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Department of Chemical Engineering

Talamban, Cebu City, Philippines 6000

Individual Laboratory Report


(Form CHEL-3)
Laboratory Course : CHE 512L Chemical Engineering Laboratory 2
Experiment Title : Filtration: Plate-and-Frame Filter Press
Student’s Name & Signature : Solatorio, Mark Vincent S.
Scheduled Date : September 04, 2019
Date Performed : September 04, 2019
Date Submitted : September 19, 2019
Submission Number : 1
Teacher’s Name : Engr. Kramer Joseph A. Lim
Term and Academic Year : First Semester 2019-2020

Data Processing and Results Grade


Introduction (x0.20)
Methodology (x 0.20)
Presentation of Results (x 0.20)
Discussion of Results and Conclusions (x 0.20)
Writing Style (x 0.10)
Appearance and Formatting (x 0.10)
Grade

Assessed and Graded By: ENGR. KRAMER JOSEPH A. LIM


(Signature over printed name)
Date and Time
School of Engineering
Talamban, Cebu City, Philippines

CHE 512L
Chemical Engineering Laboratory 1

FILTRATION
(Plate and Frame Filter Press)

A laboratory report submitted to

Engr. Kramer Joseph A. Lim


CHE 512L Instructor

by

Solatorio, Mark Vincent S.

September, 19 2019
1. Introduction
Filtration is a process of removing solid particles from a fluid (may be liquid or gas) by allowing the fluid
to pass through a porous medium that retains the particles as separate phase (Geankoplis, 2015). Particles
with sizes small enough will pass through the medium thereby leaving large particles retained. The flow of
the fluid is driven by the pressure difference between the medium which can be done by means of fluid
pressure upstream (pressure filters) or suction downstream (vacuum filters). Due to the different sizes of
solids to be filtered, wide range of filter designs is needed. Filters are classified into cake filters, clarifying
filters, and crossflow filters (Sutherland, 2008).
A filter medium is any material that under operation conditions of the filter, is permeable to one or more
components of the mixture, solution or a suspension, and is impermeable to the remaining components
(Sutherland, 2008). The selection of the filter media is very important. Some factors that must be taken into
consideration in choosing the filter media are the following: (1) It must retain the solid to be filtered, giving
reasonable clean filtrate; (2) it must not plug or bind; (3) it must not react to the fluid being filtered or other
substances present during filtration; (4) it must permit cake formed to discharge cleanly and completely; (5)
it must be cost friendly. Commonly used industrial filter cloth are canvas, and duck or twill weave (McCabe,
Smith, & Harriott, 1993).
In filtration, solid particles are separated from the fluid as it passes through the filter medium. Particles
having size smaller than the spaces (mesh) of the filter media passes through, and particles having larger
size are retained. The clear liquid that passes through the filter cloth is called the filtrate. The retained particles
would then build up forming cake. The cake formed induces resistance to flow and would have certain
maximum permeability. The total pressure drop of the system will then be changed because of the
resistances induced by the filter cloth and the cake as can be shown in Equation 1.
∆𝑃 = ∆𝑃𝑚 + ∆𝑃𝐶 (𝐸𝑞𝑛. 1)
Where ∆𝑃, ∆𝑃𝑚 , 𝑎𝑛𝑑 ∆𝑃𝐶 are the total pressure drop, pressure drop in the medium, and pressure drop in the cake
respectively in (N/m2).

For the filtration process driven by a constant pressure difference, assuming that the flow of filtrate
through the porous medium is laminar, and that the cake formed is incompressible, the Carman-Kozeny
equation can then be reduced into the following form:

