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Institut für Verfahrenstechnik

Prof. S.E. Pratsinis

pratsinis@ptl.mavt.ethz.ch
www.ptl.ethz.ch

Practica in Process Engineering II

Praktikum “Mechanical Engineering”

Spring semester 2016

Filtration

Supervisor: Georgios Sotiriou
ML F18
georgios.sotiriou@pharma.ethz.ch
Tel.: 044 632 68 52

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............................................................... 9 3............. 2 2 INTRODUCTION ...............................................................................mavt.....................2 Filter placing...................................ethz..........................................ch Practica in Process Engineering II 1 Table of Contents 1 TABLE OF CONTENTS ....... 8 3...................................................................1................................................. 2 .................................. 9 4 REPORT.................................. Pratsinis pratsinis@ptl.4 Measure the pressure-drop under constant flow-rate ............................. Alternatively...................... For theoretical background in English please refer to Ullmann’s Encyclopedia of Industrial Chemistry........... available online on www....................................ch www....................................... 8 3......................................................................................... Institut für Verfahrenstechnik Prof.............................. 10 4.................. you may ask your assistant for a hardcopy............................... 14 6 CONSTANTS AND GEOMETRICAL DATA .......................................................... 13 5 LIST OF SYMBOLS .1....... 9 3................1 Constant pressure-drop measurements .... 17 7 BIBLIOGRAPHY ..............................................2 Constant flow-rate measurements ..................... 3 3 EXPERIMENTAL .......................................ethbib.................................. 17 Please note: This is a very brief summary of the filtration description in German.. 10 4..............................2 Final discussions ................................... 10 4........................................................................ 8 3.. 11 4........................ethz.....................................................................ethz.....................................................5 Shutting down and cleaning .......1 Specific tasks (in results and discussion) ......................ptl.............1 Suspension preparation ................ch.........................E....................................................................... S..................3 Measure suspension flow rate under constant pressure ...

E.g. either for the removal of valuable product or for cleaning of a product liquid (e.ch Practica in Process Engineering II 2 Introduction In many industrial processes dispersions of particles in a fluid (liquid or gas) need to be separated from their fluid.ethz. One of the basic procedures for this is filtration. {hk / k * η} = (βM + αc * hk) (2) Combining equation (1) and (2) results in 3 . water purification). Here. S. This law can be used to describe the build-up of a filter cake. Two different operation modes will be used: a) constant pressure drop and b) constant suspension volume flow rate. Information related to the structure of the resulting filter-cake can be extracted from this data. The suspension flow rate will be measured during constant pressure filtration whereas pressure drop across the filter is measured during constant suspension flow experiment. Institut für Verfahrenstechnik Prof.ethz. In the following you will find the equations based on the classic differential equations for cake-filtration: Darcy’s law describes the flow of a liquid through a porous medium: Vf ∗ k ⋅ Δp Δp = = (1) AF hk ⎧ h ⎫ η⋅⎨ k ⎬ ⎩ k ⋅ η⎭ Here the term η * {hk / k * η } describes the total resistance against flow through the filter. The resistance term η * {hk / k * η } is now separated into a filter medium resistance βM and a filter cake resistance αc * hk.ch www. αc is the height specific cake resistance and hk is the (time-dependent!) cake height. In this filtration practicum we will investigate the separation of CaCO3 particles from an aqueous suspension (solid-liquid system) by filter pressing.ptl.mavt. Pratsinis pratsinis@ptl.

