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Filtration and Centrifugation Training Exercise 2 dc5
Filtration and Centrifugation Training Exercise 2 dc5
Background
In this exercise, you will explore a dynamic model for cake filtration in the Cake Filtration Toolbox. The
Cake Filtration Toolbox allows you to evaluate the cake filtration properties based on representative
filtration data and predict the filtration performance under alternative conditions and equipment. The
toolbox contains two different methods to evaluate the cake filtration properties. The first method uses
a part of the toolbox called the Buchner Funnel calculator to calculate a crude estimate of the specific
cake resistance based on single data point – making good use of the limited data that are commonly
available in process development. The second method uses the Pocket Filter model to fit the specific
cake resistance and compressibility index from experiments with multiple filtrate data points. This
method gives a more accurate measure of the cake filtration properties, which you can reliably apply to
predict the filtration performance over larger pressure ranges. You can use both tools to generate
reports of your analysis to compare or track the filtration performance throughout the development
lifecycle. This exercise introduces the Pocket Filter model, and gives you practice applying the model for
fitting cake filtration properties, making predictions and comparing the results with the Buchner Funnel
calculator.
2. Click the Pocket Filter Data worksheet to review the layout and data requirements for the
Pocket Filter model. Similar to the Buchner funnel calculator, this interface has columns that
resemble a filter. The white cells are for user inputs. You use the Pocket Filter Data sheet to
prepare the experimental data prior to fitting the cake properties and filter medium resistance.
After fitting, you use the Results and Scale-up worksheet to review the results and define a
scale-up scenario for prediction based on the regressed cake and medium properties.
Note: This toolbox contains a filter database on the FilterDB worksheet, which stores the
dimensions and information for common filters. The default database includes the filters needed
for this exercise. Users can add or modify filters on this worksheet.
Note: In these experiments, you will select slurry/cake building for the Filtration Type since all
the experiments start with a slurry. If you wanted to model a wash filtration (i.e., filtering a neat
solvent through a constant cake mass), you would select ‘wash/cake established’. This selection
alters where the solid mass is initialized in the model, i.e., in the slurry phase or cake phase.
Note: You can change the units for any of the inputs. Ensure the values and units match the
screenshot below.
Note: By default, the sheet copies some inputs – such as the liquid density, liquid viscosity, and
solid density – from the first experiment to the other experiments and to the prediction. This
streamlines your work. You can alter the values and units as required.
Note: This sheet can accommodate three experiments at different pressures – a common dataset
for this work. However, you can enter data for up to five experiments. Clicking the ‘Add Expt’
button will unhide columns for additional experiments. Clicking the ‘Hide’ button will re-hide the
experiment.
Tip: If you cannot measure the final cake height, enter an estimate for the cake height such that
the cake voidage (row 43) is a reasonable value. Typically, the cake voidage is 30-70%.
4. Review the Pre-fitting Results for these experiments in the table with the green background. In
particular, look at the voidage (row 43), which is typically around 30-70%, and the height to
diameter ratio of the cake (row 42), which should be above 0.1 (if the cake is too thin, then you
will only measure the media resistance). The cake density is also calculated (dry cake mass
divided by the filtered cake volume), which can be useful for predicting the cake volume when
the filtration is scaled.
Scroll to the right to view a plot of the filtration profiles in the Preview of Data area.
Use this plot to ensure that your data look reasonable. This plot converts the filtrate mass to kg
and the time to seconds. Consider some of the following questions:
Are the final filtrate amounts and filtration times as expected?
Did the final raw filtrate mass exceed the predicted filtrate mass for each experiment
(row 36)? (This model will not predict the deliquoring regime, when the liquid level falls
below the cake. Therefore, for the best regression, you should remove any data beyond
the predicted filtrate mass, which would be when the cake is deliquoring.)
Are the series in the expected order? (Higher pressures generally means faster
filtrations except for highly compressible cakes.)
Is there curvature in the profiles? (A linear filtrate vs time profile could indicate only
media resistance was significant, or that the solids settled quickly, or that the
experiment was conducted by allowing significant cake to form before the filtrate flow
was started.)
Change the Plot type to Time/Filtrate vs Filtrate (integral plot). Each data set should give a
linear plot (allowing for some scatter). The lines should move in order with the applied pressure
difference.
Scrolling to the right of the main plot in the Preview of Data, you will find guidance diagrams.
Curve A shows the expected results for the integral and differential plots (straight lines). Curves
B through F show possible deviations with some explanations.
Tip: Consider resolving any ‘Observations’ on this sheet prior to fitting. The sheet can show a
number of observations based on your data. For instance, it may be preferred to reduce the
number of data points or remove certain portions of the data. In Dynochem 6, you can use the
Data Reduction tool in the Dynochem Ribbon to help reduce your data.
