BATCH PROCESSES

MODULE 2 PART 4 – Process Design & Development

ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

LEARNING OUTCOMES DESIGN CALCULATIONS FOR BATCH

The key reasons for choosing PROCESSES
Identify
batch process In the production of an API (active
Explain The nature of batch sequencing pharmaceutical ingredient, the following batch
The batch sequencing recipe is used:
Demonstrate
calculations through an example - 500 kg of reactant A (MW = 100
The use of Gantt chart to kg/kmol) is added to 5000 kg of a
graphically represent a batch mixture of organic solvent (MW =
Explain 200 kg/kmol) containing 60%
sequencing or batch process step
scheduling excess of a second reactant B (MW
The concepts of non-overlapping, st – 125 kg/kmol) in a jacketed
1
Illustrate overlapping operations, and cycle reaction vessel (R-301), the reactor
Step
times is sealed.
- The mixture is stirred and heated
(using steam in the jacket) until the
KEY REASONS FOR SELECTING BATCH temperature has rise to 95°C.
PROCESSING - The density of the reacting mixture
 Small Production Volume is 875 kg/m3.
 Seasonal Variations in Product Demand - Once the reaction mixture has
 A need to document the production history reached 95°C, a solid catalyst is
of each batch 2 nd
added, and the reaction takes place
Step while the batch of reactants is
GUIDE QUESTIONS IN DESIGING BATCH stirred.
PROCESSES - The required conversion is 94%.
 Will there be more than one product made - The reaction mixture is drained
using the same equipment? from the reactor and passed
3rd
 What is the optimal size of the equipment? through a filter screen (SC-301)
Step
 How long must the equipment run to make that removes the catalyst and stops
each different product? any further reaction.
 What is the trade-off between economics - The reaction mixture (containing
and operability of the plant? API, solvent, and unused reactants)
is transferred to a distillation
column (T-301) where it is distilled
BATCH SEQUENCING under vacuum.
The order and timing of the individual - Virtually all of the unused reactants
processing steps and approximately 50% of the
What makes it challenging: 4th
solvent are removed as overhead
- The types of design calculations are Step
product.
very different for batch compared with - The end-point for the distillation is
continuous processes. when the solution remaining in the
- Batch calculations involved transient still contains less than 1 mol% of
balances, which are different from reactant. This ensures that the
steady state design calculations taught crystallized API, produced in Step
in much of the traditional ChE 5, meets specification.
curriculum. - The material remaining in the still is
pumped to a crystallizer (CR-301)
where the mixture is cooled under
CASE ANALYSIS: Batch production of an 5th & vacuum and approximately 60% of
Active Pharmaceutical Ingredient (API) 6th the API from Step 2 crystallizes out.
Step - The API is filtered from the
crystallizer and placed in a tray
dryer (TD-301) where any
entrapped solvent is removed.
- The dried API is sealed and
7th packaged in a packing machine
Step (PK-301) and sent to a warehouse
for shipment to the customer.

DESIGN CALCULATIONS FOR BATCH

PROCESSES
Solution strategy:
- In batch sequencing operations, the
time per step is the first to be
estimated
- We apply allowances for uncertainties in
the calculations and minor activities that
BATCH PROCESSES
MODULE 2 PART 4 – Process Design & Development
ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

do not have to be rigorously estimated Where to get or how to estimate these data? –
during preliminary design stage. Specifications sheets
Step 1: Reactor Vessel - Preheat
- The reaction vessel, which is used to Assuming the tank to be cylindrical and
preheat the reactants and subsequently run ignoring the volume of the bottom elliptical
the reaction, is designed first. head, the tank volume is
- For the batch size specified, the volume of
the liquid in the tank (V) and the volume 𝜋𝐷 𝐻
required for the reaction vessel (Vtank) are 𝑉 =
4
estimated.
- It is assumed that the vessel is But using the tank height to diameter ratio
approximately 60% full during operation
- A safety factor assumption 3𝜋𝐷
𝑉 =
4
Calculations involved (Reaction Vessel –
Preheat) 𝐷 = 1.689 𝑚
5500 [𝑘𝑔]
𝑉= = 𝟔. 𝟐𝟖𝟔 𝒎𝟑
875
𝑘𝑔 The height of fill is
𝑚
4𝑉
5500 [𝑘𝑔] 1 𝐻 = = 2.806 𝑚
𝑉 = = 10.48 𝑚 𝜋𝐷
𝑘𝑔 0.6
875
𝑚 Now solving for the area of heat transfer
= 2768 𝑔𝑎𝑙 (assume negligible heat transfer to the vapor
space)
Because reactors of this sort come in standard
sizes, a 3,000 gal (Vtank) reactor is selected. 𝐴 = 𝜋𝐷𝐻 = 14.89 𝑚

