EH2208O

DESIGN PROJECT II (MARCH 2017)

PRODUCTION OF 20,000 METRIC TONNES OF

POLYTETRAFLUOROETHYLENE PER YEAR

CHAPTER 5: PROCESS INTEGRATION

GROUP MEMBERS

AIMAN HAKIM BIN ROSLAN 2013849224

FATIN FATIHA BINTI ABDUL RAHIM 2014850038
HANEARYTHA LITAD CHARLES 2014679702
MUHAMMAD FAHMI BIN NIZAM 2013251462
NOOR AMILIA BINTI KHOSIM 2014231358
NURBADAYU BINTI BASIRON 2013493592

SUPERVISOR:
MS CHRISTINA VARGIS

FACULTY OF CHEMICAL ENGINEERING

UNIVERSITI TEKNOLOGI MARA
SHAH ALAM
 CHAPTER 5

PROCESS INTEGRATION

5.1 PROCESS DESCRIPTION

The raw material used for the production of PTFE is chlorodifluoromethane (CHClF2).
The material is stored within a pressurized vessel at 15 bar and 25C to maintain it in
liquid phase as this allows for easier storage and transportation. Upon exiting the tank,
the pressure of CHClF2 is reduced to 12 bar using a valve to prevent damage to the
upcoming equipment due to sudden inflow of high pressure liquid.

The stream is then heated to 450C as a preparatory step before entering a

tubular reactor (Ebnesajjad, 2013). Within the reactor, gaseous CHClF2 undergoes
pyrolysis reaction and is converted to TFE (C2F4) alongside hydrochloric acid (HCl) as
the side product. When operating at 810C and 6.55 bar, a conversion of 100% can
be achieved as stated by (Ebnesajjad, 2016). The product stream containing TFE and
HCl is then condensed to liquid state before entering a distillation column for
purification and separation. Since HCl has a lower boiling point than TFE, it will exit
through the overhead stream meanwhile TFE exits through the bottom stream. The
separation produces product streams containing 99.9% w/w HCl and 99.5% w/w TFE,
respectively.

The purified HCl is then diluted with water and sold as a second source of
revenue. Meanwhile, the purified TFE is fed to a continuous stirred tank reactor
(CSTR) for polymerization reaction and produce PTFE. Additionally, water and
benzoyl peroxide are added to the reaction which acts as the solvent and organic
initiator, respectively (Ebnesajjad, 2013). According to (Mori, Tsuchiya, & Okahata,
2005), the conversion can achieve as high as 80% and produce PTFE ranging
between 10,000 g/mol to 1,000,000 g/mol.

525
 The product stream is then fed to a mixing tank whereby a surfactant, sodium
borate is added to reduce the interfacial tension and form a stable colloidal dispersion
of PTFE. (Fernandez & Jebbanema, 2007). The sludge-like stream is subsequently
transported using an extruder to a filter press to remove unwanted components (waste
stream) from PTFE.

The discharged waste stream containing unreacted TFE, HCl and water is
purified using two distillation columns whereby TFE and HCl are recycled back into
the process meanwhile water is sent to a water treatment facility. The solid PTFE is
then transferred onto a conveyer belt and dried to remove residual moisture and
achieve the desired 99% purity.

526
5.2 PROCESS FLOW DIAGRAM BEFORE HEAT INTEGRATION

Figure 5.1: Process flow diagram for PTFE production plant before heat integration

527
5.3 PROCESS FLOW DIAGRAM AFTER HEAT INTEGRATION

Figure 5.2: Process flow diagram for PTFE production plant after heat integration

528
5.4 HEAT INTEGRATION

5.4.1 Pinch Technology

The objective of pinch technology is to minimize the used of external utilities for
heating and cooling process by matching the cold and hot process stream with a
network of heat exchanger. A pinch usually happen between the hot stream and cold
curves and for minimum energy requirements, heat should not be transferred across
the pinch.

Hot stream is the stream that must be cooled and are available at high
temperatures. Cold stream is those that must be heated and raised to the target
temperature. Stream is any flow which require to be heated or cooled, but does not
change in composition, and reaction process is not a stream because there is change
in chemical composition in the stream and make-up flow is not stream because no
heating and cooling process occur in the stream line.

