EXPERIMENT 7

ULTRAFILTRATION UNIT

13.1 INTRODUCTION

New chemical separation techniques such as membrane separations are becoming

increasingly popular as it provides effective separation without the use of heat energy as
in distillation processes. Heat sensitive materials can be separated or concentrated by
virtue of their molecular weights. Membrane separation technology has evolved from a
small-scale laboratory technique to a large-scale industrial process during the past 30
years. A classification of major types of membrane processes is given in Figure 2. The
Ultrafiltration Unit (Model: FD-12) is specially designed to allow students and
researchers to carry out a membrane process that is widely used in biotechnology and
process industries — the Ultrafiltration.

Ultrafiltration membranes are usually specified in terms of their "molecular weight cut-
off" (MWCO). Polymeric membranes are widely used and supplied in the form of
modules that give membrane areas in the range of 1 - 20 m2. The membranes that are
supplied with the FD-12 unit is classified as tubular type (Figure 1), which is widely used
and have turbulent flow conditions. The system is in a cross flow configuration where the
feed solution is pumped parallel to the membrane at a velocity in the range of 1 - 8 ms-1
with a pressure difference of 0.1 - 0.5 MPa across the membrane. Liquid permeates
through the membrane and feed emerges in a more concentrated form on exit from
module.

FIGURE 1: TUBULAR (MULTICHANNEL) TYPE OF MICROFILTER

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FIGURE 2: CLASSIFICATION OF MAJOR TYPES OF MEMBRANE PROCESSES

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The advantages of cross-flow membrane separations are:

a) Higher overall liquid removal rate is achieved by preventing solid buildup on
membrane surface.
b) The concentrate (retentate) remains in a mobile form suitable for further processing.
c) The solute content of the concentrate may be varied over a wide range.
d) It may be possible to fractionate solutes of different sizes.

CLEANING SOLUTION RETUM

CIRCULATION
SOLUTION TANK
FEED

FEED TANK

TI

RECIRCULATION PUMP

SUSPENSION
RECIRCULATION
PI

PI

FI
BANK OF CROSSFLOW FILTERS

FILTRATE FI FLOW INDICATOR

PI PRESSURE INDICATOR
DRAIN/BLEED
CONCENTRATED
TI TEMPERATURE INDICATOR
SUSPENSION
VALVE

FIGURE 3: TYPICAL CROSSFLOW OPERATION INCLUDES RECIRCULATION LOOP

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13.2 SUMMARY OF THEORY

Numerous theoretical models for ultrafiltration have been proposed along with the
identification of new factors controlling flux or mass transfer through membranes. The
basic operating patterns are best outlined in terms of the hydrodynamic resistance
resulting from the buildup of deposited materials on the membrane surface.

The flux, J will be given by:

1 dV ∆Ρ ∆Ρ
J= = = (1)
Am dt v ( R m + Rc ) v[Rm + (αVCb / Am )]

For most biological materials, α is a variable depending on the applied pressure and time
(the compressible deposit), so that the expression requires a numerical solution.

A useful method for the effects of cross-flow removal of depositing materials is to write:

∆Ρ
J= (2)
v (Rm + Rd − Rr )

Removal of solute by cross-flow is sometimes assumed constant, and equal to the

convective particle transport at steady state (JssCb), which can be obtained
experimentally or from an appropriate model. In many situations however, steady state
of filtration is seldom achieved. In such cases, it is possible to describe the time
dependence of filtration by introducing an efficiency factor β, representing the fraction of
filtered material remaining deposit rather than being swept along by the bulk flow. This
gives:

βαVCb
Rc = , Where 0 < β < 1 (3)
Am

Although deposition also occurs during ultrafiltration, an equally important factor

controlling flux is concentration polarization (Figure 7). Typical operating patterns of
ultrafiltration are shown in Figure 5c.