𝑑𝑉 −𝐴∆𝑃𝑎𝑣𝑒
= (𝐸𝑞𝑛. 2)
𝑑𝑡 𝜇 (𝛼𝑐𝑠 𝑉 + 𝑅 )
𝐴 𝑚

Where 𝑉 is the volume of the filtrate (m3) collected (which can be calculated from the mass obtained and the
measured filtrate density), 𝑡 is filtration time in seconds, 𝐴 is the filtering area in 𝑚2 , ∆𝑃𝑎𝑣𝑒 is the average
pressure across the system in N/m2 , 𝜇 is the viscosity of the filtrate at the measured temperature in kg/m∙s
, 𝐶𝑠 is the calculated slurry concentration (kg solids/m3 slurry) ,𝛼 is the specific cake resistance (m/kg), and
𝑅𝑚 is the filter medium resistance with units m-1.
Rearranging Eqn. 1 and integrating from t = 0 to a certain time t, we get the linearized form of the
constant-pressure equation as:
𝑡 𝐾𝑝
= 𝑉+𝐵 (𝐸𝑞𝑛. 3)
𝑉 2

Where 𝐾𝑝 (s/m6) is an empirical constant and 𝐵 (s/m3) is directly related to the 𝑅𝑚 term. Upon inspection,
𝑡
Equation 2 is in the form of 𝑦 = 𝑚𝑥 + 𝑏 and thus, is in a form such that when 𝑉 is plotted against 𝑉, 𝐾𝑝
would then be equal to two times the slope with 𝐵 being the y-intercept. Thus, when we evaluate these
constants, given the equation of the line, we can solve for the specific cake resistance (𝛼) and filter medium
resistance (𝑅𝑚 ). When we get 𝐾𝑝 , we can consequently solve for the 𝛼 term using:

𝐾𝑝 𝐴2 (−∆𝑃𝑎𝑣𝑒 )
𝛼= (𝐸𝑞𝑛. 4)
𝜇𝐶𝑠

Likewise, upon getting the slope, we can then solve for the 𝑅𝑚 term using:

𝐵𝐴(−∆𝑃𝑎𝑣𝑒 )
𝑅𝑚 = (𝐸𝑞𝑛. 5)
𝜇

Further calculations made allows us to solve for the cake resistance (𝑅𝑐 ) via the equation below:

𝛼𝑐𝑠 𝑉
𝑅𝑐 = (𝐸𝑞𝑛. 6)
𝐴

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2. Objectives of the Experiment
Determine the specific cake resistance and filter medium resistance in the filtration of aqueous CaCO 3
slurries with different concentrations performed at constant-pressure condition.

3. Methodology
3.1. Methodological Framework
Figure 1 shows the schematic diagram of determining specific cake resistance, filter medium resistance,
and cake resistance. The data on the frame dimensions, temperature, mass of filtrate, and mass of CaCO3
cake are collected. Filtering area, total filtering area, density of filtrate, viscosity of filtrate, and slurry
concentration are then determined. Time is determined at every 400 grams of filtrate collected and t/V against
V plot is generated using the mass of filtrate data divided by the density. From the generated plot, the slope
and y-intercept is then determined. The determined slope is then used to determine parameter 𝐾𝑝 and is
used in Equation 4 along with the other determined data do get specific cake resistance (𝛼). y-intercept is
used to determine parameter 𝐵 and is used in Equation 5 along with other determined data to get filter
medium resistance (𝑅𝑚 ). 𝛼 is then used to determine the cake resistance (𝑅𝐶 ).

Plot t/V Determine specific Specific cake


Volume of Filtrate Slope resistance
against cake resistance,
Time filtrate y-intercept medium Cake resistance
volume resistance, cake
Filter medium
resistance

Figure 1. Methodological Framework in Determining Specific Cake Resistance, Filter Medium


Resistance, and Cake Resistance.

3.2. Materials
The materials used in the experiment are calcium carbonate (CaCO3) and water. Calcium carbonate
and water are weighed according to the concentration of the slurry that will be created. The materials
are mixed in the slurry tank to ensure complete and equal mixing of solid particles. The equipment used
is a plate-and-frame filter press. Four canvas cloth were used as filtering media. A pail is used as the
container for filtrate, and a top loading balance is used to measure the mass of the filtrate collected.

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3.3. Equipment
Plate-and-frame filter press is used in the experiment. Figure 2 shows the set up used for filtration.