In this process, there are 5 process streams that require heating or cooling.
These are listed below along with their thermal and flow data. A stream is referred to
as hot if it requires cooling and cold if it requires heating. The temperature of the
stream is not used to define whether it is hot or cold. Table 5.1 show the stream
data for hot and cold stream extracted from the process.

Table 5.1: Stream data for PTFE Plant

Stream No Condition Tin ( ) Tout ( ) Heat duty,H (kW)
2 Cold 25 450 637.5
5 Hot 810 400 487.78
6 Hot 400 180 238.47
7 Hot 180 30 147.03
8 Hot 30 -50 370.4

529
 The heat transferred between the streams is obtained from Hysys. Before
integration, the minimum hot and cold shown in calculation as below:

, , = 2 = 637.5
, , = 5 + 6 + 7 + 8 = 1243.6

Therefore, the total energy requires to heat the cold stream is 637.5 kW and 1243.6
kW of energy is need to cold the hot stream before heat integration.

5.4.2 Problem Table Algorithm (PTA)

In the pinch analysis, there are two methods that can be used for the process
integration which is the Problem Table Algorithm (PTA) and Composite Curve. For the
analysis, PTA is used because the method is more accurate compared to the
Composite Curve method. The steps used in the method are as shown below:

Step 1: Choosing a minimum approach temperature.

This represents the smallest temperature difference that two streams leaving or
entering a heat exchanger can have. Typical value are from 5 to 20. The effect of
using different minimum approach temperature on the economics trade-offs are
straightforward. As the minimum approach temperature increase, the heat transfer
area for the process heat exchangers decreases, but the loads on the hot and cold
utilities increase. Therefore, capital investment decreases but the operating cost
increase. For this plant, 10 is being used throughout the calculation.

Table 5.2: Minimum temperature difference used in industrial

(Ref: sectorwww.cheresources.com)
No Industrial Sector Experience ()
1 Oil refining 20-40
2 Petrochemical 10-20
3 Chemical 10-20

530
Step 2: Construction of temperature interval diagram.
The minimum temperature, Tmin is 10C. To determine the interval temperature,
equation below is used:

; =
2

; =
2

For stream where the specific heat capacity can be taken as constant and there is no
phase change, CP equation is shown as:
=
Where:
m= Mass flow rate (kg/s)
Cp= Specific heat capacity (kJ/.kg)
and,

Since the value of Q and T are available, CP can be calculated and are tabulated in
Table 5.3.

Table 5.3: Temperature Interval Table

Stream and Actual Interval Heat duty, T CP
condition temperature Temperature H (kW) () (kW/)
Tin ( ) Tout ( ) Tin ( ) Tout ( )
2 Cold 25 450 30 455 637.5 425 1.50
5 Hot 810 400 805 395 487.78 410 1.19
6 Hot 400 180 395 175 238.47 220 1.08
7 Hot 180 30 175 25 147.03 150 0.98
8 Hot 30 -50 25 -55 370.3 80 4.63

531
 Table 5.4: Temperature Interval Diagram
T CP,hot -
Internal Surplus /
CP,cold H (kW)
temperature () Deficit
(Kw/)
5
805

350 1.19 416.5 Surplus

CP=1.5
455

60 -0.31 -18.6 Deficit

6
395 CP=1.19
220 -0.42 -92.4 Deficit
7
175
CP=1.08
145 -0.52 -75.4 Deficit

30 2
5 0.98 4.9 Surplus
8
25 CP=0.98
80 4.63 370.4 Surplus

-55 CP=4.63
605.4

532
Step 3: Construction of Cascade Diagram

The cascade diagram simply shows the net amount of energy in each temperature
interval. Because energy can always be transferred down a temperature gradient, if
there excess energy in a given temperature interval this energy can be cascaded down
to the next temperature level. From the cascade diagram, it is evident that there is a
point in the diagram at which no more energy can be cascade down, and that energy
most often must be supplied from the hot utility to the process. Excess heat must be
rejected from the process to the cold utility.