The heat-transfer characteristics of this vessel Substituting these values to the equation
are then checked. For a jacketed vessel, the derived from integration, time required for
unsteady-state design equation is: preheating the reactor is

𝑑𝑇 Δ𝑡 = 3288 𝑠 = 𝟓𝟓 𝒎𝒊𝒏
𝜌𝑉𝐶 = 𝑈𝐴(𝑇 − 𝑇)
𝑑𝑡
The additional time required for cleaning, filling,
- 𝜌 – the liquid density sealing, and inspecting to the vessel prior to
- CP – liquid heat capacity heating, and possible process issues that
- T – temperature of the liquid in the tank require a slower temperature ramp are roughly
(95°C desired) estimated.
- U – overall heat transfer coefficient from
the jacket to the liquid in the tank To be on the safe safe, we can assume 1 hr for
- A – heat transfer area of the jacket the other activites. Hence,
(cylinder surface) 𝑡𝑜𝑡𝑎𝑙 𝑡𝑖𝑚𝑒 𝑓𝑜𝑟 𝑝𝑟𝑒ℎ𝑒𝑎𝑡𝑖𝑛𝑔 = 𝟏. 𝟓 𝒉𝒐𝒖𝒓𝒔
- TS – the temperature of the condensing
steam Step 2: Reactor Vessel – Reaction
- It is assumed that the reaction of one
How about other forms of heating/cooling? – mole each of A and B to form one mole
heat exchangers of the product is 2nd-order and that the
rate constant is 7.09𝑥10 𝑚 /𝑘𝑚𝑜𝑙 ∙ 𝑠.
Normally, there is also a jacketed bottom to
such a vessel, but this added heat-transfer area The relationship for a batch reactor is
is ignored in this example for simplification.
𝑑𝐶
Integration of this equation yields: = −𝑘𝐶 𝐶
𝑑𝑡
𝑇 −𝑇 𝑈𝐴Δt - A and B are the two reactants, and A is
ln =−
(𝑇 − 𝑇 ) 𝜌𝑉𝐶 the limiting reactant

- T0 – initial temperature in the tank The standard analysis for conversion in a

(assumed 25°C) reactor yields:
- CP – 2,000 J/kg°C
- TS – 120°C (200 kPa saturated steam) 𝐶 = 𝐶 (1 − 𝑋)
- U – 300 W/m2°C 𝐶 = 𝐶 (𝜃 − 𝑋)
- Tank height to Diameter Ratio – 3/1 (so 𝑑𝑋
= 𝑘𝐶 (1 − 𝑋)(𝜃 − 𝑋)
H = 3D) 𝑑𝑡
BATCH PROCESSES
MODULE 2 PART 4 – Process Design & Development
ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

Step 4: Distillation of Reaction Products

- A material balance on the reactor at the
- 𝐶 = = 0.796 end of Step 2 yields the following

Since reactant B is present in 60% excess,

𝜃 = 1.6

The desired conversion, Xfinal = 0.94.

Integration of the dX/dt equation with t0 = 0 - Initially, the reaction mixture is heated
conc yields: to its boiling point of 115°C at the
operating pressure. Done by
1 𝜃−𝑋 condensing steam in a heat exchanger
ln = 𝑘𝐶 Δ𝑡 located in the still of the column.
𝜃−1 1−𝑋
The time to heat the mixture from 95°C (the
When all of the values inserted, temperature leaving the reactor, assuming no
heat loss in the filter) to 115°C is given by the
Δ𝑡 = 7082 𝑠 = 118 𝑚𝑖𝑛 = 𝟐 𝒉 equation with the following values:

