 Distillation Column D1:

For the final purification of maleic anhydride, distillation column is used. Maleic
anhydride is separated from water. The distillation is operated at 1 atmosphere and
feed is entering the column at around 50° C.

The process design of the distillation column has been divided into the following steps:
a. Specify the degree of separation required: Set product specifications.
b. Select the operating conditions: Batch or continuous; operating pressure.
c. Compute distillate dew point and bottoms bubble point and the relative volatility of
constituent components
d. Select the type of contacting device: plates or packing.
e. Determine the stage and reflux requirements: the number of equilibrium stages.
f. Size the column: diameter, number of real stages.
g. Design the column internals: plates, distributors, packing supports.
COLUMN DESIGN:

a. Feed composition and Flow rates:

Component Mass Flow rate Molar Flow rate Mole Fraction
(kg/hr) rate (kmol/hr)
Maleic Anhydride 633.47 6.46 0.80
Water 28.08 1.56 0.199
Acrylic Acid 0.648 0.009 0.001(negligible)
662.198 8.03 1

b. Top Product Composition and Flow Rate

Component Mass flow Molar Flow Rate Mole Fraction
rate(kg/hr) (kmol/hr)
Maleic 9.5 0.097 0.015
Anhydride
Water 27.66 1.54 0.9841
Acrylic Acid 0.5832 0.00081 0.0009(negligible)
37.74 1.64

c. Bottom Product Composition and Flow Rate

Component Mass Flow Molar Flow Rate Mole Fraction
Rate(kg/hr) (kmol/hr)
Maleic 623.97 6.36 0.996
Anhydride
Water 0.42 0.023 0.0036
Acrylic Acid 0.0648 0.0009 0.00014(negligible)
624.45 6.38 1

Assumption:
 1. Binary Distillation of Water and Maleic Anhydride
2. Ideal gas behaviour of vapours

Column operates at 1 bar pressure. This is a binary distillation in which water is the more
volatile component and is removed at the top and desired maleic anhydride is removed at the
bottom. The vapour-liquid equilibrium data between water and maleic anhydride is generated
by thermodynamic calculations.

The vapour pressure of all the components can be found as a function of temperature using
Antoine equation
log10P = A - B/ (T+C); P is in bar and T is in Kelvin
Antoine constants:

Component A B C
Maleic 3.79916 1431.009 -101.093
Anhydride
Water 3.5596 643.748 -198.043

The vapor-liquid equilibrium data has been generated using Raoult’s law since it‘s not
available directly.

Raoult’s Law:

Where P – Total pressure/ operating pressure

yi – Gas mole fraction
xi – Liquid mole fraction
Pi – Vapor pressure
Total pressure is the sum of partial pressures (P.P) of individual components.
P = P.P1 + P.P2
Let V.P be the vapor pressure
P = V.P * x1 + V.P * x2
𝐵1 𝐵2
1.01325 = 10^ (𝐴1 − 𝑇+𝐶1 ) * x1 + 10^ ( 𝐴2 − 𝑇+𝐶2) * x2
𝐵1 𝐵2
1.01325 = 10^ (𝐴1 − 𝑇+𝐶1 ) * x1 + 10^ (𝐴2 − 𝑇+𝐶2 ) * (1- x1)
Where 1 denotes water and 2 denotes maleic anhydride
Steps to Generate VLE Data:

1. Take a number of liquid phase mole fractions i.e (0.1 to 1 here in this case). Substitute an
value in eqn. (3) along with the Antoine‘s constants and solve for T (Use solver for an error
function i.e. LHS – RHS of eqn. (3) set equal to zero by changing T) .Continue to do that for
remaining values and find T
2. Now we have a set of T values for a set of values. Calculate the vapour pressure of the
more volatile component at that temperature using the corresponding Antoine‘s constants
and eqn. (1). Then we get a set of vapour pressure values.