From cascade heat flow of Figure 5.3, the first interval has a surplus of 416.5
kW, which is cascaded to the next interval. This second interval has a deficit of -18.6
kW, which leaves the heat cascaded from this interval to be 397.9 kW. In the third
interval, the process has a deficit of -92.4 kW, which leaves 305.5 kW, to be cascaded
to the next interval. And in the last interval, the process has a surplus of 370.3 kW,
which leaves 605.4 kW.

In normal situation, there is often a point whereby there is insufficient energy

to be cascaded down the process, taking the energy from the hot utility, hence the
name pinch zone. To continue the process, excess heat must be rejected from the
process to the cold utility. However, as based on cascade diagram from Figure 5.3, it
shows that heat is only cascaded or rejected to the cold utility. After cascading the
energy downward, the conditions of hot and cold streams would be either there is an
excess of energy or the energy is exactly balanced in every temperature interval. In
this case, it is not necessary to supply energy from hot utility to the process (Turton et
al., 2013).

533
 HOT UTILITES

805 0 kW
KKKKWK

H = 416.5

455 416.5 kW

H = -18.6

375 397.9 kW

H = -92.4

175 305.5 kW

H = -75.4

30 230.1 kW

H = 4.9

25 235 kW

H = 370.4

-55 605.4 kW

Cold utility

Figure 5.3: Cascade heat flow

534
5.4.3 Energy Target and Pinch Temperature

As shows in Figure 5.3, there is no supply of energy from hot utility to the process and
heat is only rejected to the cold utility, therefore;

QC,min = 605.4 .kW

; = + = 805 + 5 = 810
2

; = + = 805 5 = 800
2

5.4.4 Heat Exchanger Network

Heat exchangers are drawn as two circles connected in vertical line. The circles
connect the two streams between which heat is being exchanged; that is, the stream
that would flow through the actual exchanger. Heater and coolers are drawn as a
single circle, connected to the appropriate utility. There are few rule that must be taken
into consideration before a match is made between the hot and cold streams. The
rules are:
1. No exchanger has a temperature difference < Tmin
2. Heat must not be transferred across the pinch
3. There must not be external cold utility above the pinch
4. There must not be external hot utility below the pinch

The heuristics for devising a network for maximum heat recovery are given below:
1. Divide the problem at the pinch
2. Design away from the pinch
3. The network design above the pinch meeting the restriction of:

In making a match adjacent to the pinch the heat capacity, CP of the hot stream
should be equal to or less that of the cold stream to ensure that the minimum
temperature difference between the streams is maintained.

535
4. The network design below the pinch meeting the restriction of:

Below the pinch have the same procedure as the above the pinch. The criteria
of the matching stream are that the heat capacity CP for the hot stream must be equal
or greater than the hot stream which to ensure the minimum temperature difference is
maintained.

Table 5.5: CP Table for below pinch

CPhot ( kW/) CPcold ( kW/)
1.19 (S5) 1.5 (S2)
1.08 (S6)
0.98 (S7)
4.63 (S8)

The total number of heat exchanger unit that can be used in the process can
be determine from the equation below:

Nunir = no of hot stream + no of cold stream + no of utilites -1

Nunit = 4 + 1+ 1 -1 = 5 units

At below pinch, stream 2 has to split in order to heat the cold stream to
temperature, 450C. Because of the original CP value of stream 2 is higher than CP
in hot stream. This stream is split into 2 with CP of 0.352 and 1.148 to ensure the
minimum temperature difference is maintained. After the split, the stream 5 and 6 will
transfer the heat to the stream 2 through heat exchanger H-101 and H-102. After
contacting with the cold stream, stream 6 still has excess energy of 88 kW. The excess
energy combined, along with the excess energy from unpaired stream 7 and stream
8, 147.03 kW and 370.4 kW respectively will be transferred to the heat sink, or cold
utility through cooler E-102, E-103 and E-104.

536
Figure 5.4: Heat exchanger below pinch

537
5.4.5 Feasibility Study

Feasibility study is to know either the integration is feasible or not. The integration is
feasible if:
1. The temperature of both hot and cold streams does not cross each other
thus obey the 2nd Law of Thermodynamics.
2. The temperature differences between the streams are not less than Tmin used
which is 10

Figures 5.5: Feasible Study on Heat Exchanger Network Stream 2 and 4

Figures 5.6: Feasible Study on Heat Exchanger Network Stream 2 and 6

Temperature profiles above have shown clearly that for two heat exchangers
that have been integrated, the T for each end is not less than Tmin. The temperature

538
profiles also not cross-linking for all streams. So, all of the heat exchange processes
are feasible.