6. From the Dynochem Ribbon in Excel click on the Open in Fitting icon ( ). If the model
contains no errors it will ‘parse’ successfully, then click the OK button and the model will open in
the Fitting module.
7. Select the data for all three scenarios by checking the Select All box at the top left as shown
below.
Note: The LN_media_res and LN_spec_cake_res_0 are the natural logs of the medium
resistance and specific cake resistance at 1 bar, respectively. Fitting to the natural log of
these parameters is preferred because these parameters may vary over orders of magnitude.
Tip: The ‘initial guess’ may be edited prior to fitting. A good starting point for the initial guess is
25 for the LN_media_res and LN_spec_cake_res_0 and 0.5 for the compress_index.
Press play ( ) and monitor fitting progress in the Fitting Results panel. You can move
between plots for each scenario by using the << and >> buttons at the bottom right to watch the
fitting progress.
When you see the Fitting Complete message, click OK. Review the parameter values and
confidence intervals displayed in the top left of the Fitting results panel and ensure that the
confidence intervals are of the order of tens of percent or less. These statistics indicate that
fitting has given good estimates of the parameters from the data.
Check that your fitted parameter values are as follows:
LN_media_resistance LN_spec_cake_resistance_0 compress_index
22.3 24.5 0.76
Tip: Click the icon while in Fitting to see more detailed statistics describing the fit. If you
would like to export a detailed fitting report into your Excel model, click the button in the
Fitting toolbar. This will add a new worksheet to your file.
10. Return to Excel and click on the Results and Scale-up worksheet. The table with the green
background shows the results for the three experiments. The LN_media_res,
LN_spec_cake_res_0, and compressibility index should match the values you saw in Fitting.
11. Click the Add to Report button at the top of the column for each experiment to save the details
and results of each experiment to the Report worksheet. Click on the Report worksheet to view
the saved information and results.
Note: For pocket filter experiment with filtrate and pressure profile data, this information is
saved in the report. Scroll down to the ‘Filtrate & Pressure Profiles Inputs’ section (row 63). The
data will be saved in the report after converting to standard units and comma separated.
13. Return to the Results and Scale-up worksheet and fill in the information for the Scale-up
Filtration, as shown below. In this case, the prediction is considering a larger scale filtration and
applying a slightly higher pressure difference.
Please be sure you choose the appropriate Location and Name for the filter. You will see the
equipment information retrieved from the FilterDB sheet.
Note: You can change the units for any of the inputs. Ensure the values and units match the
screenshot below.
Note: It is preferred to study the impact of pressure on the specific cake resistance over a range
that spans the pressure difference applied in the prediction. In this prediction, the chosen
pressure difference lies within the pressure range explored in the pocket filter experiments.
Note: The scale-up scenario is a prediction for an identical slurry to the experiments. The relative
amounts (e.g., the liquid-to-solid ratio) in the experiments and scale-up scenario are the same.
Note: Generally, the medium resistance is an insignificant contribution to the overall filtration
resistance. You can see the value of the medium resistance pulled from the filter database. You
can enter a new value here on the Results and Scale-up sheet to overwrite the database value.
For instance, if your scale-up filtration will use a medium like that used in the pocket filter
experiments, the fitted medium resistance may be a more accurate value for the prediction.
14. Review the results in the table with green background, as shown below. The Applied Cake
Properties section shows the properties that will used in the prediction. In the Predicted
Performance section, you can record the filtration time and average flux from the simulation in
the white cells. In the next few steps, we will use Simulator to solve the model equations and
predict the filtration time and average flux. In the Filter Analysis section, results on the slurry
and cake fill are available because the filter database contained information on the filter’s
capacity. In this case, the cake would consume about 50% of the filter’s capacity, and the slurry
would exceed the filter’s capacity, fill at 191% (see Observation #5 in the gray box to the right of
the Scale-up prediction columns). Therefore, a fed batch operation or filtering over several
loads should be considered.
16. When presented with a list of scenarios, uncheck all except the last scenario Plant Scale: 25 psi
scenario, then click OK. When the scenario has opened, click the Play button ( ) below the
plot to simulate this scenario (the plot colors may vary depending on the version of Dynochem
you have installed).
18.0
9.0
0.0
0.0 5.29 10.58 15.869 21.159 26.449
Time (min)
17. Return to Excel and the Results and Scale-up worksheet. Record the predicted filtration time
(26 min) and average flux (780 L/m2h) in the ‘Predicted Performance’ (rows 49-50), as shown
below.
