Assignment Filtration Adsorption

Separation processes II
Module CPPT 9004: Separation processes II
1
Contents
Object
Introduction
Process Operations
Applicability
Theory
Limitations
Counter current model
Co-current model
Column High and diameter
Modeling
General Process Summary
Conclusions
References
Appendix A
Appendix B
2
Object
Part A : Filtration
Filtration and drying are two important unit operations in most pharmaceutical
and chemical processes and are usually carried out in series. In the aspirin
production process you will have conducted mass and energy balances over the
filter. Based on these balances, critically examine a number of filtration options
and select what you consider to be the most suitable types, giving your reasons.
Filtration unit operation:
The stream from the crystalliser is fed to a filtration unit (feed composition is
based on the mass balance performed in Module 9001). Laboratory tests have
given the following data. (Assume an incompressible filter-cake and that the
resistance related to the filter medium and initial layer is negligible)
The filter cake porosity = 0.1
Filtrate specific gravity = 1.0 kg per litre
Specific resistance of the filter-cake, r = 8.0 x 1013 m-2.
Filtrate viscosity, μ = 1.0 x 10-3 Ns m-2
Design vacuum and pressure filtration units for the required duty. Support your
argument with clear references to both authoritative literature and your design
calculations.
After washing, the filter-cake is pre-dried down to 2.0%w/w water in the
filtration unit before being fed to the dryer.
Part C : Adsorption
Problem No. 1:
Adsorption on 6x10-mesh activated carbon is being considered to recover
methyl ethyl ketone (MEK) from an air stream at 25 oC and 1 atm. The airflow is
12,000 std ft3/min, and the air has 0.4 lb MEK/1000 std ft 3. If the superficial
velocity is 0.5ft/s, and an adsorption cycle of at least 8 h is desired, what bed
dimensions should be used? Assume the bulk density of the carbon is 30 lb/ft3.
3
Problem No. 2:
Granular carbon is used to remove phenol from an aqueous waste. If 10x20 –
mesh carbon is used with a superficial velocity of 0.03m/s, estimate the number
of transfer units in a bed 4 m deep. The effective diffusivity in the particles can
be taken as 0.2 times the bulk diffusivity.
Properties of MEK = C4H8O8
T oC 14 25 41.6 79.6
P mm Hg 60 100 200 760
ρ = 0.805 g/cm3 at 20 oC
M= 72.1
Incoming air has 0.40 lb MEK/1000 SCF
0.40 / 72 .1
y= = 1.99*10 -3
mol fraction MEK
1000 / 359
p = 1.99*10-3 (760) =1.51 mm Hg
At 25 oC , p/P= 1.51/100 = 0.0151
If the bed heats up to 40 oC during adsorption,

-3
p/P= 1.51/192= 7.86*10
We have to estimate equilibrium adsorption at 25 oC and 40 oC . From the table

of additive volume increments.
V = 4(14.8) + 8(3.7) +9.9 = 98.7
At 25 oC
(T/V) log (f/fs) = (298/98.7)log(100/1.51)= 5.498
4
Using the curve for n-paraffins:

Volume adsorbed =25cm3/100g
W=0.25*0.805=0.20g/g carbon
At 40oC,
(T/V) log (f/fs) = (313/98.7)log(192.1/1.51)= 6.670
W= 0.20*0.805=0.16 g/g carbon

Air flow at bed inlet:
(12000/60)*(298/272) = 218 ft3/s
For uo=0.5 ft/s, area = 436 ft2
For a cylindrical bed:
Dbed = (436*4/π)0.5 = 23.6 ft
A rectangular bed 14 ft x 31.1 ft or 16 ft x 27.3 ft could also be used. Check bed

depth to see if a horizontal cylinder could be used.
Per ft2 of cross section, MEK adsorbed in 8 h is:

8*0.5*3600*(273/298)*(0.40/1000) = 5.28 lb
Carbon needed: 5.28/0.16 = 33lb
Bed density is 30 lb/ft 3 or 30 lb/ft for 1 ft2
Lmin= 33/30=1.1 ft
If half the bed capacity is used at the breakpoint,a bed 2.2 ft long would suffice.
Then a racterngular bed 2-3 ft deep could be placed in the middle of a horizontal
cylinder vessel. This would be less expensive than a 23.6 ft diameter cylindrical
bed.
Estimate N, the number of transfer units
Dp= (3.327+1.651)/ 2= 2.49 mm

At 25oC μlρ for air = 0.152cm2/s
0.249 (0.5 * 30 .48 cm / s )

Re= = 25 .0
0.152
5
Introduction
The separation of the components of a liquid mixture by treatment with a

solvent in which one or more of the desired components is preferentially soluble
is known as liquid–liquid extraction—an operation which is used, for example, in
the processing of coal tar liquids and in the production of fuels in the nuclear
industry, and which has been applied extensively to the separation of
hydrocarbons in the petroleum industry. Extraction is a process that separates
components based on chemical differences. The basic principle behind extraction
involves the contacting of a solution with another solvent that is immiscible with
the original. The solvent is also soluble with a specific solute contained in the
solution. Two phases are formed after the addition of the solvent, due to the
differences in densities and immiscibility. The solvent is chosen so that the
solute in the solution has more affinity toward the added solvent. Therefore
mass transfer of the solute from the solution to the solvent occurs. Further
separation of the extracted solute and the solvent will be necessary. However,
these separation costs may be desirable in contrast to distillation and other
separation processes for situations where extraction is applicable.
It is possible to combine stages A-(bringing the feed mixture and the solvent
into intimate contact) and B-(separation of the resulting two phases) into a
single piece of equipment such as a column which is then operated continuously.
Such an operation is known as differential contacting. Liquid–liquid extraction is
6
also carried out in stagewise equipment, the prime example being a mixer–
settler unit in which the main features are the mixing of the two liquid phases by
agitation, followed by settling in a separate vessel by gravity.[1],[8]
General Extraction Flowsheet
EXTRACT
FEED
SOLVENT
RAFFINATE
Figure 1: Flowsheet for the extraction column.
A general extraction column has two input stream and two output streams. The
input streams consist of a solution feed at the top containing the solute to be
extracted and a solvent feed at the bottom which extracts the solute from the
solution. The solvent containing the extracted solute leaves the top of the
column and is referred to as the extract stream. The solution exits the bottom of
7
the column containing only small amounts of solute and is known as the
raffinate. Further separation of the output streams may be required through
other separation processes. In this case be practical distillation column for
further purification of ethanal, from the water – ethanal raffinate solution.
Therefore extraction is in many ways complementary to distillation and is
preferable in the following cases: [1],[8]
(a) Where distillation would require excessive amounts of heat, i.e. when the
relative volatility is near unity.
(b) When the formation of azeotropes limits the degree of separation obtainable
in distillation.
(c) When heating must be avoided.
(d) When the components to be separated are quite different in nature
Process Operation
There are certain design variables that must be assigning in an extraction