3. Then use the above vapour pressure value, the corresponding liquid mole fraction value in
eqn. (2) and solve for gas phase mole fraction value – y. we already know the total pressure-
1 bar. After solving we get the gas phase mole fraction y. Now we have a list of x and y values.
4. Then we calculate relative volatility (α)
α = {[y1/x1] / [(1-y1) / (1-x1)]}
Calculation of number of stages
The feed is saturated liquid i.e. q=1
Let R be the Reflux ratio

Where xf = xmin and α is 21.7

xf = 0.199
Therefore ymin = 0.84
xD = 0.9841
xB = 0.0036
D = 1.64 kmol/hr
B = 6.38 kmol/hr
Using Underwood method, minimum reflux ratio is found to be 1.26
Therefore reflux ratio R=1.25*Rmin
R = 1.57
Number of Plates:
Using Fenske’s Equation, we get minimum number of plates
𝑥1𝑑 𝑥2𝑏
ln⁡(( )( ))
𝑥2𝑑 𝑥1𝑏
Nm = d = distillate and b = bottom
ln⁡(𝛼)
Nm = 3

Actual Number of theoretical stages:

Using Kirk-Bride equation to calculate actual number of theoretical stages
𝑁 − 𝑁𝑚 𝑅 − 𝑅𝑚 0.566
= 0.75 × [1 − ( ) ]
𝑁+1 𝑅+1
Therefore N = 8
Column Efficiency = E = 0.48
Actual number of plates:
 𝑁−1
Taking reboiler as a stage,𝑁𝑎 = 𝐸
Na = 15

Column diameter calculation

Vapor flow rate is one of the important parameter that determines the column diameter. The
vapour velocity must be below that which would cause high pressure drop and excessive
entrainment.
The stepwise procedure for estimating the column diameter is explained below. As the molar
flowrates may not be constant, we have to calculate the column diameter at two different
places - top and bottom respectively.
1. Calculating vapour flow rate:
Vapour mass flowrate = (R+1)* flowrate of distillate
= (1.57+1) * 37.74
Hence, G’= 96.99 kg/hr
Calculation of vapour density
It can be found out by using ideal gas law,

where, P = 1atm = 101325 Pa

M = avg molecular weight of the distillate = 19.25
T = 388.16 K
R = 8.314 m3 Pa K−1 mol−1
After substituting the values, vapour density is found out to be 1.63 kg/m3

Selection of packings:
Since, maleic anhydride is an organic compounds, ceramic packings are not recommended as
organic liquids do not wet the ceramic packings. However, we can use either plastic or
metallic packings. Metallic packings are more durable and can withstand high temperatures,
whereas plastic packings are susceptible to thermal degradation. Here, temperatures are
around 410°C in the column. Hence, we select metallic packings.
Considering the cost factor, Pall rings are selected as the packings for distillation column.
The diameter of the packings should be less than 1/8th the column diameter.
Thus, we can initially guess a diameter of the packings to calculate the diameter of the
column and then check if the above criterion is satisfied or not and accordingly modifying the
calculations.
Packings: Pall Rings
Material of Construction: Metal
Nominal size: 16 mm
For these packings, the packing factor (Cf) = 70 (From Treybal)
Cd = 133.4
e = 0.93
ap = 341 m2/m3
5) Pressure drop at flooding:
Normally, ΔP/L for an atmospheric distillation column is around 400 to 600 N/m3.
Estimation of Column Height
Height equivalent to the theoretical plate as given by Peters and Timmerhaus (2003), is given
by,
HETP = 0.5 x T0.3
Thus, HETP = 0.4 m
Height of the packing = HETP x number of theoretical plates = 6 m
In order to account for loss of equilibrium at reflux entrance and feed entrance, we take factor
of safety as 1.2.
Hence, Height of Column = 1.2 x 6 = 7.2 m.
We have assumed, ΔP/L = 400N/m2/m
Thus, total ΔP = 2880 N/m2