.5

xd

xb

Volume
(mL)

Time
(s)

P
(mm H2O)

T1-T14

xd

xb

Volume
(mL)

Time
(s)

P
(mm H2O)

T1-T14

Data
Variation Feed Composition
RR

Power
(KW)

Feed
Position

Flow
Rate
(L/hr)

xf

5:1

0.50

Middle

2.0

0.5

5:1

0.50

Middle

2.0

0.7

xd

xb

Volume
(mL)

Time
(s)

P
(mm H2O)

T1-T14

Calculus
Calibration
of the Pump

Exercise
A: Variation of Column

Pressure Drop

18
16
14
12
10

Flow Rate (L/hr)

Pressure Drop (mm H2O)

8
6
4
2

Setting

0.5

1.5

Boil-up Rate (L/hr)

2.5

Calculus
Exercise
B: Use of the Density Meter for

Determining Mixture Compositions

Exercise
C: Overall Column Efficiency

Fenske Equation (@Total Reflux )

Ethanol and Water Fraction

McCabe- Thiele
Rectifying Section
y
Stripping Section

*Repeat the same procedure for

determinate the mole fraction at the bottom
of the column.

Calculus
Exercise
C: Overall Column Efficiency

q- line

Specific Heat of the Mix

Heat of Vaporization

Intercept of q

Exercise C: Overall Column Efficiency

Safety
The major potential hazards associated with this particular

equipment are:

Electrical Safety

Hot Surfaces

Hot Liquids and Gases

Chemical Safety

Water Borne Hazards