Department of Chemical Engineering University of San Carlos Technological Center Nasipit, Talamban, Cebu City

ChE 512L Chemical Engineering Laboratory 2

FILTRATION (Plate and Frame Filter Press)

A final report submitted to Engr. Ramelito Agapay Instructor, ChE 512L

By

Pinton, Noel Jeffrey

September 21, 2011

Introduction

Filtration Filtration is a kind of solid liquid separation process which employs a filter medium which permits the passage of molecules that are smaller than its pores. Since solids are generally larger than liquid molecules, filtration is used in order to separate them from a mixture. A pressure difference is set up that causes the fluid to flow through the filter medium where the solids are blocked from passage and a porous cake of solid is formed in the filter medium while the liquid pass through and called filtrate. The desired product of filtration could be the filter cake or the outlet fluid or filtrate and in either case, the slurry or cake should have a large percentage of solids and the filtrate should have trace amounts of suspended particles. There are two modes of filtration, the constant-pressure and constant rate filtration. Carman and Kozeny established a relation which relates rate of filtration with the pressure difference as the driving force of filtration and cake and filter media as resistances. (1)

Most of filtration operations are operated in constant-pressure conditions. Equation (1) can be inverted and rearranged to give (2) By integration and dividing by V, we get (3) where and , is the viscosity of the liquid (Pa-s), is

the specific cake resistance (m/kg), CS is mass solids/volume of filtrate (kg/m3), A is the filter area (m2), -p is the pressure difference (Pa), Rm is the filter medium resistance (m-1), V is the volume of the filtrate (m3) and t is the time of filtration (sec).

Depending on the type of solid, proportion of the liquid to the solid in the mixture, the viscosity of the fluid and other factors, different types of filtration system is used for the separation process. In this experiment, a plate and frame filter press is utilized for the separation of CaCO3 and water. Plate and Frame Filter Press Plate and filter presses are one of the important types of filters. These filters consist of plates and frames assembled alternately with a filter cloth over each side of the plates (Geankoplis, 2003). Each plate has channels for the filtrate to pass through. The slurry is pumped into the press and flows through the duct in to each of the open frames so that the slurry fills the frames. The filtrate passes through the filter cloth while the solids remain building up a porous cake. The filtration proceeds until the frames are completely filled with solids. When the frames are full, the frames and plates are separated and the cake is removed. The separation of the frames and plates and the removal of the cake consume labor cost and time, this is a common disadvantage of a batch process like this kind of filtration. Insert image of filter blah.

Objective Determine the specific cake resistance and filter medium resistance in the filtration of aqueous CaCO3 slurries with different concentrations performed at constant-pressure condition.

Materials and Apparatus Plate and Frame Filter Press Frame Dimensions: Height Length Width Pressure Gauge: Slurry Tank Capacity: 180 mm 180 mm 25 mm

5 psi (maximum) 60 liters

Oven Pails Weighing Scale (30 kg) Stopwatch Thermometer CaCO3 powder Water Ruler

Procedure Preparations Twenty liters of slurry of 10% by weight was prepared by mixing CaCO3 powder and tap water. The slurry was stirred and poured into the slurry tank as quick as possible to prevent the settling of CaCO3 in water. A pail was mounted on a weighing scale with a 30-kg capacity and was placed underneath the filtrate outlets. The filtering area of the plates was measured using a ruler then each face of every plate was covered with a piece of filter cloth. The temperature of the slurry was taken before the filtration proper is started.

Filtration Proper The agitator and filter press was switched on. As soon the first drop of filtrate fell the time was started. The time was recorded for every 400 g of filtrate collected in the pail. The pressure was kept constant by the regulation of the recycle valve in the slurry tank. The operation was stopped when there was very little amount of filtrate coming from the outlets. Washing and Filter Cake Removal After the operation was stopped one gallon of tap water was poured in the slurry tank to start the washing of the cake. The pump was switched off when no more water comes out from the filtrate outlets. The cake was carefully removed retaining its shape from the frames by holding a pre-weighed aluminum tray below. The cake was dried in an oven for 4 hours at 100 C. The mass of the dried cake is weighed afterwards. The experiment was repeated using 20 liters of 14 % by weight CaCO3 slurry.

Results and Discussion The results of the experiment are presented below by plotting the mass of the filtrate taken and time:

16 14 mass filtrate (kg) 12 10 8 6 4 2 0 0.0 250.0 500.0 750.0 filtration duration (sec) 1000.0 1250.0 1500.0

Figure 2. Plot of filtrate mass and filtration duration of 10 wt% CaCO3 slurry

10 9 8 mass filtrate (kg) 7 6 5 4 3 2 1 0 0.0 500.0 1000.0 1500.0 filtration duration (sec) 2000.0 2500.0 3000.0

Figure 3. Plot of filtrate mass and filtration duration of 14 wt% CaCO3 slurry

As seen from the graphs, the time interval to collect 400 g of filtrate increases when the mass of the total filtrate collected increases. The cake that is formed inside the frames contributes to the increased interval of filtrate collected. As expected, the slurry with the higher concentration fills the frames with solids first as to hinder the collection of the filtrate as seen in Figure 3 where starting at t = 1000 secs the filtrate collection proceeds very slowly. These points are neglected in the calculation of the resistances of the cake and filter medium. The mass of the filtrate water is converted to its equivalent volume based on its density using the recorded temperature. Using the Carman-Kozeny equation, the graphs in figures 2 and 3 are converted in to plots of time/volume of filtrate versus volume of filtrate which are presented below.
100000.0 90000.0 80000.0 70000.0 t/V (sec/m3) 60000.0 50000.0 40000.0 30000.0 20000.0 10000.0 0.0 0.0000 0.0020 0.0040 0.0060 0.0080 V (m3) 0.0100 0.0120 0.0140 0.0160 y = 5E+06x + 17776 R = 0.9916