ch www. the filtrate volume flow rate decreases over time 4 . Pratsinis pratsinis@ptl. Institut für Verfahrenstechnik Prof. c) The resistance of the filter medium βM is constant for the whole filtration process. In this practicum two approaches will be used to solve equation (5): a) ∆p = ¢ i.ethz. The cake height hk is eliminated by a mass balance over the solid material: A F ⋅ h k ⋅ (1 − ε) ⋅ρsolid = Vf ⋅ c (4) Substituting hk from equation (4) into equation (3): 1 dVf Δp Δp ⋅ = = (5) A F dt ⎛ αC c ⋅ Vf ⎞ ⎛ c ⋅ Vf ⎞ η ⋅ ⎜ βM + ⋅ ⎟ η ⋅ ⎜ βM + α ⋅ ⎟ ⎝ ρsol ⋅ (1 − ε) AF ⎠ ⎝ AF ⎠ In equation (5) the term αc / ρsol (1-ε) is replaced by the area specific cake resistance α.mavt.e.ethz. which (for convenience) will be called cake resistance from now on. S.ptl.ch Practica in Process Engineering II Vf ∗ 1 dVf Δp = ⋅ = (3) AF AF dt η⋅(βM + α C ⋅ hk ) For the integration of the differential equation (3) the following assumptions are made: a) The filtrate flow is laminar b) The built filtercake is incompressible.E. d) The filter efficiency is 100% Based on these assumptions equation (3) can be integrated. therefore its porosity is independent of the pressure (αc =const).

S. From the slope the cake resistance α can be calculated. the solution for ∆p = ¢: For integration of (5) with the boundary conditions Vf = 0 at t = 0 : η ⎛ α ⋅c ⎞ ⋅⎜ ⋅Vf +βM ⎟ ⋅ dVf = dt ∫ (6) A F ⋅ Δp ⎝ AF ⎠ V η ⎡ α⋅c 2 ⎤ f ⋅ ⋅V + βM ⋅ Vf ⎥ = t (7) A F ⋅ Δp ⎢⎣ 2⋅ A F f ⎦ 0 t= ( η ⋅ α ⋅c ⋅Vf2 + 2 ⋅ AF ⋅βM ⋅Vf ) (8) 2 2 ⋅A ⋅ Δp F For a graphical analysis of (8) use the following: t η ⋅c ⋅α η ⋅β M = 2 ⋅ Vf + (9) Vf 2 ⋅A F ⋅ Δp A F ⋅ Δp A graphic representation of t / Vf as function of Vf gives a straight line (Figure 4). the filtration pressure increases over time Following a).ethz.ch Practica in Process Engineering II b) Vf* = dVf / dt = ¢ i.ch www.mavt. 5 .E.ethz. Institut für Verfahrenstechnik Prof. while from the intercept the filter medium resistance βM can be found.e.ptl. Pratsinis pratsinis@ptl.

the solution for Vf* = dVf / dt = ¢: With Vf = t .ch Practica in Process Engineering II t Vf α βM Vf Figure 4: t / Vf vs Vf for ∆p = ¢ Following b). 6 .mavt.ch www. Institut für Verfahrenstechnik Prof. Vf* from (5) you get: η ⋅α ⋅c ⋅Vf∗2 βM ⋅ η⋅ Vf∗ Δp(t) = ⋅t + (10) A2F AF This means the pressure increases linearly with time.E. By plotting ∆p as function of t you can determine α as well as βM (Figure 5). S.ethz.ptl.ethz. Pratsinis pratsinis@ptl.

Institut für Verfahrenstechnik Prof.ptl. Pratsinis pratsinis@ptl. for Vf* = ¢ Plotting the specific cake resistance α from different experiments at different constant ∆p in double logarithmic scale as function of ∆p.mavt.ch www. for compressible cakes n increases from 0 to approximately 1.2. S. 7 . you will find a near to linear dependency according to the following formula: α = α o ⋅(Δp / Δpo ) n (11) From this you can calculate the compressibility n: log α / α o n= (12) log Δp / Δpo For incompressible filter cakes n becomes 0.E.ethz. At n = 1 the filtrate volume is after a certain time quasi- independent of the filtration pressure.ch Practica in Process Engineering II Δp α βM t Figure 5: ∆p versus t.ethz.