process. As in many separation processes, the pressure and temperature
conditions play a large role in the effectiveness of the separation. In order for a
good split of the feed the pressure and temperature must be such so as to
ensure that all components remain in the liquid phase. The process will be
adversely affected if one or more of the components are allowed to become a
vapour, or the extraction may not occur at all if a large enough portion of a
component is allowed to vaporize. In addition, the temperature should be high
enough that the components are all soluble with one another. If extremes in
temperature are present, finding a suitable solvent for extraction can be
problematic. This is however generally not the case since one of the biggest
benefits in the extraction process is that it can be done at ambient pressures
and temperatures. In many applications, a separation process is desired where
an extreme temperature will destroy the desired product such as the
pharmaceutical industry. For these applications, extraction is ideally suited,
since the only temperature requirement is that dictated by the solubility. At this
point the biggest challenge would be finding a suitable solvent for the
extraction. We can also use the pharmaceutical industry in another example for
the benefits of extraction and this has to do with the volumes involved for
effective extraction. The extraction process can become very expensive if the
8
solvent needed to be used is costly these expenses can be contained if a batch

process is being used and this is often the case in medicines. In a non-batch
process the solvent would need to be constantly supplied and this would involve
either a huge amount of solvent or another separation process in order to
recycle the solvent. [4]
In this case, we assume:
1. Operating temperature, temperature of entering stream 15oC (ambient).
2. Operating pressure, pressure of entering stream 1 atm (ambient).
3. Feed Flow Rate 1000kg/h.
4. Composition of feed 0.0526 kg Ethanal /kg Toluene in feed,
kgEthannal 50
x2 = = = 0.0526 .
kgToluene 950
Applicability
It must decide which extractor would be relevant for our situation. The
specifications for each of these different systems are relatively the same. The
design limitations should be placed on each system in order to optimize the
individual process, maximize surface area of mass transfer, and adjust flow
feeds for maximum solute recovery. Generally, there are three main types of
extractors:
1. Mixer-settlers - are used when there will only be one equilibrium stage in the
process. For such a system, the two liquid phases are added and mixed. Due to
their density differences, one phase will settle out and the mixture will be
separated. The downfall to this type of extractor is that it requires a large-
volume vessel and a high liquid demand.
9
Figure 2: Example of mixer-settler [2]
2. Contacting columns - are practical for most liquid-liquid extraction systems.

The packings, trays, or sprays increase the surface area in which the two liquid
phases can intermingle. This also allows for a longer flow path that the solution
can travel through. In the selection of a packing, it is necessary to select a
material that is wetted by the continuous phase. Lastly, the flow in a column
should always be counter-current.
10
Figure 3: Example of mixer-settler [2]
3. Centrifugal contractors - are ideal for systems in which the density difference
is less than 4%. In addition, this type of system should be utilized if process
requires many equilibrium stages. In these systems, mechanical devices are
used to agitate the mixture to increase the interfacial area and decrease mass
transfer resistance.
11
Figure 4: Example of centrifugal contractor [3]
Bellow tabulated advantages and disadvantages for the various extractor types.
Type of extractor Advantages Disadvantages

Mixer-settler - efficient - large area to by
- good contacting used
- any number of - cost (high
stages operation and set-
- low head room up)
Centrifugal extractor - able to separate - high set-up and
liquid with small operation cost
density differences - not applicable for
- short holding time many stages
Column - small investment - difficult to scale-up
( without agitation) and operation cost - less efficient then
mixer-settlers
- high head room
Column (with agitation) - low investment - not applicable for

cost high flow ratio
- handle many - separation difficult
number of stages for small densities
- good dispersion differences
Table 1: Advantages and disadvantages various types of extractors. [4]
12
Theory
Usually in a liquid-liquid system there are three components, A, B, and C, in two

phases. Substituting into the phase rule gives 3 degrees of freedom. There are 6
variables: temperature, pressure, and four concentrations. Two of the mass
fractions in a phase can be specified with the third determined by the equation:
XA + XB + XC = 1.0
For most situations temperature and pressure are set, therefore the system can
be fixed by setting one concentration in either phase. Ternary Phase diagrams,
triangular coordinates, are used to represent the equilibrium data of three-
component systems. This is shown in figure bellow.
Figure 5: Example of general triangular diagram.
For example the mass fraction xc is designated by the perpendicular distance to

