Programme: BASC Process Engineering

Separation Processes I

SEPR2003

Assignment: Distillation Lab

Name Student ID #
Nakeyah Collins 77258

Jesse Manigro 85340

Contents
ABSTRACT..............................................................................................................................................3
AIM........................................................................................................................................................4
METHOD................................................................................................................................................4
TESTING THE PURITY OF METHANOL.................................................................................................4
COLLECTING DATA FOR CALCULATING FLOWRATES..........................................................................5
DCS SHUTDOWN OF THE DISTILLATION COLOUMN..........................................................................5
RESULTS................................................................................................................................................5
TABLE 1: RAW DATA COLLECTED DURING PURITY TESTING..............................................................5
TABLE 2: TIME THE SAMPLE CHANGED ITS DISTANCE FROM THE START AND STOP TIME FLOW.....5
FIGURE 1: DCS SCREEN SHOT.............................................................................................................6
FIGURE 2: DCS SCREEN SHOT 2..........................................................................................................7
TABLE 3: TEMPERATURE AT EACH RESPECTIVE TRAY IN COLUMN....................................................8
GRAPH 1: TRAY NUMBER VS TEMPERATURE.....................................................................................8
TABLE 4: EQUILIBRIUM DATA FOR METHANOL-WATER SYSTEM AT 1 ATM......................................9
CALCULATIONS....................................................................................................................................10
GRAPH 2: MOLE FRACTION METHANOL IN LIQUID VS IN VAPOUR..................................................11
FLOWRATE OF FEED.........................................................................................................................11
FLOWRATE OF TOP PRODUCT.........................................................................................................12
FLOWRATE OF BOTTOM PRODUCT.................................................................................................12
OVERALL MATERIAL BALANCE.........................................................................................................13
MATERIAL BALANCE FOR METHANOL.............................................................................................13
MATERIAL BALANCE FOR WATER....................................................................................................14
OVERALL HEAT BALANCE.................................................................................................................14
TABLE 5: CONTROLLER AND TRANSMITTERS PV, SP AND OUTPUT VALUES...................................14
DISCUSSION........................................................................................................................................16
SOURCES OF ERROR............................................................................................................................17
CONCLUSION.......................................................................................................................................17
RECOMMENDATIONS.........................................................................................................................17
ABSTRACT

For this lab, the aim was to determine the overall efficiency of the trays used to distil a
mixture of methanol and water and compare with it to literature. Temperatures were also
measured for both the feed components, and the cooling water.

The reflux ratio was found to be 0.67 based on the amount of top product being returned to
the column for purification in comparison to the amount of top product removed. The
efficiency of the column was also found to be low for the type of trays used in the distillation
column (was found to be 60%), which can also be attributed to the lack of steady state in the
column.
AIM – To determine the overall efficiency of the trays used to distil a mixture of methanol
and water and compare with the literature.

METHOD
 The power cabinet was turned on
 The control was changed from local to DCS
 The control was changed for manual to control
 The power to the reboiler cabinet was turned on
 Four (4) water valves (colour coded red) was opened
 The compressed air supply valve was opened
 A feed tray was selected and was opened to the selected valve of five (5)
 The Stripping section was then stabilized

TESTING THE PURITY OF METHANOL

 A measuring cylinder was used to take the sample which was filled approximately
three quarters of a 250 ml cylinder
 A thermometer was used to measure the temperature of the sample and the
temperatures were recorded.
 A hydrometer was used to measure the specific gravity by inserting hydrometer and
spinning it.
 Once the spinning had stopped and the hydrometer was ensured to not be touching the
insides of the measuring cylinder, the measurements were recorded
 A graph was used to interpolate/extrapolate data for the approximate purity of
methanol
COLLECTING DATA FOR CALCULATING FLOWRATES
 To be done for the top and bottom product accumulators and the feed tank, measure
the time for the start and stop time flow, then a ruler was used the measure the
distance between those points.

