Example SPC-2: Effect of Increasing Column P

on a C3 splitter
Consider the separation of a mixture of 50 mol/hr of propane C3H8(1) and 50 mol/hr
propene, C3H6(2) at a pressure of 1.1 bar and a bubble point feed temperature of
230 K (-43oC).Under these conditions, P01=930.5 mm and P02=724.1 mm
and a 1/2=1.285. Setting the recoveries (percentage) of the two components at
2=0.99 and 1=0.01, we find out that minimum number of trays, Nm is:

 0.99 0.99 
Nm  ln  .  / ln  1 / 2  36.65
 0.01 0.01 
Now, if the pressure is increased tenfold to P=10.94 bar, we have a bubble
point feed temperature of 300K (27oC) and P01=8975.6 mm, and P02=7458.5 mm
And separation factor, 1/2=1.203. As a result, for the same recoveries,
the separation becomes more difficult and the minimum number of
trays increases to Nm=49.72.

Separation factor 1/2 has to larger than 1.0 for good separation !!
 Time Out Session SPC-1 - Setting
Column Pressure for a C3 splitter
A liquid mixture containing 50 mole % propane (C3-), 50 mole % propene (C3=) is fed at a
rate of 1000 mole/h to a distillation unit. Estimate the operating pressure for a column
separating C3- from C3=, assuming cooling water at 30oC is available for use.

What would be the top temperature of the column?

TABLE 3: BOILING POINT (oC) OF COMPOUNDS AT PRESSURES BETWEEN 1

atm AND 40 atm
 Flowsheeting: Process Conditions (T and P levels)

non-condensibles

Ptop,C1
R1 F1 =1bar Ptop,C2=1.5bar
1.1 bar
(feed from Preactor: 40 bar C1
ambient Treactor: 250°C Pflash: 3 bar
conditions) (from flash Ptop,C2=1.8bar
calculations) C2
Pbot,C1=
1.2bar
• Set column pressures based on product
bubble points C3
Pbot,C2= Ptop,C2=
• Negative pressure gradient downstream? 1.7bar 2.0bar
• Rearrange/Readjust pressure levels to achieve positive
gradient and facilitate flows? heavies
 Flowsheeting: Process Conditions (T and P levels)

non-condensibles

Ptop,C1=
R1 F1 2.2bar Ptop,C2=2.0 bar
1.1 bar C1
(feed from Poperation: 40 bar
ambient Toperation: 250°C Ptop,C2=1.8bar
conditions)
C2
Pbot,C1=
2.4 bar
• Rearrange/Readjust pressure levels to achieve
positive gradient and facilitate flows. C3
Pbot,C2= Ptop,C2=
• Check that specs and flowrates are met.
2.2 bar 2.0bar
Recalculate Ps and Ts as necessary.
 Flowsheeting: Process Conditions (T and P levels)

non-condensibles

Ptop,C1=
R1 F1 2.2bar Ptop,C2=3.0 bar
1.1 bar C1
(feed from Poperation: 40 bar
ambient Toperation: 250°C 1.5 bar
conditions)
C2
Pbot,C1=
2.4 bar
• AVOID ROUND TRIPS!
(unnecessary ups and downs in Pressure C3
Pbot,C2= Ptop,C2=
and Temperature levels 3.5 bar 2.0bar
 For our VC production
1st column to separate HCl (overhead).
For column P equal 1 atm, the condenser has to operate at
low temperature (-84.8oC), expensive refrigeration.
Patent suggest P=12 atm, so outlet from condenser
will be -26.2oC.
The bottom product will be at bubble temp of 93oC.
Higher pressure is avoided too prevent operation
near critical regions.
This bottom temperature will allow the used of lower pressure steam (lps)
for reboiler.
Feed will enter at bubble point, so the T is 6oC at 12 atm.
Higher feed T (e.g. 30oC), will introduce vapor to column that will
increase condenser duty. Not a good idea.
 For our VC production

2nd column to separate VC (overhead).

For P=4.8 atm, the condenser outlet is at 33.1oC.

So could use CW at 25oC

The bottom product will be at bubble temp of 146oC and could use
medium pressure steam (mps) for reboiler
 With separation system

Fig 4.6

There may be other, possibly better alternative configurations, as discussed in

(Chapter 5) later.
Synthesis Tree
 Preliminary Process Synthesis
Process Synthesis involves:
 Selection of processing mode: continuous or batch
 Fixing the chemical state of raw materials, products, and by-products,
noting the differences between them.
 Process operations (unit operations) - flowsheet building blocks
 Synthesis steps:
 Eliminate differences in molecular types (chemical reaction)
 Distribute chemicals by matching sources and sinks (mixing &
recycle)
 Eliminate differences in composition (separation)
 Eliminate differences in temperature, pressure and phase
 Integrate tasks (combine tasks into unit operations)
 Eliminate differences in temperature,
pressure and phase

In other words, identify all T, P and phase change to

determine the required utility systems…
How do we set the T and P?
General Guidelines for Range of Process Operations

Sensible operating range to avoid severe processing difficulties

Parameter Range Rationale

Most equipment can go up
Pressure Between 1 to 10 bara to 10 bar without increase
in capital cost
Limited by utilities
Temperature 40 to 250ºC available: cooling water @
(30ºC) and steam between
40 to 60 bar, to 260ºC
 Sensible Pressure Range
The decision to operate outside the range of 1 to 10 bar usually is a
compromise between performance and the capital and operating costs of
process equipment.