Figure 2. Filtration Set – Up


The motor drives the agitator to ensure equal distribution of solid particles inside the tank. The slurry
tank contains the slurry that will be filtered. Outlet valves regulates the flow of slurry coming out of the
slurry tank. Pump induces the flow of slurry towards the filter medium. Pressure gage determines the
pressure drop between the filter plates. Frames provides support for the filter cloth during the filtration
process. Tightening screw, and lock bar ensures that the filter press is tightly pressed. Plates will
contain the cake formed after filtration. Filtrate outlet is where the filtrate passes to ensure that the
filtrate that will be connected will go to the container. In determining the density of the filtrate, a
densitometer was used.

3.4. Procedures
Prior to the preparation of 10% and 14% slurry, the mass of the calcium carbonate and water was
determined. Samples containing 10% and 14% slurry were prepared using 10.0076 grams, and 14.0332
grams of CaCO3 in 90.1304 grams, and 86.05 grams of water respectively. The densities of the samples are
then determined using a densitometer. The exact masses of water and CaCO3 that will be used to prepare
20-L 10% and 14% slurry are then determined using the measure densities of the sample.

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Prior to the filtration process, the set-up is cleaned three times by using tap water in each run. In each
run a pail was placed under the filtrate outlet to contain the liquid. After making sure that the filtration set up
is clean, filter cloth was then used to cover the filter frame and plate in an alternating manner (frame-cloth-
plate-cloth-frame). Lock bar was then installed to press the plate-and-press and a lock bar was used to ensure
that the set-up is tightly pressed. A pail on top of a top-loading balance was then placed under the filtrate
outlet. Pre-weighed water was then put into the slurry tank. The agitators are turned on, and the measured
CaCO3 are then mixed in a gradual addition manner to ensure no clumping of CaCO3. The slurry was allowed
to mix for 5 minutes inside the tank. After five minute, the pump was turned on and the outlet slurry valves
was opened. The recycle valve was then adjusted to maintain a constant pressure drop of 5 torr.

The timer is started upon the first drop of liquid in the container. Time is recorded for every 400 grams
of filtrate collected. The pressure was recorded for every 30 seconds, and is adjusted if the pressure reading
exceeds or goes lower thank 5 torr. When the slurry tank is almost empty (no slurry can be seen in the bottom
the tank) 1 gallon of tap water was added into the slurry tank. Sample of filtrate was then collected and the
density is then determined. The density determined was then used to get the volume of filtrate. t/V is then
plotted against V and the slope is then determined. The temperature of the filtrate was also recorded (this
was used to determine the viscosity of the filtrate assuming it was water). After little to no droplet was
collected, the pump was turned off and the filter cakes were collected. Using a steel tray, the filter cakes were
transferred from the press to the oven. The filter cake for 10% slurry was then allowed to dry for 4 hours at a
temperature of 100℃. Same process was done for the 14% slurry, but the time of drying was 24 hours, and
at a temperature of 100℃. The masses of the dried filter cakes are then measured and recorded.

The determined slope is then used to determine parameter 𝐾𝑝 and is used in Equation 4 along with the
other determined data do get specific cake resistance (𝛼). y-intercept is used to determine parameter 𝐵 and
is used in Equation 5 along with other determined data to get filter medium resistance (𝑅𝑚 ). 𝛼 is then used
to determine the cake resistance (𝑅𝐶 ). The masses of the filter cakes are then used to determine 𝑐𝑆 and is
used in Equation 6 to determine 𝑅𝐶 along with the other parameters.

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4. Results and Discussions

4.1 Filtration time and volumetric flowrate with respect to slurry concentration

The filtration time approximately took about 79 minutes and 191 minutes for the 10% and 14% CaCO3
slurry, respectively. Longer filtration time was observed for the 14% CaCO3 slurry since more cake was
formed, thus offering greater resistance to fluid compared to the 10% CaCO3 slurry. For the same reason, it
can be expected that the filtrate volume collected is higher for the lower slurry concentration. Figure 3 shows
the plot of filtrate volume collected against time.