Figure 4. Plot of t/V and V of 10 wt% CaCO3 slurry

120000.0 y = 1E+07x + 23352 R = 0.9972

100000.0

80000.0 t/V (s/m3)

60000.0

40000.0

20000.0

0.0 0.0000

0.0010

0.0020

0.0030

0.0040 V (m3)

0.0050

0.0060

0.0070

0.0080

Figure 5. Plot of t/V and V of 14 wt% CaCO3 slurry

The slope and the intercept of the regressed points are used in order to calculate for the specific cake resistance and the filter medium resistance. The results are shown in the table below.
Table 1. Specific cake resistance and Filter medium resistance

CaCO3 slurry 10 wt% 14 wt%

Cs (kg/m3) 130.11 236.80

(m/kg) 2235455.63 2794308.08

Rm (m-1) 4771469.47 5870389.14

The specific cake resistance slightly increased when the concentration of the slurry is increased based on the results of the experiment. Specific cake resistance is a function of porosity and the specific surface area of the solid particle So (Geankoplis, 2003). In the experiment, the same solid is used in the two runs therefore the specific surface area is the same. A decrease in porosity increases the specific cake resistance. The porosity can be affected by pressure but since pressure is kept constant all throughout the experiment. In the experiment, the specific cake resistance is expected to be the same for both trials. A factor on the experiment is

considered for not meeting the expectation. Comparing figures 2 and 3, it is observed that during the filtration of the 14 wt% CaCO3 slurry, it can be said the operation finished to completion denoted by the points that are considered outliers pinpointing that the porosity of the cake is very small because of compression. On the other hand, the filtration with the 10 wt% CaCO 3 slurry is stopped even before the porosity similar on the 14 wt% CaCO3 slurry run is reached. Therefore, at the end of each trial, the porosity of the first trial was higher than the second trial with the higher concentration. The filter medium resistance is a function of the filter medium and the material being filtered but the filter medium resistance in the experiment also increased with increased concentration of the slurry. Another factor which was disregarded during the experiment is that the filter medium used during the second trial of increased slurry concentration. The filter cloth of the first trial was reused during the second trial because fresh filter cloth used for the second run produced leaks in the set-up. Reused filter cloths are expected to have higher resistance to filtration because the pores may have already been clogged by the previous filtration and that the cloth may not have been washed thoroughly before it was used again. These clogged pores may alter the property of the cloth where the filter medium resistance is a function to.

Recommendations The filtration time should be long enough that there is no filtrate coming out of the filtrate outlet in order to ensure that the end of filtration conditions of both trials is the same. The filter cloth used should be fresh and should be identical on both trials. If the filter cloth is to be reused, it should be washed thoroughly to unclog the pores then dried.

Reference Geankoplis C. (2003). Principles of Transport Processes and Separation Processes. Prentice Hall, New Jersey.

Appendix
Table 2. Raw Data for 10 wt% CaCO3 slurry

Mass Filtrate (kg) 2 2.4 2.8 3.2 3.6 4 4.4 4.8 5.2 5.6 6 6.4 6.8 7.2 7.6 8 8.4 8.8 9.2 9.6 10 10.4 10.8 11.2 11.6 12 12.4 12.8 13.2 13.6

Time (sec) 64.0 81.0 87.0 106.0 126.0 148.0 170.0 211.0 221.0 248.0 279.0 311.0 343.0 378.0 413.0 452.0 494.0 536.0 580.0 624.0 672.0 717.0 765.0 814.0 871.0 924.0 986.0 1055.0 1129.0 1211.0

Table 3. Raw Data for 10 wt% CaCO3 slurry

Mass Filtrate (kg) 0.4 0.8 1.2 1.6 2 2.4 2.8 3.2 3.6 4 4.4 4.8 5.2 5.6 6 6.4 6.8 7.2 7.6 8 8.4 8.8 0.4 0.8 1.2 1.6 2 2.4 2.8

Time (sec) 10.0 25.0 44.0 67.0 91.0 122.0 152.0 187.0 228.0 269.0 311.0 359.0 406.0 463.0 523.0 582.0 648.0 726.0 820.0 995.0 1644.0 2793.0 10.0 25.0 44.0 67.0 91.0 122.0 152.0

Table 4. Operating Conditions and other Parameters

(Pa-s) A (m2) A2 (m4) (-p) (N/m2) Temperature (C)

0.001 0.11 0.012 2.45 26

Table 5. Drying of Cake

Tray # 1 (10% slurry) 2 (14% slurry) Sample Calculations Filtration Area

Mass of tray (kg)

Mass of tray and dry cake (kg)

Mass of dry cake (kg)

(number of filter medium) (4)

CS

Specific Cake Resistance

From figure 4:

by substitution ( )

Filter Medium Resistance

From figure 4: