PROCESS EQUIPMENT DESIGN

PART-1

FEBRUARY 1, 2018
GROUP-8
IIT KHARAGPUR
 INDEX
Serial Number Contents Page Number

1. Problem 2

2. Batch Distillation 2

3. Analysis of Feed 3

4. Single Stage Calculation 3

5. Constant Reflux Calculation 4

6. Matlab Codes 5

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 Problem
Ortho-xylene is contaminated with 1%w/w benzene and 1.5 w/w toluene. Design a batch distillation
process to bring down benzene content in the stream to below 0.25 w/w in batches of 3 𝑚𝑚3 feed. Design
the batch distillation column for the following options and comment on the best design:

1. Single state batch distillation

2. Constant Reflux Ratio
3. Constant Distillate Composition

Solution
Batch production is usually carried out in relatively standardised types of equipment, which can easily be
adapted and if necessary reconfigured to produce many other different products. It is particularly suitable
for low volume, high value products such as pharmaceuticals, polymers, biotechnological or other fine
chemicals for which annual requirement can be manufactured in few days or few batches in an existing
plant. The flexibility of the production arrangements can also cope with the fluctuations or rapid changes
in demand, which is often characteristic of products of this type. Other factors (Shah, 1992) which favours
batch processing are:

• increased global competition in the bulk chemicals sector

• need to produce customer specific products
• seasonal demands of certain products

Where small amounts of different products must be produced, it is usually more economically efficient to
manufacture them in a common facility such as multipurpose batch plant, rather than operating one plant
per product.

Batch Distillation
Batch distillation is, perhaps the oldest operation used for separation of liquid mixtures. For centuries and
also today, batch distillation is widely used for the
production of fine chemicals and specialised
products such as alcoholic beverages, essential oils,
perfume, pharmaceutical and petroleum products.
It is the most frequent separation method in batch
processes (Lucet et al., 1992). The essential features
of a conventional batch distillation (CBD) column
(Figure 1) are:

• A bottom receiver/re-boiler which is

charged with the feed to be processed and
which provides the heat transfer surface.
• A rectifying column (either a tray or packed
column) superimposed on the re-boiler, Figure 1: Conventional Batch Distillation (CBD)
coupled with either a total condenser or a partial condenser system.
• A series of product accumulator tanks connected to the product streams to collect the main and
or the intermediate distillate fractions.

Operation of such a column involves carrying out the fractionation until a desired amount has been distilled
off. The overhead composition varies during the operation and usually a number of cuts are made. Some
of the cuts are desired products (main-cuts) while others are intermediate fractions (off-cuts) that can be

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recycled to subsequent batches to obtain further separation. A residual bottom fraction may or may not
be recovered as product.

The main advantages of batch distillation over a continuous distillation lie in the use of a single column as
opposed to multiple columns and its flexible operation.

Analysis of feed:
Feed (F, Liquid)

%
ρ Initial feed
Component MW
w/w (mt/m3) m3 mt Kilo-moles

B 1 78.11 0.8787 0.03003554114 0.02639223 0.337885418

T 1.5 92.14 0.8636 0.04584106646 0.039588345 0.4296542761

0-x 97.5 106.16 0.88 2.92413911932 2.573242425 24.239284335

100 0.879741 3 2.639223 25.0068240291

𝑧𝑧𝐹𝐹,𝐵𝐵 = 0.01351172854

𝑧𝑧𝐹𝐹,𝑇𝑇 = 0.01718148116

𝑧𝑧𝐹𝐹,𝑂𝑂−𝑥𝑥 = 0.96930679029

Single Stage Calculation:

We simulated the single stage distillation column in Matlab but could find that the yield is very low. Every
at low pressure of around 0.1 bar, we could achieve a yield of around 79 percent. Code written in MATLAB
is attached at the end. The results of the code at various pressure are tabulated below:

Pressure Temperature Yield

0.1 bar 346 K 79.99 %

0.2 bar 364 K 75.61 %

0.3 bar 375.8 K 73.43 %

0.4 bar 384.6 K 71.80 %

0.5 bar 391.7 K 70.49 %

0.6 bar 397.8 K 69.39 %

0.7 bar 403.15 K 68.44 %

0.8 bar 407.89 K 67.599 %

0.9 bar 412.18 K 66.84 %

1.0 bar 416.11 K 66.16 %

1.1 bar 419.73 K 65.55 %

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Constant Reflux Calculation:
The total reflux start-up period ends with the column reaching its steady state i.e. the still and the column
top temperatures become steady. During this production phase, the column operates with a suitably pre-
set fixed reflux ratio so that the distillate purity from the initial to the end reduces from a high value to a
lower value and the collected distillate with average purity matches the target.

Number of Trays Yield

2 7.698570174188067e-01

3 9.630443337951142e-01

4 9.918644835198509e-01

5 9.944764863453053e-01

6 9.945040118606243e-01

7 9.944920212505404e-01

8 9.944860674006514e-01

Constant Distillate Calculation:

On reaching the required distillate purity, the start-up period ends. Product take off is started and a
constant composition product is collected by steadily increasing the reflux ratio until a specified amount
of distillate has been collected. During this period the column top temperature is kept constant by
continuously varying (increasing) the reflux flow. The operation ends when the reflux ratio has climbed to
some high value considered to be uneconomic.

After simulating N = 8 and finding reflux scheme, we could find that reflux ratio varies from 1.226220e+01
to 6.684029e+01 with a yield of 99.99 %. Since, the product concentration in the output was much less, we
had to move to a very high reflux ratio in every case.

Comments:
After qualitative determination the overall economics of the process, we can comment that a very high
yield of product is associated with a very reflux ratio, so we should move for a moderate yield of product
around 75 per keeping the reflux ratio normal.

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