S. Pratsinis pratsinis@ptl.2 Filter placing Check that the filter (degas) valves E are closed. Institut für Verfahrenstechnik Prof. make sure the outlet valve A is closed and the pressure release valve of the stirrer tank is opened properly. Find the relevant valves and its proper position on the P&ID for the two modes of operation.1 Suspension preparation Weigh 250 g of CaCO3. Press the plates together with 8 .mavt. Place the filter between the plates (smooth surface towards the incoming flow).E. 3.ch Practica in Process Engineering II Figure 7: Piping and Instrumentation diagram (P&ID) of the plate filter setup.ptl. 3.ethz. Make yourself familiar with the setup before operation. 3 Experimental Figure 7 shows the piping and instrumentation diagram of the filter press used for the experiments. Then fill approximately 60 L of water through valve B and add the pre-suspension through valve B as well and fill in water until 70 L are in the tank. Before water is filled in through valve B. add some water and stir to make a rather thick pre- suspension. Start the stirrer C and the recirculation pump D to achieve a homogeneous suspension.ethz.ch www.

For the first experiment choose ∆p = 1 bar. Next.3 Measure suspension flow rate under constant pressure First close the pressure release valve E and the filling valve B on the tank. Drain the rest of the suspension by opening the valve A. Open the path leading through the flow meter (G) and close the path through the bypass line. Disconnect all electrics (stirring.ch Practica in Process Engineering II the clamp. the tank needs to be pressurized to the required pressure level for the corresponding experiment. Change the filter and redo the measurement at ∆p = 3 bar (set valve F to 3 bar). pump.mavt.ethz. After the filter is wetted it might be needed to reinforce the clamp pressure as the filter settles a bit when wet. Set the flow rate on the FIC to 80 l/h. Close degas valves and start the measurement. Shut down the stirring (C) and suspension circulation (D). 3. Clean the working place. After the second experiment you have to drain the remaining suspension in the tank through valve A and prepare a new 70 L batch of suspension. Measure the pressure drop during approximately 10 minutes every 15 s. recording the flow- rate every 15 s. 9 . 3. Institut für Verfahrenstechnik Prof. This can be done by adjusting the pressure control valve (PIC). Change the filter (release overpressure through valve E before opening the press) and redo the measurement at ∆p = 2 bar (set valve F to 2 bar). After all experiments have been carried out you can compare the appearance of the filter cakes like cake thickness and porosity. Turning clockwise will increase the pressure and vice versa (please lift the red plastic ring while adjusting). 3. S.ptl. Switch the pressurized air supply on (main valve on the wall).4 Measure the pressure-drop under constant flow-rate Set the pressure to 3 bar (valve F) and replace the filter. Let some suspension pass through the filter press by opening the final valve to the plate filter (valve J) and simultaneously open the degas valves E until suspension runs out. Air flows into the tank and fills up the volume above the liquid (give it some time to reach equilibrium). Measure the flow under constant pressure for 8-12 minutes. Once the tank is pressurized.5 Shutting down and cleaning Close the valve to the pressurized air (F).ch www. check that the flow through the flow controller (FIC) is bypassed. Pratsinis pratsinis@ptl. flow and pressure-meters).ethz.E.

Conclusions (what are the discoveries of the experiment.1 Constant pressure-drop measurements a) Neglecting the filter resistance βM in equation (8).ch www. Experimental (describe the experimental procedure) 4. 10 . Results (plot the result curves and perform the needed calculations) 5. The report should be approximately 8 pages long and include the following chapters: 1. S.ethz.ethz. Following equation (13) you should get a linear dependency with a slope of 0. Discussions (discuss the results and refer to literature if needed) 6.1 Specific tasks (in results and discussion) 4.ptl. Discuss the results and draw some qualitative conclusions from the plotted results.1.E.5. what does it mean in practice) 4.mavt. Theory (equations which will be used in the result part must be introduced) 3. Institut für Verfahrenstechnik Prof.ch Practica in Process Engineering II 4 Report Each member of the group has to write his/her own individual report. the filtration for constant pressure is then described by η ⋅ c ⋅ α ⋅V f2 t= (13) 2 ⋅ AF2 ⋅ Δp Vf 2 ⋅ t ⋅ Δp = (14) AF c ⋅η ⋅α Plot the filtrate volume Vf [m3] per filter area Af [m2] as a function of time t [s] in double logarithmic scale. Abstract (describe shortly what was done and what were the major findings) 2. Pratsinis pratsinis@ptl.