base AB. Furthermore these diagrams are fitted with curves and lines presenting
the equilibrium data for the components in the mixture. A typical phase diagram
is shown in Figure 3. For example the mass fraction xc is designated by the
perpendicular distance to base AB. Furthermore these diagrams are fitted with
curves and lines representing the equilibrium data for the components in the
mixture. A typical phase diagram is shown in figure bellow.
13
Figure 6: General Liquid-Liquid phase diagram
The mixture in Figure 3 will separate into two phases following the tie line that
runs through point M. Point A is the raffinate phase and B is the extract phase.
Several other tie lines are shown. Point P represents the point where the two
phases are the same, this is known as the Plait point. The area of the two-phase
region and the path of the tie lines depend on the equilibrium data for the
system. These graphs change due to variables such as the components used in
the system, temperature, and pressure.
Equilibrium data
The equilibrium condition for the distribution of one solute between two liquid
phases is conveniently considered in terms of the distribution law. Thus, at
equilibrium, the ratio of the concentrations of the solute in the two phases is
given by CE/CR = K’ where K’ is the distribution constant. This relation will apply
accurately only if both solvents are immiscible, and if there is no association or
dissociation of the solute. If the solute forms molecules of different molecular
weights, then the distribution law holds for each molecular species. Where the
concentrations are small, the distribution law usually holds provided no chemical
reaction occurs. The addition of a new solvent to a binary mixture of a solute in
a solvent may lead to the formation of several types of mixture:
1. A homogeneous solution may be formed and the selected solvent is then
unsuitable.
2. The solvent may be completely immiscible with the initial solvent.
3. The solvent may be partially miscible with the original solvent resulting in the
formation of one pair of partially miscible liquids.
4. The new solvent may lead to the formation of two or three partially miscible
liquids. [1]
14
For the purpose of this exercise I assume that toluene and water are immiscible
and the distribution coefficient or K-value is 2.20 i.e. y = 2.2x, where y = kg
ethanal/kg water and x = kg ethanal/kg toluene.
W Y in
F X A , in F X A, out
EXTRACTION COLUMN
W Yout
Figure 7: Scheme of the extraction process.
Limitations
1. Suitable Solvent [4]
- Solvent partially soluble with the carrier.
- Feed components immiscible with the solvent.
- Solute is soluble in the carrier and at the same time completely or partially
soluble in the solvent.
- Different densities than the feed components for a phase separation to
facilitate and maintain the capacity of the extractor high.
- Extremely high selectivity for the solute for the solvent to dissolve the
maximum amount of solute and the minimum amount of the carrier.
- Large distribution coefficient to reduce the theoretical number of stages
contributing to a greater efficiency
15
- Low viscosity increases the capacity of the extraction column and does not
allow for the settling rate of dispersion to be slow.
- Chemically stable and inert toward other components of the system
- Low cost, non-toxic, and non-flammable.
2. Equipment
- Interfacial tension and Viscosity
- High interfacial tension and viscosity leads to more power being supplied to
maintain rapid mass transfer throughout the extraction process.
- Low interfacial tension and viscosity leads to the formation of an emulsion.
3. Temperature preferred to be higher since solubility increases, but

temperature not higher than the critical solution temperature.
4. Pressure for condensed system must be maintained below the vapour

pressure of the solutions such that a vapour phase will not appear and interrupt
liquid equilibrium.
5. Separation may only occur for compositions in the region between the feed
composition and that apex of the carrier.

Step 1: Determine the minimum solvent-to-feed ratio (S/F)min. This calculation
needs to be completed to find the extract composition.
To find the minimum flow rate the slope from the equation need to be
calculated:
( y 2 − y1) (0.115 − 0)
SLOPE = = = 2.42
( x 2 − x1) (0.0526 − 0.005 )
2.42
a
=
s
Where a = 950 kg, therefore minimum flow rate:
950
S min = = 393 kg / hr
2.42
16
393 kg/hr is the minimum flow rate of water to achieve required purity of
toluene. Though to design extractor operating with this flow rate, will required a
large number of stages. The equilibrium curve is draw based on the equation
given as y = 2.2x .
Counter current minimum water flow rate
0.12
0.1
kg ethanal/ kg water
0.08
0.06
0.04
0.02
0
0 0.01 0.02 0.03 0.04 0.05 0.06
kg ethanal/kg toluene
equlibrium 0.0526 Smin 0.005
Figure 8: Operating line for minimum water flow.
To choose proper operating conditions, a few different water flow rates will be
examine, and the results ware plotted. First step in this operation is to
determine the slope for each of the vary water flow rates.
For 400 kg/hr water flow rate slope will be:
950
Slope = = 2.38
400
Using formula for the slope:
17
( y 2 − y1)
SLOPE = where, x1= 0.005, x2= 0.0526, y1= 0, we can determine
( x 2 − x1)
unknown y2.
( y 2 − 0)
2.38 =
(0.0526 − 0.005 )
y2= 0.113
Tabulated data for different water flow rates for counter current model.
Flow rate Flow rate
water [kg] A [kg] Slope XN XF y1 y2
400 950 2.38 0.005 0.0526 0 0.113
600 950 1.58 0.005 0.0526 0 0.075
800 950 1.19 0.005 0.0526 0 0.057
1000 950 0.95 0.005 0.0526 0 0.045
1200 950 0.79 0.005 0.0526 0 0.038
1400 950 0.68 0.005 0.0526 0 0.032
1600 950 0.59 0.005 0.0526 0 0.028
1800 950 0.53 0.005 0.0526 0 0.025
2000 950 0.48 0.005 0.0526 0 0.023
Table 2: Results for vary water flow rate for counter current model.
The plot was created using Excel spreadsheet, as seen on next page on figure 9.
18
Counter current vary water flow rates

0.12
0.1
0.08
0.06
0.04
0.02
0
0 0.01 0.02 0.03 0.04 0.05 0.06
equlibrium 0.0526 0.005 400 kg/hr water
600 kg/hr water 800 kg/hr water 1000 kg/hr water 1200 kg/hr water
Figure 9: Operating lines for vary flow rates of water
19
Step 2: Calculate the number of stages. From graphic method steping off on the
plot from operating line to equilibrium line. This procedure should be repeated
until stages have been constructed to x1, the raffinate composition.
Counter current vary water flow rates

0.12
1
2
0.1 3
4
5
6
7
0.08 8
9
10
0.06 11
12
13
0.04
14
15
0.02
16
17
0 18
0 0.01 0.02 0.03 0.04 0.05 0.06

600 kg/hr water 1000 kg/hr water 2000 kg/hr water
Figure 10: Graphical method for determining the number of stages for the
counter current flow with water flow at 400kg/hr.
As can be seen for the flow water flow rate 400 kg/hr, which is close to amount
of minimum solvent = 393, the number of stages is 18.
20
Figure 11: Graphical method for determining the number of stages for the counter current flow with water flow at
600kg/hr,1000 kg/hr, 2000 kg/hr.
21
From the plot on the previous page, it is obvious by increasing amount of our
wash solvent decrees number of stages necessary to approach required purity of
our raffinate – toluene in this case. Tabulated results for vary water flow rate vs
number of stages.
Number of stages Solvent – water used [kg/hr]

18 400
4 600
3 1000
2 2000
Table 3: Number of stages versus water flow.
number of stages versu water flow for counter current model
20
18
16
number of stages
14
12
number of stages versu water
10
flow
8
6
4
2
0
0 500 1000 1500 2000 2500
Water flow [kg/hr]
Table 12: Plot number of stages versus water flow for counter current model.
Co-current model
22
For the co-current flow if the distribution law is followed, then the equilibrium
curve becomes a straight line given by y = mx. The material balance on the
solute may then be rewritten as:
Ax2 = Ax1 + Sy1 = Ax1 + Smx1 = (A + Sm)x1
and the number of stages is given by:
n = (log(x1/x2))/log[A/(A + Sm)]
Using the same formula for the slope:

( y 2 − y1)
SLOPE = where, x1= 0.005, x2= 0.0526, y2= 0, can be determine
( x 2 − x1)
unknown y1.
Tabulated data for different water flow rates for co-current model.
Flow
rate Flow
water raet A
[kg] [kg] Slope Xn Xf Slope y1 y2
400 950 2.38 0.005 0.0526 -2.38 0.113 0
600 950 1.58 0.005 0.0526 -1.58 0.075 0
800 950 1.19 0.005 0.0526 -1.19 0.057 0
1000 950 0.95 0.005 0.0526 -0.95 0.045 0
1200 950 0.79 0.005 0.0526 -0.79 0.038 0
1400 950 0.68 0.005 0.0526 -0.68 0.032 0
1600 950 0.59 0.005 0.0526 -0.59 0.028 0
1800 950 0.53 0.005 0.0526 -0.53 0.025 0
2000 950 0.48 0.005 0.0526 -0.48 0.023 0
Table 4: Results for vary water flow rates for co-current model.
23
Co-current extraction model

0.12
0.1
0.08
0.06
0.04
0.02
0
0 0.01 0.02 0.03 0.04 0.05 0.06
equlibrium 0.0526 kg ethanal/kg
0.005 toluene 400 kg/hr water
Figure 13: Operating lines for vary water flow rates for co-current model.
24
The number of stages can be determined from graphic method, by stepping off
on the plot prom operating line to equilibrium line. This procedure should be
repeated until stages have been constructed to x1, the raffinate composition.
Co-current extraction model - number of stages
0.12
0.1
0.08
1
0.06
0.04 2
3
0.02 4
6 55
0
0 0.01 0.02 0.03 0.04 0.05 0.06
Figure 14: Graphical method for determining the number of stages for the
co-current flow with water flow at 400kg/hr.
25
Figure 15: Graphical method for determining the number of stages for the co-current flow with water flow at 600kg/hr,
1000kg/hr, 1400kg/hr, 2000kg/hr.
26
As can be observed from the plot on the previous page, the number of stages
for different water flow rates, changes as in the table bellow.
Water flow rate [kg/hr] Number of stages

400 6
600 5
1000 5
1400 4
2000 3
Table 5: Tabulated data for graphic method for estimation of number of stages
in co-current model
5
number of stages
4
number of stages vs water flow
rate for co-current model
3
0
0 500 1000 1500 2000 2500
Water flow[kg/hr]
Table 16: Plot number of stages versus water flow for co - current model.
Column High and diameter
27
After completing all estimation calculations, and choosing the best operating
conditions, the extraction column diameter, and height, can be determined as
well as the estimation operating cost. As shown in next few steps.
Step A: Determination of Extraction Column Diameter [4]

For the counter-current flow the diameter of the column must be big enough to
allow two phases to flow through the column without flooding. The column
diameter for liquid –liquid devices can be estimate based on number of variables
including:
1. Individual phase flow rates
2. Density differences between the two phases
3. Interfacial tension
4. Direction of mass transfer
5. Viscosity and density of continuous phase
6. Geometry of internals
Column diameter can be determined through scale-up of laboratory test
analysis. The experimental data are obtained by: testing unit system with
components of concern in the laboratory or pilot plants on the really small scale.
The superficial velocities are measure in each phase. The sum of these velocities
may be assumed to hold constant for larger scaled-up commercial units.
Collected data will be used to calculate diameter of column.
Step B. Determining the Height of the Column
We can determine height based on HETS (Height Equivalent to a Theoretical

Stage) it can be applied directly to determine column height from the number of
equilibrium stages. The HETS depends on the physical properties such as;
interfacial tension, phase viscosities, density difference between phases.
Total Height = (HETS)(Number of Equilibrium Stages)
Step C. Costs estimation
28
The total cost of the extraction is directly related to the extraction design
variables and type of extraction equipment applied. The variables that affecting
the economic balance are:
- at fixed solvent feed ratio, the amount of solvent extracted increases with
increased number of trays. Hence, the value of the unextracted solute may be
balanced against the cost of the extraction equipment required to recover it.
- for a fixed extent of reaction, the number of stages required decreases as the
solvent rate or reflux ratio increases. The capacity of the equipment necessary
for handling the larger liquid flow must increase with the larger reflux rate.
Hence, the cost of the equipment passes through a minimum when the
minimum numbers of stages are utilized.
- when reflux ratio and solvent rates are increased the extract solutions become
more dilute. Therefore, the cost of solvent removal is increased as well as the
operating cost for increased utilities.
As a result of these economic balances the total investment and operating costs
must achieved a minimum at the optimum solvent reflux rate. Additional cost
must be considered for the recovery of the saturated raffinate product as well as
the extract.
MODELING
29
In chemical engineering, as well as in other scientific and technical domains,

where one or more materials are physically or chemically transformed, a process
is represented in its abstract form . The global process could be characterized by
considering the inputs and outputs. As input variables (also called “independent
process variables”, “process command variables”, “process factors” or “simple
factors”), we have deterministic and random components. From a physical
viewpoint, these variables concern materials, energy and state parameters, and
of these, the most commonly used are pressure and temperature. The
deterministic process input variables, contain all the process variables that
strongly influence the process exits and that can be measured and controlled so
as to obtain a designed process output. The chemical reactions that take place
over a broad range of temperatures and pressures are extraordinarily diverse.
From the modelling viewpoint, this complexity results in a considerable number
of process and non-process parameters with an appreciable quantity of internal
links, as well as in very complex equations describing the process state. When
we build a model, some phenomena are simplified and consequently some
parameters are disregarded or distorted in comparison with their reality. In
addition, some of the relationships between the parameters could be neglected.
Based on the set of simulation of processes, we have the simulation of a
physical process, which, in fact, is a small-scale experimental process
investigation. In other words, to simulate a process at laboratory-scale, we use
the analysis of a more affordable process which is similar to experimental
investigation. [5]
Modelling can be successfully used to:[5]