DCS SHUTDOWN OF THE DISTILLATION COLOUMN

 The reboiler was turned off
 The reflux flow was turned off
 The trays was emptied from the top coming down

RESULTS

TABLE 1: RAW DATA COLLECTED DURING PURITY TESTING

Sample Temperature/ Specific Gravity % Weight of
O
C CH3OH
1st reading
Feed 20.2 0.95 39
Top Product 28 0.8 99
Bottom Product 23 0.95 35

TABLE 2: TIME THE SAMPLE CHANGED ITS DISTANCE FROM THE START
AND STOP TIME FLOW
Sample Time (s) Distance (cm)
Feed 132 2.3
Top Product 230 3.5
Bottom Product 58 13.7
FIGURE 1: DCS SCREEN SHOT
FIGURE 2: DCS SCREEN SHOT 2
TABLE 3: TEMPERATURE AT EACH RESPECTIVE TRAY IN COLUMN
Tray number Temperature /O C
10 69.0
9 70.0
8 70.9
7 73.6
6 76.9
5 80.8
4 80.9
3 81.2
2 81.8
1 83.7

GRAPH 1: TRAY NUMBER VS TEMPERATURE

Tray number vs Temperature

90
80
70
Temperature/oC

60
50
40
30
20
10
0
0 2 4 6 8 10 12
Tray Number
TABLE 4: EQUILIBRIUM DATA FOR METHANOL-WATER SYSTEM AT 1
ATM
CALCULATIONS

From the distillate values recall reflux ratio, R = (LO/D)

 40/60 = 0.67

Using the equation

To Find y-intercept = 0.99/1.67 = 0.59

To be used as the enriching operating line elongated until it meets the xD = 0.99 from the x-
axis

Assuming q = 1 (saturated liquid) which is vertical line from the xF, feed line
where xW = 1 – xD
= 1- 0.99 = 0.01

From there we draw theoretical stages from the point (xd, xd) till they pass the point (xw, xw)
Overall Efficiency (EO) = {Number of Theoretical Stages/Number of Real Stages} * 100
EO = {6/10} *100
= 60%
 GRAPH 2: MOLE FRACTION METHANOL IN LIQUID VS IN VAPOUR

ol in vapour, y

Mole fraction methanol in liquid , x

KEY
0.01 – xW (brown line)
0.39 - xF (orange line)
0.99- xD (green line)

FLOWRATE OF FEED
Fluid volume removed from feed in 132 seconds
[(0.62 * π)/4] * 0.023 = 0.0065 m3

SG of the Feed = Density of the Feed / Density of the water

Density of the Feed= SG of the Feed * Density of the water
Density of the Feed= 0.95 *1000 kg/m3 = 950 kg/m3
Density of the Feed = Mass of Feed/ Volume of Feed
Density of the Feed * Volume of Feed = Mass of Feed
950 * 0.0065 = 6.1779 kg

Mass Flow Rate of Feed = (6.1779/132) * 3600

= 168.4893 kg/hr

FLOWRATE OF TOP PRODUCT

Fluid volume removed from top product in 230 seconds
[(0.162 * π)/4] * 0.035 = 0.0007 m3

SG of Top Product = Density of top product / Density of water

Density of top product= SG of Top Product * Density of water
Density of top product = 0.8 *1000
= 800 kg/m3

Density of Top product = Mass top product/ Volume top product

Density of Top product * Volume top product = Mass top product
800 * 0.0007 = 0.56 Kg
Mass top product = 0.56 Kg
Mass Flow Rate of top product= (0.56/99) * 3600
= 20.3636 kg/hr

FLOWRATE OF BOTTOM PRODUCT

Fluid volume removed from bottom product in 58 seconds

[(0.162 * π )/4] * 0.137= 0.0028 m3

SG of bottom Product = Density of bottom product / Density of water

Density of bottom product= SG of bottom Product * Density of water
Density of bottom product = 0.95 *1000
= 950 kg/m3

Density of bottom product = Mass of bottom product/ Volume of bottom product

Density of bottom product * Volume of bottom product = Mass of bottom product
950 * 0.0028 = 2.66 Kg
Mass top product = 2.66Kg
Mass Flow Rate of top product= (2.66/58) * 3600
= 165.1 kg/hr

OVERALL MATERIAL BALANCE (Basis: 1hr)

F=D+W
Where:
F = Feed
D = Distillate (top product)
W = Bottoms (bottom product)
168.4893 kg/h = 20.3636 kg/h + 165.1kg/h

MATERIAL BALANCE FOR METHANOL (Basis: 1hr)

Methanol in = Methanol out
Fxf = DxD + Wxw
Where:
xf = mass fraction methanol in feed.
xD = mass fraction methanol in distillate
xW = mass fraction methanol in bottoms
(0.35*168.4893) = (0.99*20.3636) + (0.35*165.1)
58.9712 = 20.16 + 57.785
58.9712 kg Methanol input = 77.945 Kg methanol output
MATERIAL BALANCE FOR WATER (Basis 1hr)
(0.65 *168.4893) = (0.01 *20.3636) + (0.0.65 *165.1)
109.5180= 0.2036+ 107.315

OVERALL HEAT BALANCE

Heat in = Heat out
Heat input =
Heat Input= (15.4* 30)/100
= 4.62 kJ/s

m*Cp*∆T = Heat Output

4.62 = (m*Cp*∆T) E103 + (m*Cp*∆T) E102
N.B for E103 the delta T = 3.1
For E102 the delta T = 2.2
4.62= (m *4.184*3.1) + (m * 4.184 * 2.2)
4.62 = 22.1752m
m= 0.208 Kg/s
Heat Output = (0.208 * 4.184 * 3.1) + (0.208 * 4.184 * 2.2)
= 4.61 KJ/s
Mass flow rate of cooling water = 0.208 Kg/s
Heat input = 4.61 KJ/s
Heat Output = 4.61 KJ/s

TABLE 5: CONTROLLER AND TRANSMITTERS PV, SP AND OUTPUT

VALUES
PV SP OUTPUT
PIC 105 8.9 8.9 65
LIC 103 27.3 27.3 60
FFIC 104 8.1 8.1 25
LIC 102 5.0 5.0 36.6
FIC 101 110.1 110.1 50.0
FIT 105(bottoms) 75.5
FIT 104(reflux) 8.1
FIT 103(top) 31.4
DISCUSSION

As the value of R increases, in this case it was a large value (0.67) the ROL rotates
downwards around (xD, xD). The SOL also moved down accordingly. The area between the
equilibrium curve and ROL is now larger, and we can draw larger triangles between the
operating lines. This means that there are now greater driving force for separation, which in
turns mean that lesser number of theoretical stages are required. As the reflux ratio or R = L /
D increases the operating line will move closer to the 45° line. Larger load will impact on the
duty of condenser and reboiler. When reflux ratio increases the number of stages of plate
decreases.

The Total reflux ratio can be defined as all reflux of distillate is fed to the distillation column
to achieve desired enrichment of the component. When it happens operating curves is
completely coincides with the 45° line. Hence number of trays is the lowest value. It will
increase the operating cost of distillation. Practically, no product is outcome because all the
distillate is reflux to the column.

A graph of tray temperatures vs tray no. was plotted. There was an overall decline in tray
temperature going up the column. The line for the decline to tray 5 was less steep than that
from tray 5 to 10. This was expected as the trays above this point where those for rectifying
where the trays below were enrichening trays.

Tray efficiency measures the performance of a distillation tray or trays against the maximum
theoretical performance Since to determine the overall efficiency of the trays used to distil a
mixture of methanol and water was found to be 60%, through the equation; Overall
Efficiency = {Number of Theoretical Stages/Number of Real Stages} * 100 equivalent to EO
= {6/10} *100, = 60%

Air condition makes the equipment cold so as the vapour travels up it condenses and travels
back downwards. This can be corrected by possibly turning off the ac to work in a room that
is at room temperature.
SOURCES OF ERROR
 Incorrect values for all input and outputs may be calculated since energy was not
added from the reboiler only but also from other sources such as from pumps.
 Inaccuracies in calculation may be due to incorrect measurements, poor start and stop
time management, human error when reading values such as specific gravity,
inaccurate height measurements etc.

CONCLUSION
 Efficiency was considered low for the type of trays in the column (60%)
 Mass flow input was not equal to the outputs due to errors discussed

RECOMMENDATIONS
 Do experiment at room temperature to avoid condensation
 Ensure reflux rate is adjusted to stabilize the column