Discuss the results. 2 and 3 bar by using equation (9). The pressure loss in such channels is: ρ liq 2 h Δp Kanal $=liqξ (Re) 2 ⋅ hk v Kanal ⋅ k (15) #p Kanal = % (Re) " v Kanal " 2 dh 2 dh % pressure drop coefficient (here 64/Re) vKanal Channel mean velocity dh Hydraulic diameter hk Filter cake height Thenumber Reynolds pressure drop for such coefficient channel is: is here 64/Re (laminar flow) v Kanal " d h " $ liq Re = The &Reynolds number for such channel is: And the mean velocity in the channel is determined by the continuity equation: V f* = v Kanal " AF " ' = v0 " AvF $#" ! Kanal ⋅ d h ⋅ ρ liq free Re = empty tube (16) cross sec tion velocity η surface In reality there are no single and continuous channels.ethz. " -2 (m4. Institut für Verfahrenstechnik Prof. # (m-1). the filter measurements c) Plot the pressure drop ∆p [Pa] as a function the time t [s]. Additionally. Find the filter resistance. S.mavt.ptl. Find the cake where Vf* (m specific 3 ) isresistance filter the total filtrate αC [m -2 volume which ]. it can be defined as: 11 . the graph and equation (10) where Vf* [m3/s] is the filtrate volume flow. using βM (m (s). using the graph and equation. However.ch Practica in Process Engineering II b) Plot t/Vf [s/m3] as a function of Vf [m3] and find the specific cake resistance α from the regression.ethz. determine the resistance of the filter medium βM (m-1). in porous filter the channels are curved with changing dimensions depending on the particle properties.ch www. Pratsinis pratsinis@ptl. Themain Thus. the mean velocitycomes inaccuracy in thefrom channel the useisofdetermined the hydraulicby the continuity diameter equation: dh.2 ). and Constant flow-rate resistance of medium.1. c) Plot the pressure drop !p (Pa) as a function the time t (s) . d) Solve the compressibility n using: n ! = ! o "( #p / #po ) and d) Solve the compressibility n [-] using equation (11) or (12). and has passed resistance of through themedium the filter filter at time t -1). for each pressure drop 1.E. log ! / !o n= loge)#p / #pthe Find o porosity ε (ratio of void volume to total cake volume) of the filter cake using the Carman-Kozeny theory. In fact. the Carman-Kozeny theory shown below: The pressure loss in such channels is: Carman (1939) calculated the pressure loss in the bulk and modeled the porous filter cake as numerous continuous parallel channels. Carman (1939) calculated the pressure loss in the e) Find the porosity (ratio of void volume to total cake volume) ($) of the filter cake using bulk and modeled the porous filter cake as numerous continuous parallel channels.

Institut für Verfahrenstechnik Prof.ethz. Pratsinis pratsinis@ptl.mavt.E. Thus.ptl.ch www. the main inaccuracy comes from the use of the hydraulic diameter dh which can be defined as: 4A hk dh = ⋅ (18) U hk here A is the channel cross section area [m2] and U is the wetted channel circumference [m].ethz. In fact. Another definition of the hydraulic diameter is: 4⋅ (ε ⋅A F ⋅ h k ) dh = (19) F where F is the total wetted surface: (20) F = S ⋅ (1 {− ε ) ⋅ 1AF2⋅3hk solid volume total cake − fraction volume S= Specific particle volume surface ε = porosity With (4) and inserting the above in (15) you get: The pressure drop is: 12 . S.ch Practica in Process Engineering II V f* = v Kanal ⋅ AF ⋅ ε = v0 ⋅ AF (17) $# " ! freie Lehrrohr Querschnittsfläche Geschwindigkeit In reality there are no single and continuous channels. in porous filter the channels are curved with changing dimensions depending on the particle properties.