. reduce manufacturing costs
. reduce time and costs in all stages of the process life-cycle
. increase process efficiency
. allow a better and deeper understanding of the process and its
operation
. be used as support for the solutions adopted during the process
development and exploitation
. ensure an easy technological transfer of the process
. increase the quality of process management
30
. reveal abilities to handle complex problems

. contribute to reducing pollution
. improve the safety of the plants
. market new products faster
. reduce waste emission while the process is being developed
. improve the quality of the products
. ensure a high quality of training of the operators.
1. ASPEN MODELS
A few of the choices are described here. The key decision must be make is what
model to use for the liquid phase activity coefficient. The Help/Physical Property
Methods/Choosing a Property Method menu gives advice about which
thermodynamic model is recommended for different applications. In the liquid
phase, the simplest option is an ideal liquid, with an activity coefficient equal to
1.0. That choice leads to Raoult’s law, which may suffice for similar chemicals.
Other models include regular solution theory using solubility parameters
(although not in Aspen Plus), NRTL, Electrolyte NRTL, UNIFAC, UNIQUAC, Van
Laar, and Wilson. Characteristics of the models are:[6]
1. The Electrolyte NRTL is especially suited for acid gas adsorption, which
includes the removal of carbon dioxide and hydrogen sulfide from a gas stream.
Refineries routinely use this process when making hydrogen. This is also one
way of capturing carbon dioxide from a power plant to capture and sequester it.
2. The UNIFAC model is a group contribution method that allows the model
parameters to be estimated using the molecular structure of each chemical.
When experimental data is not available, this is the only method that can be
used.
3. The UNIQUAC model uses binary parameters, which must be determined from
31
experimental data. Once found, however, the same parameters can be used in
multicomponent mixtures of three or more chemicals.
4. Both UNIFAC and UNIQUAC can be used when two liquid phases or
azeotropes are present.
5. The Van Laar options are less recommended in Aspen Plus; they are simpler
to use than the others, but less successful in general. In Aspen Plus the ease of
use is immaterial since someone else has created the program.
6. The Wilson equation is an option if there is only one liquid phase, and it does
handle azeotropes.
The simulations ware run based on two models, as they ware the most
applicable for the system of interest: UNIFAC and UNIQUAC.
32
Overall flowsheet for extraction counter current mode in ASPEN , as seen bellow.
B1
6 8
Figure 17: Extraction flowsheet counter current mode.
Where:
Stream 6 – Water
Stream 7 - Feed
Stream 8 - Extract
Stream 9 - Raffinate
B1- Extraction Unit
The run of the sensitivity simulation was based on vary water flow rate, which
was applied for a different number of stages in column. The comparison of
results obtained using different models types, based on information provide by
ASPEN Help Library Tool. Column was set-up in two modes: UNIFAC and
UNIQUAC, temperature = 15oC (ambient), pressure = 1 Atm (ambient).
On the next page tabulated data.
33
WATER TOLUEN ETHANAL 1 ETHANAL 2 WATER TOLUEN ETHANAL 1 ETHANAL 2

KG/HR KG/HR KG/HR KG/HR KG/HR KG/HR KG/HR KG/HR
480 949.7442 24.29787 25.70213 480 949.7356 26.67466 23.32534
580 949.6974 27.68861 22.31139 580 949.6857 30.77106 19.22894
680 949.6515 30.54623 19.45377 680 949.6382 34.20682 15.79318
780 949.6074 32.96297 17.03703 780 949.5932 37.03377 12.96623
880 949.5646 35.00795 14.99205 880 949.5494 39.32546 10.67454
980 949.5231 36.74245 13.25756 980 949.5075 41.17444 8.825557
1080 949.4825 38.21617 11.78383 1080 949.4667 42.66185 7.338153
1180 949.4422 39.47256 10.52744 1180 949.4271 43.86082 6.139179
1280 949.4025 40.55028 9.449717 1280 949.3874 44.82659 5.173406
1380 949.3635 41.48076 8.51924 1380 949.3493 45.61447 4.385529
1480 949.3243 42.28418 7.715817 1480 949.311 46.25578 3.744216
1580 949.2855 42.98369 7.016307 1580 949.2732 46.78379 3.216209
1680 949.2475 43.59771 6.402294 1680 949.2356 47.22009 2.779915
2 STAGES
3 STAGES
1780 949.2092 44.13655 5.863455 1780 949.1978 47.58292 2.417084
1880 949.1715 44.61274 5.38726 1880 949.1603 47.88706 2.112941
1980 949.1337 45.03417 4.96583 1980 949.1233 48.1437 1.856299
2000 949.1261 45.11266 4.887341 2000 949.116 48.19015 1.809848
Table 6: Tabulated data for ASPEN simulation n-stages – vary water flow rate, table 1.UNIFAC mode.
34
WATER TOLUEN ETHANAL 1 ETHANAL 2 WATER TOLUEN ETHANAL 1 ETHANAL 2