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Figure 4: Concentration Polarization at a Membrane Surface. Cw is the Solute

Concentration at the Membrane Surface and Cb, is the
Bulk-Solute Concentration

Figure 5: Typical Dependence of Membrane Flux. (a) Applied Pressure Difference,

(b) Solute Concentration, (c) Cross-Flow Velocity

Solution containing macromolecular gel-forming solute will form a gel on the surface of
the membrane. The gel formation will contribute to formation of dynamic membranes.
The mechanism is as follows:

Due to convective flux through the membrane a concentration of the solution at the
surface Cw increases and eventually reaches a gel formation concentration Cg (Figure
5b). The flux, J through the membrane depends on a concentration according to the
relationship:

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Cw
J = k .n (4)
Cb

Combining Equations (1) and (4),

Cw ∆P
=
v(R m + R p )k
.n (5)
Cb

As long as concentration Cw is less than Cg, Cw, will increase with pressure, but the
moment Cw, equals Cg, an increase in ∆Ρ brings about an increase of the layer
resistance Rp, and the flux will no longer vary with pressure (Figure 5a).

Assuming no fouling effect, the membrane resistance Rm can be calculated from the flux
equation below:
∆Ρ
J= (6)
v.Rm

1
The slope obtained from the plot of flux, J versus ∆Ρ is equal to
v.R m

The retention of any solute can be expressed by the rejection coefficient, R.

1n(C f / C0 )
R =
1n (V0 / V f )
(7)

Where, C f is final macrosolute concentration in the retentate, C 0 is initial macrosolute

concentration, V0 is initial volume and V f is final retentate volume.

This expression assumes complete mixing of retentate seldom accomplished due to

concentration polarization. The apparent rejection coefficient depends on factors
affecting polarization including UF rate and mixing. For material entirely rejected, the
rejection coefficient is 1 (100% rejection); for freely permeable material it is zero.

Rejection is a function of molecular size and shape. Nominal cut-off levels, defined with
model solute, are convenient indicators. % Removal can be calculated from the relation:

% Re moval =
(Concentration in feed − Concentration in permeate) x 100
Concentration in feed
 Cf − Cp 
=   x 100
 Cf 

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where Cf = Concentration in feed

Cp = Concentration in permeate

Fractional rejection by membranes with low MW cut-off spans a narrower range of

molecular size than by more open membranes. For maximum retention of a solute,
select a membrane with nominal cut-off well below the MW of the species.

Many biological macromolecules tend to aggregate so that effective size may be much
larger than native molecule, causing increased rejection.

There are various laboratory applications of ultrafiltration (UF) systems, such as:
• Apple juice clarification
• Pineapple/lime/orange/sugar cane juice clarification
• Clarification of fermentation broths
• Enzyme separation and concentration

13.3 DESCRIPTIONS AND ASSEMBLY

13.3.1 MEMBRANES AND MEMBRANE HOUSING

The P.C.I tubular B1 system provides the user with a robust and proven module with a
wide range of fully interchangeable membrane elements. The design permits simple,
rapid, and inexpensive replacement of membranes by the user without the need to
return the equipment. Each module comprises 18 perforated stainless steel tubes,
fabricated in the form of shell and tube configuration, each tube lined with a membrane
element. Turbulent flow of that process fluid through each of the tubes is affected by the
specially designed end caps connecting all eighteen tubes in series.
The open channel, highly turbulent flow design allows a wide variety of process fluid to
be concentrated. It also allows simple clean-in-place techniques to be entirely effective.

FIGURE 6: MODULE ASSEMBLY

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The FD-12 unit is supplied with a P.C.I ES625 Polyethersulfone membrane for the
ultrafiltration operations. The ES625 Polyethersulfone membrane is rated with apparent
retention character of 25000 MWCO.

13.3.2 PUMPS

Two pumps are provided with the FD-12 unit:

i) LOWARA CENTRIFUGAL PUMP - MODEL CEAM 70/3

The Lowara Centrifugal Pump is used to circulate the liquid from the plate heat
exchanger to the water tank.

Specifications:
Maximum flow rate : 80 LPM
Maximum head : 22 m
Max. working pressure : 8 bars
Max. liquid temperature : 110 °C
Speed : 2800 rpm
Power : 0.37 kW (0.5 HP)

ii) CAT Triple Plunger Pump - Model 241

The CAT Triple Plunger pump is used to pump the liquid from the feed tank into the
Ultrafiltration Module.