5.4.6 Comparison Before and After Heat Integration

The optimum design after heat integration gives the maximum energy recovery. Thus,
the utility cost is reduced. Table 5.6 shows the comparison in number of equipment
used in the processes and the amount of hot and cold utilities used before and after
heat integration. The number of heat exchanger used decrease from 5 to 4. Plus, the
total utilities used decreases. Thus, utility cost is lowered.

Table 5.6: Comparison before and after heat integration

Before heat Cost for After heat Cost for after
integration before heat integration heat
integration, integration,
(RM/year) (RM/year)
Number of 5 RM 8,435,192 4 RM 6,748,156
heat per 5 units per 4 units
exchanger
Hot utility, kW 637.5 1,287,048 0 0
Cooling water 1243.6 59,938.26 235.03 11,327.83
utility, kW
Refrigerant 370.4 396,626.6 370.4 396,626.6
utility, kW
*Hot utility cost is calculated for RM 63.67/GJ
*Cold utility cost is calculated as RM 1.52/GJ for cooling water and RM 33.77/GJ
for refrigerant

Total utilities saving, Kw

(637.5 + 1243.6 + 370.4) (0 + 235.03 + 370.4)

= 100% = 73 %
637.5 + 1243.6 + 370.4

539
Total saving for hot utilities, QH,

1,287,048 0
= 100% = 100 %
1,287,048

Total saving for cooling water utilities,

(59,938.26 + 396,626.6) ( 11,327.83 + 396,626.6)

100% = 10.6 %
59,938.26 + 396,626.6

From the calculation, 100 % cost for hot utilities and 10.6 % cost for cold utilities
is saved after applying heat integration. The payback period of the cost to purchase
heat exchangers with respect to total cost saving is calculated. Total cost saving per
year is calculated as:

= (1,287,048 0) + (59,938.26 11,327.83)

= 1,335,658.43/

5.4.7 CONCLUSION

Based on the data calculated, it is found that the objective to reduce the utilities
consumed throughout the process is achieved where about 73 % of the energy
consumed is being recovered by exchanging the heat between hot and cold streams
that feasible for process integration. The reduction of energy consumptions had
proven process integration is very beneficial to the company because optimum
recovery of energy is achieved. For this production, the number of heat exchanger is
reduce from 5 to 4. Therefore, this pinch method can apply for TFE plant to eliminate
and reducing energy usage for this production. Based on the process flow diagram
(PFD), The piping system network is not complicated after the heat integration
analysis and of course there is significant energy and cost saving after integration,
thus make it attractive to be implemented. So, in conclusion, heat integration can be
applied in the plant.

540
REFERENCES

1. Smith, R. (2005). Chemical process design and integration. Chichester, West

Sussex,
2. England: Wiley.
3. Turton, R., Bailie, R.C., Whiting, W.C., & Shaeiwitz, J.A. (2009). Analysis,
synthesis, and design of chemical processes. United state: Pearson
4. Temperature difference in industry, (n.d). Retrieved 10 April 2017 from
sectorwww.cheresources.com
5. Ebnesajjad, S. (2013). Introduction to Fluoropolymers: Materials, Tehcnology, and
Applications (1st Edition ed.): Elsevier Science & Technology Books.
6. Ebnesajjad, S. (2016). Expanded PTFE Applications Handbook: Technology,
Manufacturing and Applications. Cambridge: Matthew Deans.
7. Fernandez, A. M., & Jebbanema, L. (2007). The Effect of Surfactant Selection on
Emulsion Polymer Properties. Retrieved from
http://www.pcimag.com/articles/87271-the-effect-of-surfactant-selection-on-
emulsion-polymer-properties
8. Mori, T., Tsuchiya, Y., & Okahata, Y. (2005). Polymerizations of
Tetrafluoroethylene in Homogeneous Supercritical Fluoroform and in Detergent-
Free Heterogeneous Emulsion of Supercritical Fluoroform/Water.
Macromolecules(39), 604-608.

541