ptl. Pratsinis pratsinis@ptl.mavt. polydisperse (“several” sizes) particles with broader size distribution would be used? • How would the plot of t/Vf as a function of Vf change if the filter media resistance (β) would change over time? • Compare the results of four different filter cake (α) and media (β) resistances. Which porosities do you get and what conclusion can be drawn? 4.ch www.ch Practica in Process Engineering II ⎛ c ⋅ Vf ⎞ Δp = η ⋅ ⎜ αC− K ⋅ ⎟ ⋅v (21) ⎝ AF ⎠ 0 With given equations derive the specific cake resistance.2 Final discussions Discuss your results and compare your experimental data to the theory: • Are the assumptions made for the integration of the filter differential equation reasonable comparing the observed results here? • How would the porosity change if instead of ideal monodisperse (“single” sized) particles. How does the magnitude of the cake (α) and filter media (β) resistances affect the values of the compressibility (n) and porosity (ε)? 13 . their order of magnitude and ratio to each other. αC-K [m/kg].ethz. Institut für Verfahrenstechnik Prof.E.ethz. Using the solved cake resistances from the pressure constant experiments α [m/kg] one can solve for the porosities for each ∆p=const experiment. S.

mass of solid per total volume [kg/m3] dh hydraulic diameter [m] F wetted surface [m2] hk cake height (channel lenght) [m] k Durchlässigkeitskoeffizient after Darcy [m3 ∙ s/kg] n compressibility [-] ∆p pressure drop over filter and cake [N/m2] S specific surface area (surface per volume of the particles) [m-1] t filtration time [s] U wetted curcumferance [m] vKanal mean velocity in the channel (pore) [m/s] 14 . Pratsinis pratsinis@ptl. S.ethz.ethz.ptl.E.mavt. Institut für Verfahrenstechnik Prof.ch Practica in Process Engineering II 5 List of symbols A channel cross section [m2] AF area of the filter [m2] c solids concentration.ch www.

ch www. S.mavt.ethz. Pratsinis pratsinis@ptl.E. Institut für Verfahrenstechnik Prof.ptl.ch Practica in Process Engineering II v0 void tube velocity [m/s] Vf suspension volume [m3] Vf* suspension volume flow [m3/s] aC cake height specific cake resistance [m-2] 15 .ethz.

Institut für Verfahrenstechnik Prof. viscosity [kg/(ms)] ρliq fluid density [kg/m3] ρsol solid density [kg/m3] x pressure drop constant [-] 16 .ptl.mavt.ethz.ethz. Pratsinis pratsinis@ptl. S.ch Practica in Process Engineering II α area based cake resistance [m/kg] αC-K flächenmassenspezifischer Kuchenwiderstand nach Carman-Kozeny [m/kg] βM resistance of the filter media [m-1] ε porosity [-] η dynam.ch www.E.

Pratsinis pratsinis@ptl. 168-188 [3] Müller.ptl.8 .E. P.: "Mechanische Trennverfahren". 1939.ethz. (IVUK-Bibliothek CIT 219/II) 17 . S. 10-6 kg/(ms) AF = 0. Herausgeber Victor Dalmont.mavt.ch Practica in Process Engineering II 6 Constants and Geometrical Data ρsol = rCaCO3 = 2710 kg/m3 ρliq (Wasser bei 14 °C) = 1000 kg/m3 S = 9.18 * 105 m2/m3 η = 1197. Institut für Verfahrenstechnik Prof.: "Les Fontaines Publique de la Ville de Dijon". Transactions-Institution of Chemical Engineers. E. Sauerländer. 1856 [2] Carman. Paris.: "Fundamental Principles of Industrial Filtration". C.ethz.ch www.0324 m2 7 Bibliography [1] Darcy. 1983. H. Band 2.