Specifications:
Maximum flow rate : 13 liter/min.
Working pressure range : 7-85 bar
Max. fluid temperature : 71 °C
Max. speed : 1725 RPM
Max. horsepower : 3.0 HP

A Pressure regulator is also installed to regulate the operating pressure of the feed
system.

13.3.3 TANKS AND HEATING/COOLING SYSTEM

The FD-12 unit is supplied with a feed tank and a product tank, both having maximum
capacity of 15 liters. The feed and product tanks are made of stainless steel for
corrosion and chemical resistance. The retentate line is equipped with a unit of
FLATPLATE FP5X12-14 plate Heat Exchanger (Figure 7). The detail specifications can
be found in appendix D.

13.3.4 WATER FLOW METER

The FD-12 unit is supplied with a CT Platon water flow meter.

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13.4 OPERATING PROCEDURES

13.4.1 CONTROL VALVES

In order to prevent damage to any parts of the FD-12 unit, it is very important to fully
understand the process flow diagram (Figure 7) of the system prior to operating. The
correct flow of fluid is achieved by setting the appropriate valves in the correct direction.
The FD-12 unit has been installed with 2-way and needle valves as follows:

Item Description Type

V1 Controls product tank outlet flow into the 2-way
plunger pump

V2 Controls feed tank outlet flow into the plunger 2-way

pump
V3 Product tank drainage valve 2-way
V4 Feed tank drainage valve 2-way
V5 Flow shut off for maximum pressure setting 2-way

V6 Drainage valve 2-way

V7 Controls the UF retentate flow rate to vary ΔP Needle

V8 Drainage valve 2-way

V9 Plate Heat Exchanger Inlet 2-way

V10 Plate Heat Exchanger Outlet 2-way

V11 Bypass of the Plate Heat Exchanger 2-way

V12 Product Sampling 2-way

V13 Inlet to the Heating Tank 2-way

V14 Heating Tank Drainage 2-way

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13.4.2 PUMPS AND PRESSURES

i) CAT TRIPLE PLUNGER PUMP

1. In order to set the maximum working pressure, close valve (V5).

2. Be sure that the feed tank is not empty. Open valve (V2) and then switch on the
plunger pump (P1). Observe the pressure gauge (PG1) located next to the pressure
regulator (PR1). The pressure will rise steadily until it reaches the previously set
pressure.

3. Using a wrench, adjust the pressure regulator to obtain the desired maximum working
pressure (clockwise to increase pressure; counter-clockwise to decrease pressure).

4. Re-open the valve (V5) for the liquid to flow.

NOTE: If the pressure fails to increase or keeps dropping, there must be air trapped in
the membrane system. Shut off the pump and let the air to escape. Make sure no air
being introduced into the system.

ii) HEAT EXCHANGER

The FD11 Cross Flow Membrane Filtration System is equipped with a FLATPLATE plate
heat exchanger. If the user decides to heat up the feed liquid before entering the
membrane, valve (V9) and (V10) will be opened whereas valve (V11) is to be closed.
The opposite will apply should feed heating is not required in the operation.

The FLATPLATE Plate Heat Exchanger is connected to a heating tank. Please ensure
that the liquid level inside the tank is always above the heater element. Set the desired
temperature at the temperature controller on the control panel. Switch on the centrifugal
pump (P2) to circulate the liquid through the heat exchanger.

iii) DRAINING THE LEFTOVER

Before flushing the membrane, the leftover liquid has to be completely drained after
each session in order to prevent bacterial formation overnight. There are six drainage
points provided with the FD-12 unit. For a complete drainage of the system (excluding
the heating tank), open valves (V3), (V4), (V6), and (V8).

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FIGURE 7: A SCHEMATIC DIAGRAM OF

ULTRAFILTRATION UNIT

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FIGURE 8: A VIEW OF THE ULTRAFILTRATION UNIT

13.4.3 DETERMINATION OF MEMBRANE RESISTANCE, RM

OBJECTIVE

The objective of this experiment is to find out Membrane resistance Rm by using

deionized water.