0.018

0.016

0.014
Filtrate Volume (m3)

0.012

0.010

0.008 10%
14%
0.006

0.004

0.002

0.000
0 2000 4000 6000 8000 10000 12000 14000
Time (sec)

Figure 3. Plot of collected filtrate volume against time for 10% and 14% CaCO3 slurries

Increase deposition of CaCO3 results into an increase in resistance. Filtrate volume collected per unit of time
is lower in the higher concentration due to the higher resistance from cake build up to filtrate flow. It can be
observed in the figure above that a steeper curve was achieved for the 10 weight % CaCO3 slurry
concentration. Thereby, the slope of the 10% CaCO3 slurry is steeper compared to the 14% CaCO3 slurry.

The data of the filtration time and collected filtrate volume are used in Equation 2 to generate the
linearized equation derived earlier in Section 1.

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4.2 Monitoring of pressure during filtration

5
Pressure Drop (psig) 4

0
0 1000 2000 3000 4000 5000
Time(sec)

Figure 4. Graph of pressure drop against time for 10% (w/w) slurry

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Pressure Drop (psig)

0
0 2000 4000 6000 8000 10000 12000
Time(sec)

Figure 5. Graph of pressure drop against time for 14% (w/w) slurry

In figures 4 and 5, fluctuations in pressure drop can be observed as depicted by the blue line. The red line
indicates the average pressure of 4.9740 pisg and 5.0435 psig for 10% (w/w) and 14% (w/w) slurry
respectively. An increase in cake resistance happens as cake builds up inside the filter plate resulting to an
increase in pressure drop. This explains the fluctuations that can be seen in figures 4 and 5. As filtration goes
to completion less solution is pumped into the filter medium causing the decrease in the pressure drop. During
the experiment, the recycle valve was adjusted to maintain a constant pressure.

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4.3 Reciprocal of the volumetric flow rate and volumetric flow rate with respect to slurry
concentration
900000

800000

700000

600000
t/V (sec/m3)

500000

400000 10%
y = 30000000x + 34044 14%
300000 R² = 0.9994

200000

100000 y = 12888896x + 71638


R² = 0.988
0
0.000 0.002 0.004 0.006 0.008 0.010 0.012 0.014 0.016
V(m3)

Figure 6. Graph of t/V against the filtrate volume of 10% and 14% CaCO3 slurries with selected points
used in the determination of the resistances

Figure 6 shows the graph of t/V against the filtrate volume of 10% and 14% CaCO 3 slurries with selected
points used in the determination of the resistances. In obtaining the specific cake resistance, cake resistance
and the filter media resistance, the points in the linear region are carefully selected since Equation 2 can only
be used for the data points representing a linear trend. The slope and y-intercepts are acquired to obtain the
empirical constants 𝐾𝑝 and B, respectively. Figure 4 shows the selected points ( and ) used in the
determination of the resistances.

There are regions where the data points deviate from linearity. Most of these are found in the first
and last points. According to Tarleton et al (2006), the nonlinear region at the start represents the region
where filter medium resistance is dominant, since the cake has not been formed yet. This nonlinearity is said
to be the result of the permeability k of the filter cake still not constant in the initial stages of filtration according.
Non-linearities may also be observed at the start and towards the end of filtration. This is due to one or more
factors. At the start, the filter plate is not yet fully occupied. This would result to a higher volumetric flow rate.
When the chamber is full of cake, the filtrate volume collected in any time interval is reduced; if a cake has
been formed and the slurry being fed is completely used, the applied pressure difference serves to deliquor
the cake, and again reducing the filtrate volumetric flowrate.

Equation 3 represents the regions between the blackened points due to the linearity of the data
points. The values for the slope or Kp/2 are 12888896 and 30000000 for the 10% and 14% CaCO3 slurry,
respectively. The t/V-intercept values (B) are 71638 and 34044 for the 10% and 14% CaCO3 slurry,
respectively.

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As can be observed in Figure 6, (t/V) value for 14% (w/w) slurry is lower than that of the 10% (w/w)
until the red dot. Operating at high pressure may speed up dewatering process or increases solid
concentration in the cake. An increase in solid concentration decreases cake permeability. During the initial
time of filtration, the former predominates (Rushton, Ward, & Holdich, 1996). Speeding up dewatering
process means higher volume at a certain time which gives a low time to volume ratio. After the red dot, time
to volume ratio of 10% (w/w) slurry became lower than that of the 14% (w/w) slurry.