Conditions Justification Penalty

e.g. in gas operations,
increased density,
lower volume, smaller more costly,
P higher than 10 bar equipment (for the thicker-walled
same residence time), equipment needed
higher quality heating
media (steam)
Larger equipment.
Prevent degradation Need special
P lower than 1 bar of heat-sensitive equipment
materials construction for
vacuum operations
 Sensible Temperature Range
Temperature
• Several critical temperature limits apply to chemical processes.
• At elevated temperatures, common construction materials
(primarily carbon steel), suffer a significant drop in physical
strength and must be replaced by more costly materials (see next
example SPC-1).
 Effect of Temperature Excursions
Example SPC-1
The maximum allowable tensile strength for a typical carbon steel
and stainless steel, at ambient temperature, 400oC, and 550oC is
provided below (from Walas [1])

Tensile Strength (bar) of Material

At Temperature Indicated
Temperature Ambient 400oC 550oC
Carbon Steel (grade 70) 1190 970 170
Stainless Steel (Type 1290 1290 430
302)

Determine the fractional decrease in the maximum allowable tensile

strength (relative to the strength at ambient conditions) for the
temperature intervals: (a) ambient to 400oC and (b) 400oC to 550oC.
 Effect of Temperature Excursions
Answer to Example SPC-1
a. Interval ambient to 400oC:
Carbon Steel: (1190-970)/1190 = 0.18
Stainless Steel: (1290-1290)/1290 = 0.0
b. Interval 400oC to 550oC:
Carbon Steel: (970-170)/1190 = 0.67
Stainless Steel: (1290-430)/1290 = 0.67
Example SPC-1 shows that carbon steel suffers a loss of 18% and the stainless steel suffers
no loss in tensile strength when heated to 400oC. With an additional temperature increase
of 150oC to 550oC, the stainless steel suffers a 67% loss while the carbon steel suffers an
additional 67% loss in strength. At operating temperatures of 550oC, the carbon steel has a
maximum allowable tensile strength of about 15% of its value at ambient conditions. For the
stainless steel, the maximum allowable strength at 550oC is about 33% of its ambient value.
Conclusion: Carbon steel is unacceptable for service temperatures above about 400oC, and
that the use of stainless steel is severely limited. For higher service temperatures, more
exotic (and expensive) alloys are required and/or equipment may have to be refractory
lined.

A decision to operate above 400ºC must be justified

 Temperature Excursions – Effects
on Operating Cost

All other equipment being equal (T & P).

However, avoid excursions in T and P,
150
but aim high T, rather than low T
(due to higher cost to operate at lower T.
Relative Cost/Btu

Cooling
100
Heating

50

-150 Room 400°F

Temperature

Cost of temperature excursions from [Rudd 72]

 T(°C)

Flue Gas 300°

Hot Oil

HP Steam 250°
Typical Utility
Medium 200°
Levels Pressure
(MP) Steam Lower 150°
Pressure
(LP) Steam
100°
Air Preheat Boiler feed water

C.W
Tambient 30°

Refrigeration
(high level) -10°

Refrigeration (low level)

 Utility Systems – General Rule for Cost
Effective Operations

In general:
• for hot utilities,
USE at the LOWEST level and GENERATE at the
HIGHEST level possible

• for cold utilities,

USE at the HIGHEST level and GENERATE at the
LOWEST level possible
 General Guidelines for Range of Process Operations
Equipment Guidelines for Setting Process Conditions
Reactor Pressure and Temperature depends on favourable conversion & yield

Separator:
Distillation Set top column pressure assuming (if possible) a water-cooled condenser
Azeotropic As in distillation, but may operates for special pressure to avoid azeotrope
conditions
Absorption Operation between ambient pressure and 10 bar to prevent solvent loss

Flash Operation at much lower pressure (and temperature) than upstream equipment
depending on the required split fraction of key component
LL-Extraction Operation around ambient pressure and temperature
S-L Separation Operation around ambient pressure and temperature
Adsorption Find the optimum (high) pressure to enable separation
Membrane Find the optimum (high) pressure to enable separation

General Rule : Pressure : Between 1 to 10 bara

Temperature : 40 to 250oC

Azetrope: a mixture of two liquids that has a same/constant boiling point and composition in distillation proceses.
  Eliminate differences in T, P and phase

Fig 4.7
Copyright@FKKKSA, UTM Computer-Aided Process Simulation Project
 Synthesis Tree