PROCEDURES

1. Before starting, be sure to set the correct maximum working pressure. Maximum
pressure of 13.5 bars shall be set when running through the UF membrane.
2. In order to set the maximum working pressure, close valves (VI) to (V5) and fill up
the feed tank with tap water. Then, open valve (V2) and start the plunger pump (PI).
Observe the pressure gauge (PG1) installed next to the pressure regulator (PR1).
Using a wrench, adjust the pressure regulator to the desired maximum working
pressure. Stop the plunger pump and re-open valves (V2), (V4), (V5) and (V6) to
drain off the water in the tank.
3. Fill the feed tank with de-ionized water. Check and make sure that all valves are in
the correct positions.
4. Vary the differential pressure by adjusting the needle valve (V7), from 1 to 5 bar by
increament 0.5 bar and permeate flux is to be calculated from volume collected in the
obsereved time period.
5. Plot permeate flux J vs ∆P

Note:
a) The effective membrane area is 0.9m2
b) The membrane must be cleaned before operation to avoid membrane
fouling which could affect the result.

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Calculate the membrane resistance, Rm from the slope of the graph which is equal to
1
.
v.Rm

13.4.4 ULTRAFILTRATION: CLARIFICATION OF ORANGE JUICE

OBJECTIVE

The objective of the experiment is to clarify orange juice by ultrafiltration and to find out
the operating parameters for removal of high molecular weight solids contained in juice
by ultrafiltration.

PROCEDURES

1. Make a calibration curve of orange juice concentration vs spectrophotometer

readings as X and Y axis respectively by taking various concentration of juice e.g.
0.1, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8 and 2.0 %.
2. Orange juice of 1 % and 2 % are to be made in deionized water to make each
solution of 10 liters in volume for experimental run of ultrafiltration unit.
3. Set the maximum working pressure at 13.5 bars.
4. Make sure that all valves are in the correct positions.
5. Fill up the feed tank with 10 liters of filtered sugar cane juice solution. The feed shall
always be maintained at room temperature. Switch on the centrifugal pump (P2) to
circulate the cold water through the plate heat exchanger.
6. Start the plunger pump. Set membrane inlet pressure to 1 bar by adjusting valve
(V7).
7. Record the flux of the filtrate over time (at least 15 minutes). Record the outlet or
retentate pressure. Record the inlet flow rate from the flow meter. Record
concentration of orange juice solids in feed and permeate solution from
spectrophotometer readings.
8. Stop the plunger pump and close valve (V2). Mix all the filtrate and retentate back in
the feed tank.
9. Repeat steps 4 to 7, at this time vary the inlet pressure between 1-5 with increase of
0.5 bar by manipulating the retentate control valve (V7). Determine the flux at various
pressure ranges and % Removal of solids at a particular flow rate.
10. Repeat steps 4 to 7, at this time vary the flow rate between 2 to 10 liters/min with
increment of 2 liters at each stage.
11. Plot flux vs operating pressure, ∆P on Y and X axis at various flow rates.
12. Plot % Removal vs operating pressure, ∆P at different flow rates.
13. Graphs and Results are to be obtained for both 1 % and 2 % orange juice
concentrations.

Note: Discussion is to be done for each graph and results should be in tabulated form.

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13.4.5 CLEANING OF THE MEMBRANE

After the experimental runs the membrane unit is to be cleaned with 0.5% NaCl solution
at 500C by recirculating the salt solution for 15 minutes.

13.5 SAFETY AND MAINTENANCE

PUMPS LIMITS

The centrifugal pump has a maximum operating pressure of 8 bars. On the other hand/
the plunger pump has a working pressure range of 7 to 85 bars. However, in order to
protect the membranes, it is advisable to always operate the pumps below the pressure
limits of the respective membranes. The pressure relieve valve (PR1) shall be adjusted
such that the maximum working pressure of the plate heat exchanger is not exceeded.

MEMBRANE LIMITS

a) The maximum operating pressures is 15 bars. The operating temperature shall not
exceed 70 °C.
b) Operation of membranes at maximum limits of pressure or temperature will affect
their subsequent performance at lower temperatures and pressures. In addition, it
is
not advisable to operate at the limits of temperature and pressure at the same time.
c) Test conditions determine the precise retention character.
d) A wider pH range can be used for cleaning membranes.

CONTROL VALVES

All valves must be set at the correct positions in order to avoid possible damage to the
unit.

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