4.4 Determination of the specific cake resistance, cake resistance, and filter medium resistance

The specific cake resistance 𝛼, cake resistances Rc, and filter medium resistance Rm were
determined for each concentration of the CaCO3 slurry with their corresponding % differences and are
summarized in Table 1.

Table 1. Obtained filtration parameters from experimental determination


Filtration Parameter 10% CaCO3 slurry 14% CaCO3 slurry % Difference
Specific cake resistance, 𝛼 (m/kg) 6.43529 × 1011 1.04898 × 1012 47.91
Filter medium resistance, Rm (m-1) 1.47958 × 1012 7.05618 × 1011 70.84
Cake resistance, Rc (m-1) 8.71217 × 1012 1.96586 × 1013

The specific cake resistance α describes the amount of resistance to flow per unit of solid processed
per unit area and it is independent on thickness. It is solely dependent on the physical properties of the solid
(particle size, shape, cake porosity, and particle density), so that it is constant for every solid regarding the
concentration of the solids present (McCabe, Smith, & Harriott, 2005). In addition, it may also vary with
pressure for incompressible cakes, but for the experiment performed, the compressibility of the cake was not
investigated because pressure was held constant so an assumption was made that the cake was
incompressible.

The filter medium resistance Rm is defined by the ratio of the thickness to the permeability of the filter
medium. It is a function of the properties of the filter medium and the equipment used. It can then be expected
that for both filtration runs, the values of the filter medium resistance are equal since the same filter mediums
and equipment were used. Rm may vary with the age and the cleanliness of the filter medium used since its
pores might be clogged by some solid particles trapped in the medium matrix (McCabe, Smith, & Harriott,
2005).

The cake resistance, Rc is function of the concentration of the slurry. The cake resistance is much
greater at 14 wt% than that at 10 wt% CaCO3 slurry. This is because thicker cake was formed in 14
wt% CaCO3 compared to 10 wt% CaCO3 slurry offering more succeeding layers for the filtrate to pass
through (Brown, et al., 1973).

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5. Conclusions
In the filtration of aqueous calcium carbonate slurries of varying concentrations maintained at a constant
𝑚
pressure of about 5 psig, the specific cake resistance (𝛼) were found to be 6.43529 × 1011 𝑘𝑔 for the
𝑚
10% by weight CaCO3 slurry and 1.04898 × 1012 𝑘𝑔 for the 14% by weight CaCO3 slurry. Ideally, the 𝛼
values should be constant for both slurry concentrations. For the given experiment, a percent difference of
about 47.91% was found.

The filter medium resistance (𝑅𝑚 ) were found to be 1.47958 × 1012 𝑚−1 and 7.05618 ×
1011 𝑚−1 for the 10% and 14% CaCO3 slurries, respectively. The percent different between the two filter
medium was found to be 70.48%.

It was further determined that the cake resistance values for the 10% by weight and 14% by weight
CaCO3 slurries were 8.71217 × 1012 𝑚−1 and 1.96586 × 1013 𝑚−1 , respectively. It is evident that for
a CaCO3 slurry of greater concentration, more cake is formed; thereby introducing a greater resistance to the
filtration system.

6. References
Geankoplis, C. J. (2015). Transport Processes & Separation Process Principles. Philippines: Pearson Education
South Asia PTE. LTD.

McCabe, W. L., Smith, J. C., & Harriott, P. (1993). Unit Operations of Chemical Engineering. Singapore:
McGraw-Hill Book Co.

Rushton, A., Ward, A., & Holdich, R. G. (1996). Solid - Liquid Filtration and Separation Technology. New
York: VCH Publishers Inc.

Sutherland, K. (2008). Filters and Filtration Handbook. Hungary: Elsevier Ltd.

Tartleton, E. S., & Wakeman, R. J. (2007). Solid/Liquid Separation: Equipment Selection and Process
Design. Great Britain: Elsevier Ltd.

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ANNEX

Data Processing & Analysis Report

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