480 949.7314 27.82472 22.17528 480 949.7313 27.82126 22.17874
580 949.6794 32.45003 17.54997 580 949.6796 32.45437 17.54563
680 949.6302 36.33282 13.66718 680 949.6303 36.33481 13.66519
780 949.5839 39.45853 10.54147 780 949.5839 39.45944 10.54056
880 949.5401 41.89971 8.100288 880 949.54 41.90028 8.099716
980 949.4977 43.76311 6.236886 980 949.4982 43.76568 6.234318
1080 949.4578 45.17746 4.822539 1080 949.4578 45.17708 4.822922
1180 949.4181 46.24061 3.75939 1180 949.4185 46.24196 3.758043
1280 949.3798 47.04437 2.955626 1280 949.3802 47.04483 2.95517
1380 949.342 47.65511 2.34489 1380 949.3419 47.65458 2.345424
1480 949.3045 48.12135 1.878653 1480 949.3044 48.12109 1.87891
1580 949.2674 48.48126 1.518742 1580 949.2674 48.48107 1.518926
1680 949.23 48.76071 1.239287 1680 949.2302 48.76108 1.238921
4 STAGES
5 STAGES
1780 949.1934 48.98069 1.019305 1780 949.1929 48.98037 1.019629
1880 949.1565 49.15472 0.84528 1880 949.1564 49.15465 0.845346
1980 949.1192 49.2935 0.706496 1980 949.1194 49.29358 0.706417
2000 949.1119 49.31784 0.682159 2000 949.1119 49.31784 0.682162
Table 7: Tabulated data for ASPEN simulation n-stages – vary water flow rate, table 2.UNIFAC mode.
35
T o lue n v s wa te r v a ry wate r flow ra te
1870
1670
1470
2 stages
Water [kg/hr]
1270 3 stages
4 stages
5 stages
1070
870
670
470
949.1 949.2 949.3 949.4 949.5 949.6 949.7 949.8
T olu ene [kg /hr]
Figure 18: Plot for results toluene Vs water for UNIFAC mode.
36
Bellow collected data for toluene versus ethanal in extract stream for 2, 3, 4,
and 5 stages in UNIFAC mode.
Sensitivity S-1 Results Summary

50.0
ETH1
45.0
40.0
KG/HR
35.0
30.0
25.0
949.05 949.1 949.15 949.2 949.25 949.3 949.35 949.4 949.45 949.5 949.55 949.6 949.65 949.7 949.75 949.8
TOLUEN KG/HR
Figure 19: Toluene Vs Ethanal in extract stream for 2 stages, UNIFAC mode.

50.0
ETH1
45.0
40.0
KG/HR
35.0
30.0
25.0
949.05 949.1 949.15 949.2 949.25 949.3 949.35 949.4 949.45 949.5 949.55 949.6 949.65 949.7 949.75 949.8
TOLUEN KG/HR
37

50.0
ETH1
45.0
40.0
KG/HR
35.030.0
25.0
949.05 949.1 949.15 949.2 949.25 949.3 949.35 949.4 949.45 949.5 949.55 949.6 949.65 949.7 949.75 949.8
TOLUEN KG/HR

949.8
TOLUEN
949.7
949.6
949.5
KG/HR
949.4949.3
949.2
949.1
22.0 23.0 24.0 25.0 26.0 27.0 28.0 29.0 30.0 31.0 32.0 33.0 34.0 35.0 36.0 37.0 38.0 39.0 40.0 41.0 42.0 43.0 44.0 45.0 46.0 47.0 48.0 49.0 50.0
ETH1 KG/HR
Sensitivity test was repeated for the same variables, using UNIQUAC mode. On
the next page tabulated data.
38
WATER TOLUEN ETH1 ETH2 WATER TOLUEN ETH1 ETH2

480 949.759 7.76179 42.23821 480 949.7589 7.932407 42.06759
580 949.7083 9.258436 40.74156 580 949.7083 9.529974 40.47003
680 949.658 10.71364 39.28636 680 949.6576 11.10162 38.89838
780 949.6077 12.13846 37.86154 780 949.6068 12.64101 37.35899
880 949.5574 13.50642 36.49358 880 949.5564 14.1679 35.8321
980 949.5071 14.82227 35.17773 980 949.5054 15.64362 34.35638
1080 949.4572 16.10266 33.89734 1080 949.4551 17.10797 32.89203
1180 949.4072 17.32702 32.67298 1180 949.4047 18.52515 31.47485
1280 949.3571 18.50375 31.49625 1280 949.3544 19.89388 30.10612
1380 949.3071 19.62506 30.37494 1380 949.3042 21.24955 28.75045
1480 949.2579 20.74037 29.25963 1480 949.2539 22.52621 27.47379
1580 949.208 21.7648 28.2352 1580 949.2035 23.77485 26.22515
1680 949.1582 22.75903 27.24097 1680 949.153 24.98476 25.01524
2 STAGES
3 STAGES
1780 949.109 23.72184 26.27816 1780 949.1035 26.12244 23.87756
1880 949.0598 24.65211 25.34789 1880 949.0538 27.24526 22.75474
1980 949.0105 25.52951 24.47049 1980 949.0039 28.29413 21.70587
2000 949.0002 25.69364 24.30636 2000 948.9943 28.51686 21.48314
Table 8: Tabulated data for ASPEN simulation n-stages – vary water flow rate, table 1.UNIQUAC mode.
39
WATER TOLUEN ETH1 ETH2 WATER TOLUEN ETH1 ETH2

480 949.759 7.968364 42.03164 480 949.7592 7.991244 42.00876
580 949.7084 9.592094 40.40791 580 949.7084 9.604901 40.3951
680 949.6571 11.17303 38.82697 680 949.6576 11.21473 38.78527
780 949.6067 12.78024 37.21976 780 949.6067 12.81812 37.18188
880 949.5557 14.34613 35.65387 880 949.5561 14.42265 35.57735
980 949.5052 15.9139 34.0861 980 949.5047 15.98823 34.01177
1080 949.4548 17.45886 32.54114 1080 949.4539 17.56418 32.43582
1180 949.4037 18.96508 31.03492 1180 949.4035 19.15834 30.84166
1280 949.3529 20.44868 29.55132 1280 949.3525 20.69463 29.30537
1380 949.3022 21.89732 28.10268 1380 949.3017 22.19923 27.80077
1480 949.252 23.33526 26.66474 1480 949.2515 23.73277 26.26723
1580 949.2009 24.69912 25.30088 1580 949.2008 25.16638 24.83362
1680 949.1517 26.04809 23.95191 1680 949.1499 26.6151 23.3849
4 STAGES
5 STAGES
1780 949.1009 27.33494 22.66506 1780 949.0998 28.02938 21.97062
1880 949.0509 28.58773 21.41227 1880 949.0496 29.34275 20.65725
1980 949.0008 29.7772 20.2228 1980 948.9983 30.61331 19.38669
2000 948.9904 30.00157 19.99843 2000 948.9893 30.91345 19.08655
Table 9: Tabulated data for ASPEN simulation n-stages – vary water flow rate, table 2.UNIQUAC mode.
40
Toluene vs water for UNIQUAC mode
1850
1650
1450
Water [kg/hr]
2 stages
1250 3 stages
4 stages
1050 5 stages
850
650
450
948.98 949.18 949.38 949.58 949.78 949.98
Tolue ne [kg/hr]
Figure 23: Plot for results toluene Vs water flow rate for UNIQUAC mode.
Bellow collected data for toluene versus ethanal in extract stream for 2, 3, 4,
and 5 stages in UNIQUAC mode.