For simplicity, the additional reaction time that 𝑑𝑇

occurs after the mixture leaves the reactor until 𝜌𝑉𝐶 = 𝑈𝐴(𝑇 − 𝑇)
𝑑𝑡
the catalyst is removed from the reacting
mixture has been ignored. - TS = 120°C
- U = 420 W/m2°C
Step 3: Draining Reaction Vessel and - 𝜌 = 875 kg/m3
Catalyst Filtration - A = 10 m2
- Modeled as a draining tank, significantly - Cp = 2000 J/kg°C
underestimate the actual required time
for draining and filtering. Solving for unknown time, we get
- In reality, experimental data on the
filter medium and inclusion of the exit 𝑡 = 4215 𝑠 = 𝟕𝟎. 𝟑 𝒎𝒊𝒏
pipe frictional resistance would have
to be included to determine the actual The distillation is performed using a still with
time for a specific tank. three theoretical stages (N = 3), a boil up rate
(V = 30 kmol/h), and a reflux ratio (R = 4.5).
Generally, the filter is the bottleneck in such a The volatilities of each component relative to
step. Here, a 2-in Schedule 40 exit pipe, with a the product are given as follows:
cross-sectional area of 0.00216 m2, is
assumed. 𝛼 = 3.375
𝛼 = 2.700
For a draining tank, the model is 𝛼 = 1.350
𝛼 = 1.000
𝑑𝑚 𝑑(𝜌𝐴 𝐻)
= = −𝑚 = −𝜌𝐴 𝑣
𝑑𝑡 𝑑𝑡 The solution methodology involves a numerical
integration.
- 𝜌 – density of the liquid in the tank
- At – cross-sectional area of the tank The overall material and component balances
- AP – cross-sectional area of the exit are given by:
pipe
- Vp – velocity of liquid in the exit pipe 𝑑𝑊 𝑉
- from Bernoulli’s – turbulent flow: − =𝐷=
𝑑𝑡 1+𝑅
(2gH)0.5 𝑑 𝑊𝑥 𝑑𝑊
=𝑥
The equation becomes 𝑑𝑡 𝑑𝑡

- W – total moles in the still

𝑑𝐻 (2𝑔) . 𝐴 . - 𝑥 𝑎𝑛𝑑 𝑥 – mole fractions of
=− 𝐻
𝑑𝑡 𝐴 component i at any time t (overhead
product and in the still)
Integrating t0 at H = 2.806 to find time yields:
The previous equations are solved in
Δt = 785 s = 𝟏𝟑 𝐦𝐢𝐧𝐬 conjunction with the sum of the gas phase mole
fraction equaling unity and the Fenske-
Resistance to flow (pipe and filter) is neglected Underwood-Gilliland method for
so to be on the safe side, this could be roughly multicomponent distillation
doubled or up to 30 minutes for this step.
BATCH PROCESSES
MODULE 2 PART 4 – Process Design & Development
ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

- Step 4 – 3.5 hr
- Step 5 – 2 hr
- Step 6 – 4 hr
- Step 7 – 1 hr

Total of 14.5 hours of operation

- Rmin and Nmin are the minimum values
for the reflux ration and the number of UNIQUE FEATURES OF BATCH
theoretical stages, respectively. OPERATIONS IN THE EXAMPLE PROBLEM
- Heating, reaction, and separation steps
Change of Still contents and Yields of P and S are unsteady state
with time - It is observed that no provision was
made to recycle the unreacted materials
which should be included to ensure
profitability

How to recycle in batch process?

- The overhead product from the batch
distillation contains unreacted raw
material and product in the solvent
which could be sent to a holding tank
and periodically mixed with a stream
Change in Composition of Still Material with containing pure solvent and just
time enough reactants A and/or B to make
up a single charge to the process in
Step 1.
- However, must be investigated
carefully to determine whether
unwanted side reactions take
place at higher product
concentrations.
- The other 60% of the product made in
the reactor or the mother liquor
(solution containing product to be
From the previous figure, the mole fraction of crystallized after some has crystallized
reactant B is seen to drop to less than the out) could be crystallized again to
specification of 0.01 (1 mol%) at a time of recover some of the valuable product.
approximately 2.3 h. - Achieved through 2nd and 3rd
cooling or crystallization step
This time, coupled with the heating time of 70.2 - Store the mother liquor from
minutes, gives a total of 3.5 h. several batch processes until a
sufficient volume is available
Step 5: Cooling and Crystallization of for another cooling or
Product crystallization step.
- Assumed that the times for each of
these steps have been determined
through laboratory-scale experiments. GANTT CHART SHOWING SEQUENCE OF
EVENTS FOR THE MANUFACTURE OF API
The amount of product crystallized is 80% of Gantt charts are tabular representations used
the product recovered from the still or 60% of to illustrate a series of tasks (rows) that occur
the 1057.5 kg produced in the reactor (634.5 over a period of time (columns). These charts
kg). Hence the total time for step 5 is 2 h. graphically represent completion dates,
milestone achievements, current progress, and
Step 6: Filtration and Drying so on.
- Assumed through lab-scale experiments Segregated through steps

The time required for filtration and drying is 4 h.