Copyright@FKKKSA, UTM Computer-Aided Process Simulation Project Intro to PD - 23

 Preliminary Process Synthesis
Process Synthesis involves:
 Selection of processing mode: continuous or batch
 Fixing the chemical state of raw materials, products, and by-products,
noting the differences between them.
 Process operations (unit operations) - flowsheet building blocks
 Synthesis steps:
 Eliminate differences in molecular types (chemical reaction)
 Distribute chemicals by matching sources and sinks (mixing &
recycle)
 Eliminate differences in composition (separation)
 Eliminate differences in temperature, pressure and phase
 Integrate tasks (combine tasks into unit operations)
 Integrate tasks (combine tasks into unit
operations)

In other words, specify all the tasks in term

of unit operations within the flowsheet…
Chlorination reactor
 Cl2 and C2H4 in vapor phase bubble through the liquid
C2H4Cl2 (with dissolve ferrite catalyst).
 Heat is released as C2H4Cl2 formed causing some of the
product to vaporise and rise up through rectifying section
(trays)
Condenser is added the top of reactor to condense the vapor
with CW. Some condensate is return to rectifying section.
• Pump
 To increase the pressure of liquid C2H4Cl2 from 1.5 to 26
atm.
• Evaporator
 To increase liquid temperature and to boil it to saturated
vapor at 26 atm, 242oC
• Pyrolysis Furnace with Economizer
 The economizer (function similar to HEX) at inlet is to
preheat the sat vapor to 500oC and followed by pyrolysis
reaction in the present of catalyst (Nickel).
• Spray quench tank and cooler
 To rapidly quench the pyrolysis effluent to avoid carbon
deposition? in HEX tubes (if send directly to HEX).
 The outlet stream is at its dew pressure of 170oC, 26 atm
 Hot gases are showered with cold liquid. The heat transferred
to liquid is removed when the liquid is circulated in the
adjacent cooler (using CW).

• Condenser and valve

 To reduce temperature and then condense the stream to its
bubble point of 6oC and 12 atm
• Recycle cooler
 To cool the recycle dichloroethane from 146.1oC to to 90oC
prior mixing with dichloroethane from chlorination reactor.
  Integrate tasks (tasks  unit operations)

Fig 4.8
Assembly of synthesis tree

The bold branches trace

the development of
only one flowsheet of
VC process.
 What next?
• Identify promising alternative flowsheet(s) for
further development
• We call this base-case design (s)
• First we need to create detailed PFD
• Gather additional database
• Do pilot plant test
• Simulation
• Continuous improvement
Block Flow Diagram (for VC)

Fig 4.18 (Almost similar to Figure 4.5)

 Process Flow Diagram (PFD)
• Much more detailed view of the process.
• Usually constructed using process simulators.
• Updated throughout much of process design.
• Almost similar to flowsheet develop after the completion of
task integration (with stream and unit operation numberings).
• Unit Operation is identified with U-XYY ,(e.g. P-102)
U – Unit type (P for pump), X –single digit identifying process
area, YY –two-digit equipment number.
• Each stream in label as a numbered diamond.
 Process Flow Diagram (PFD)
• Information (T,P, vapor fraction, component molar flow rates,
total mole and mass flow rates, also enthalpy, density, heat
capacity, viscosity) for each stream is tabulated and place at
the bottom of PFD (e.g. 3.6)
• Equipment summary, see Table 3.8
Note: Mass and Energy Balance are almost complete for the
flowsheet.
• More details information to begin the construction
engineering work are in the Piping and Instrumentation
Diagram (see Ulrich 1984, Sandler & Luckiewicz 1993).
Contain additional info on location and type of control
instruments, valves (isolation and control), MOC of piping
(size, schedule) etc
 Icons for process unit

Fig 4.20
 Utilities
• Cooling
Cooling water (cw), Refrigerated Brine (rb)
propane refrigeration (pf)
• Heating
fuel gas (fg), high-pressure steam (hps)
medium-pressure steam (mps), low-pressure steam (lps)
• See Table 4.7 for typical operating range.
 Development of Base-case Design
Develop one or two of the more promising flowsheets from the
synthesis tree for more detailed consideration.
 What next?
• Check assumptions?
• Refining and adding preliminary database (e.g. kinetics data)
• More simulation (using process simulator and/or simulation
model) for any changes (different unit operation or process
parameters)
• Pilot-plant testing by development team (need planning as
time consuming/expensive)
• Process Integration
Heat and Power Integration (for Energy saving), see Ch 10
Mass Integration (e.g. minimize solvent used),
see Ch 11
• Detailed design calculations……
Further Reading for Hierarchical Approach to
Process Synthesis:

J. M. Douglas, Conceptual Design of Chemical Processes,

Chapter 1, McGraw-Hill, 1988.

Biegler et al. Systematic Methods of Chemical Process Design,

Chapter 2, Prentice hall, 1997.
THANK YOU