949.8
TOLUEN
949.7
949.6
949.5
KG/HR
949.4949.3
949.2
949.1
6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0
ETH1 KG/HR
Figure 24: Toluene Vs Ethanal in extract stream for 2 stages, UNIQUAC mode.
41

949.8
TOLUEN
949.7
949.6
949.5
KG/HR
949.4
949.3
949.2
949.1
949.0
6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 30.0
ETH1 KG/HR

35.0
ETH1
30.0
25.0
KG/HR
20.0
15.0
10.0
948.95 949.0 949.05 949.1 949.15 949.2 949.25 949.3 949.35 949.4 949.45 949.5 949.55 949.6 949.65 949.7 949.75 949.8 949.85
TOLUEN KG/HR
42

35.0
ETH1
30.0
25.0
KG/HR
20.015.0
10.0
948.95 949.0 949.05 949.1 949.15 949.2 949.25 949.3 949.35 949.4 949.45 949.5 949.55 949.6 949.65 949.7 949.75 949.8 949.85
TOLUEN KG/HR
Comparison UNIFAC VS UNIQAC model
2500
2000
Water [kg/hr]
1500
UNIFAC
UNIQUAC
1000
500
0
948.8 949 949.2 949.4 949.6 949.8
Toluene [kg/hr]
Figure 28: Comparison of UNIFAC and UNIQAC modes, based on 2 stages

sensitivity test.
Co –current mode
43
For co-current mode, ware run few different run with vary flow of wash solvent,
as well as vary number of stages. Set up for co – current run was as describe:
mixer to which fresh feed and solvent stream ware introduced, was followed by
settler, from which extract was collected at the bottom, and the raffinate from
the top was send it to the nest stage, so in that case to next mixer unit.
Operating conditions ware applied as describe for counter current flow,
temperature= 15oC , and the pressure = 1 atmosphere. Use of Aspen Plus was
based on UNIFAC model. Bellow – next page, general flow shets, and table
results, for 2, 3, 4 stages separation unit with vary water flow rates: 500, 1000,
1500 [kg/hr] respectively.
44
Figure 29: 2 stages co-current mixer – settler separation unit.
45
Table 10: 2 stages co-current mixer – settler separation unit results for 500[kg/hr] water flow rate.
46
47
48
49
50
51
52
53
54
55
56
57
Co-current mode is mostly used in batch operation. Batch extractors have

traditionally been used in low capacity multi-product plants such as are typical in
the pharmaceutical and agrochemical industries. For washing and neutralization
operations that require very few stages, co-current operation is particularly
practical and economical and offers a great deal of flexibility. The extraction
equipment is usually an agitated tank that may also be used for the reaction
steps. In these tanks, solvent is first added to the feed, the contents are mixed,
settled and then separated. Single stage extraction is used when the extraction
is fairly simple and can be achieved without a high amount of solvent. If more
than one stage is required, multiple solvent-washes are given. Though operation
in co-current mode offers more flexibility, it is not very desirable due to the high
solvent requirements and low extraction yields. The co-current operation is
mostly used in low capacity multi-product batch plants. For larger volume
operation and more efficient use of solvent, counter current mixer-settlers or
columns are employed. Counter current operation conserves the mass transfer
driving force and hence gives optimal performance.
Comparison of co-current and counter current model
20
18
16
14
number of stages
12
co-current
10
counter current
8
0
0 500 1000 1500 2000
water flow [kg/hr]
Figure 32: Comparison of counter and co-current modes.
58
General Process Summary
EXTRACT
FEED ETHANAL
RAFFINATE
SOLVENT=WATER DISTILLATION
COLUMN
EXTRACTION
COLUMN
WATER
Figure 33: General process flowsheet.
After extraction process, we will have extract containing 99.5% of toluene and
0.5% of ethanal, and raffinate on the bottom of the extraction column
containing 0.5% of toluene, water and 99.5% of ethanal. Raffinate will be sent it
to distillation column for recovery and purification of the ethanal. As water-
ethanal system doesn’t create azeotrope solution, it will be easy to separate.
The boiling point of the ethanal = 20.2 oC, and the boiling point of the water =
100 oC. [11] the feed our raffinate will be introduced to distillation column at
o
temperature of 20 C, liquid at boiling point, with no vapour. Drawing a
equilibrium curve for water – ethanal system, based on the Antoine coefficients
which can be found in chemical engineering books. From the curve we are able
to compute the mass balance on the process. Composition on the top and the
bottom of the column is required, to step off the number of stages required to
achieve specific purity. The stepping off starts at the feed of around 20%(data
taken from Aspen Simulation counter current mode, water flow=480[kg/hr], and
finishing at point giving a distillation composition of 99%(as this is required
59
ethanal-acetaldehyde composition). Next step is to find reflux ratio, the equation

can be used:
Cp L (Tb − Tf )
q =1+
λ
Where:
Cp L =Specific Heat capacity of liquid
Tb = Bubble point
Tf = Feed temp
λ =Latent heat of vaporisation.
After completing mass balance for distillation column and energy balance,
diameter, and high can be estimate.
60
CONCLUSION
As we have seen in the sections above, there are a number of factors affecting
extraction performance. Laboratory and pilot plant testing using actual feed and
solvent help in optimization. The study could often be an iterative cycle
involving laboratory testing followed by process simulation and design. In most
industrial extractors, there is usually a good scope for optimizing solvent usage
and energy consumption. The extraction model, which I used for separation
ethanal/toluene/water is continuous process, counter current mode. The counter
current mode of operation outperforms the co-current mode. This is
demonstrated in a case study presented. This process was chosen because the
system operating with high quantity flow rate. Also I have used vary information
and methods for describing the material balance, designed of extraction column,
flow diagram. The system will operate at ambient pressure and temperature
which will be equal respectively 15oC and 1 atmosphere for the extraction
column. Based on the UNIQUAC Aspen model using binary parameters, which
are determine from experimental data. The same parameters can be used in
multicomponent mixtures of three components i.e. toluene / ethanal / water.
General design process required determination of solvent- water flow [kg/hr],
basic design of the system, number of stages, and equipment required. Based
on the run simulations in Aspen Plus, I will suggest counter current flow with 2
stages centrifugal extractor. As we can see from the results simulation for Aspen
counter current Sensitivity test, the best effectively we will achieve when we will
use 480-580 [kg/hr] of solvent- water, used in two stages step. I will suggest
“Pod” liquid-liquid centrifugal extractor and separator, as seen on the figure on
the next page.
61
Figure 34 : The Podbielniak Contactor
The Podbielniak is providing differential counter current extraction in a compact