Step 7: Packaging
- Assumed through lab-scale experiments

The time required for packaging is 1 hr.

Summary and the Total time consumed in

the operation: Segregated through equipment
- Step 1 – 1.5 hr
- Step 2 – 2 hr
- Step 3 – 0.5 hr
BATCH PROCESSES
MODULE 2 PART 4 – Process Design & Development
ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

OVERALAPPING BATCH SEQUENCING

The shifting of batches backward in time. The
total time to process all the batches can be
reduced by starting a batch before the
preceding batch has finished.
Overlapping scheme – the limit of shifting or
overlapping process occurs when two time
NON-OVERALAPPING BATCH blocks in consecutive batches just touch each
SEQUENCING other
 In general, product is produced throughout - Assuming that cleaning, inspection, and
an extended period of time by using a charging times are included
repeating sequence of operations
 For example, the batch process described Backward shifting of batches, giving rise to
produces a certain amount of crystallized overlapping sequencing
API, namely 634.5 kg per batch.
 If it is desired to produce 5000 kg, then the
sequence of steps must be repeated

5000
≅ 𝟖 𝒕𝒊𝒎𝒆𝒔
634.5

Nonoverlapping scheme – The total

processing time is the number of batches The time to complete n batches using this
multiplied by the time to process a single batch. limiting overlapping scheme is given by:
𝑇 =𝑛 𝑡 𝑇 = 𝑇 = (𝑛 − 1) max (𝑡 ) + 𝑡
,…,

- TNO is the total time to process n - TO is the minimum total (overlapping)

batches without overlapping time and [(max (ti)] is the maximum
- Each batch having m steps of duration individual time step for the batch
t1, t2, tm process
- The subscript O denoting
From the example problem that is, overlapping will be dropped, and
T will be used as the total
8 (3.5 + 0.5 + 3.5 + 2 + 4.0 + 1.0) = 116.0 ℎ processing time from this point
on.
This notes that using the non-overlapping
scheme, the equipment is used infrequently, For the example,
and the total processing time is unduly long. 𝑇 = (8 − 1)(4.0) + (14.5) = 42.5 ℎ
However, such a scheme might be employed in
plants that operate only a single shift per day. The Limiting Case for Overlapping Batch
- In such cases, the production of a single Sequencing
batch might be tailored to fit an 8 to 10
h shift (14.5 h for this example), with the
limitation that only one batch would be
produced per day.

Although such a scheme does not appear to be

very efficient, it eliminates prolonged storage
of intermediate product and certainly makes
the scheduling problem easy. The use of overlapping sequencing reduces
the processing time significantly and makes
Nonoverlapping Scheme For The Example much better use of the equipment.
Problem - The equipment is operated for a higher
fraction of time in the overlapping
scheme compared with the
nonoverlapping scheme.

CYCLE TIME
The average time required to cycle through all
necessary steps to produce a batch.
Cycle time scheme – dividing the total time to
Do we have other options to optimize batch produce a number of batches by the number of
processing operations? – using recycle batches.
stream?
BATCH PROCESSES
MODULE 2 PART 4 – Process Design & Development
ChE 45 – Chemical Engineering Design 1
Lapeña, Don Kim S.

Equations become:
Non-overlapping scheme operating at cycle
time

𝑇 𝑛∑ 𝑡
𝑡 , = = = 𝑡
𝑛 𝑛

Overlapping scheme operating at cycle time

with small batches

𝑇
𝑡 , =𝑡 =
𝑛
(𝑛 − 1) max (𝑡 ) + ∑ 𝑡
,…,
=
𝑛

Overlapping scheme operating at cycle time

with number of batches to be produced is
large

𝑡 ≅ max {𝑡 }
,…,