hermetic rotor. Is used successfully for more than fifty years to solve extraction
problems in the chemical process industry, the Pod can provide up to 5
theoretical stages in one unit and can separate liquids with a specific gravity
difference as low as 0.01. The Pod has a bright future in new technologies as
indicated by ongoing research in non-conventional applications. [10] Counter
current configuration increase extraction efficiency at a given flow rate ratio.
Using Pod as an extractor we can reduces solvent usage and operating costs
while producing better product at higher yields in a safer environment. Complete
enclosure will provide safer operations process, the possibility of product
contamination will be reduced. Large interfacial area, and high flow rate will
shorten residence time when necessary. More stable then other types because
of horizontal orientation reduce possibility for formation of emulsion.
Introduce further separation process applies only for recovery of ethanal,
implement distillation reduce solvent and solute losses.
62
REFERENCES
1. Coulson and Richardson’s CHEMICAL ENGINEERING VOLUME 2,5th Edition

Particle Technology and Separation Processes,2002.
2. http://www.halwachs.de
3. http://www.bjtoptec.com
4. Seader,J.D. and Henley, E.J. Separation Process Principles. John Wiley
and Sons, 1998.
5. Chemical Engineering: Modelling, Simulation and Similitude Tanase Gh.
Dobre, José G. Sanchez Marcano ,2007.
6. INTRODUCTION TO CHEMICAL ENGINEERING COMPUTING, BRUCE A.
FINLAYSON, PH.D., A JOHN WILEY & SONS, INC., PUBLICATION, 2006.
7. http://www.akpetrochem.com
8. Unit Operations, Warren L. McCabe, Jul;ian C. Smith, Peter Harriott,
2001.
9. CHOPEY,N.P. Handbook of chemical engineering calculations
10. http://www.pharmaceuticalonline.com/article.mvc/Podbielniak-
Contactor-A-Unique-Liquid-Liquid-0003?VNETCOOKIE=NO
11. http://en.wikipedia.org
63
Appendix A
Acetaldehyde specification
64
Appendix B
Toluene specification
65

Assignment Filtration Adsorption

Caricato da

Informazioni sul documento

Descrizione originale:

Copyright

Formati disponibili

Condividi questo documento

Condividi o incorpora il documento

Opzioni di condivisione

Hai trovato utile questo documento?

Questo contenuto è inappropriato?

Copyright:

Formati disponibili

Assignment Filtration Adsorption

Caricato da

Copyright:

Formati disponibili

Separation processes II

Module CPPT 9004: Separation processes II

Counter current model

Column High and diameter

General Process Summary

Properties of MEK = C4H8O8

At 25 oC , p/P= 1.51/100 = 0.0151

If the bed heats up to 40 oC during adsorption,

We have to estimate equilibrium adsorption at 25 oC and 40 oC . From the table

V = 4(14.8) + 8(3.7) +9.9 = 98.7

Using the curve for n-paraffins:

W= 0.20*0.805=0.16 g/g carbon

For a cylindrical bed:

Dbed = (436*4/π)0.5 = 23.6 ft

A rectangular bed 14 ft x 31.1 ft or 16 ft x 27.3 ft could also be used. Check bed

Per ft2 of cross section, MEK adsorbed in 8 h is:

Estimate N, the number of transfer units

Dp= (3.327+1.651)/ 2= 2.49 mm

0.249 (0.5 * 30 .48 cm / s )

The separation of the components of a liquid mixture by treatment with a

General Extraction Flowsheet

Figure 1: Flowsheet for the extraction column.

There are certain design variables that must be assigning in an extraction

solvent needed to be used is costly these expenses can be contained if a batch

Figure 2: Example of mixer-settler [2]

2. Contacting columns - are practical for most liquid-liquid extraction systems.

Figure 3: Example of mixer-settler [2]

Figure 4: Example of centrifugal contractor [3]

Type of extractor Advantages Disadvantages

Column (with agitation) - low investment - not applicable for

Table 1: Advantages and disadvantages various types of extractors. [4]

Usually in a liquid-liquid system there are three components, A, B, and C, in two

Figure 5: Example of general triangular diagram.

For example the mass fraction xc is designated by the perpendicular distance to

Figure 6: General Liquid-Liquid phase diagram

Figure 7: Scheme of the extraction process.

3. Temperature preferred to be higher since solubility increases, but

4. Pressure for condensed system must be maintained below the vapour

Counter current model

Counter current minimum water flow rate

equlibrium 0.0526 Smin 0.005

Figure 8: Operating line for minimum water flow.

Using formula for the slope:

Counter current vary water flow rates

Figure 9: Operating lines for vary flow rates of water

Counter current vary water flow rates

equlibrium 0.0526 0.005 400 kg/hr water

Number of stages Solvent – water used [kg/hr]

Table 3: Number of stages versus water flow.

number of stages versu water flow for counter current model

Using the same formula for the slope:

Co-current extraction model

Co-current extraction model - number of stages

Water flow rate [kg/hr] Number of stages

Column High and diameter

Step A: Determination of Extraction Column Diameter [4]

Step B. Determining the Height of the Column

We can determine height based on HETS (Height Equivalent to a Theoretical

Step C. Costs estimation

In chemical engineering, as well as in other scientific and technical domains,

Modelling can be successfully used to:[5]

. reveal abilities to handle complex problems

Counter current model