18. Click the Add to Report button for the Scale-up Filtration to save the details and results of this
prediction to the Report worksheet. Click on the Report worksheet to view the saved
information and results.
20. Return to the Results and Scale-up worksheet and review the Check Model Graphs to the right.
Similar to the Pocket Filter Data worksheet, this sheet includes graphs of the Filtrate vs Time,
Time/Filtrate vs Filtrate (integral plot), and Time/Filtrate vs Filtrate (differential plot). Use the
drop list to change the plot type. In these plots, you can compare the raw data (points) with the
prediction from the fitted values that were saved in the model (solid lines). This graph makes it
easy to check how well the model represents your data. For the integral plot, you will see that
the predicted lines pass through the data points very well. For the differential plot, the points
Scrolling down, you will see a log-log plot for the specific cake resistance versus pressure
difference. The pocket filter model assumes the commonly observed power relationship
between the specific cake resistance and pressure, where the compressibility index is the
exponent. Therefore, this plot will form a straight line with a positive slope, where the slope is
the compressibility index. The predicted line from the model gives a good match to the data in
this exercise.
21. Review the Report worksheet to view the saved details and results from Buchner Funnel
Calculator, from the prior exercise, and Pocket Filter model, from this exercise.
Note: The Filtration Time (row 38) for the Scale-up Prediction was approximately 24 min from
the Buchner Funnel Calculator and 26 min from the Pocket Filter model. Despite the limited
data, the Buchner Funnel Calculator provided a fair estimate of the filtration time compared to
the Pocket Filter Model. However, the Pocket Filter Model is expected to be more accurate
because the compressibility index was fitted to experiments at three different pressure
differences. The parameters from the pocket filter model should provide more reliable estimates
for higher pressure filtrations and centrifugations.
This exercise usually ends here. There are several optional parts below. If you are taking this exercise as
part of instructor led training, please check whether the instructor wants you to do these parts.
Part B is about using Dynochem ‘automation’ to generate a large volume of results for a range
of input conditions.
Part C is about how to use the toolbox to predict the cycle time for displacement washes.
Part D is about how to use the toolbox with data collected from an experiment where you vary
the pressure profile. This allows you to determine the medium resistance, cake resistance and
compressibility index from a single experiment. This approach is also called the “dynamic
pressure modulation” (DPM) method.
1. From the Dynochem ribbon in Excel, select Full Factorial ( ) to produce the dialog box shown
below.
3. In the Variables.deltaP row, set up a minimum pressure of 1 psi, maximum of 30 psi, and 10
logarithmic levels. In the Variables.solvent_viscosity set up a minimum pressure of 0.47 cP,
maximum viscosity of 0.77 cP, and 10 linear levels. See screen shot below.
4. Press Run to generate the new scenarios and run them in the background behind Excel.
5. After a short time, a new Full Factorial worksheet will appear in your model, containing
tabulated input (‘Factors’) and output (‘Responses’) values from the 110 new scenarios. The
inputs are from your scenarios tab and the responses are those variables that are plotted in your
model.
6. Click on Response Surface (or Contour Plots in Dynochem 6) and select both the
‘solvent_viscosity’ and ‘deltaP’ as the Factors and cycle_time as the Response.
7. Click Create. A contour plot of these 110 virtual experiments will be generated in your default
browser, as shown below.
1. Click on the Results and Scale-up worksheet and scroll down to the Wash Calculation below the
Scale-up Filtration (row 62).
2. Fill in the inputs for the Wash Calculation section as shown below.
4. Click the Add to Report button for Scale-up Filtration to save the details and results of this
prediction to the Report worksheet. Click on the Report worksheet to view the saved
information and results.
Note: The predictions for the wash calculation is saved in the Scale-up Wash Entries and Scale-
up Wash Predictions sections (row 53-62).
Alternatively, you can simulate profiles for this displacement wash in the Simulator by setting up a new
prediction. To explore this approach, complete the following steps.
5. Return to the Results and Scale-up worksheet and edit the prediction by changing the Scale-up
Name to ‘Plant Scale Wash’, Filtration Type to wash/cake established and changing the liquid
mass to 5 kg, as shown below.
Note: By changing the Filtration Type to wash/cake established, the model will initialize the
solids in the cake rather than in the slurry.
6. From the Dynochem Ribbon in Excel click on the Simulator icon ( ). If the model contains no
errors it will ‘parse’ successfully, then click the OK button and the model will open in the
Simulator module.
7. When presented with a list of scenarios, uncheck all except the last ‘Plant Scale Wash: 25 psi’
scenario, then click OK. When the scenario has opened, click the Play button to simulate (the
plot colors may vary depending on the version of Dynochem you have installed).
6.0
3.0
0.0
0.0 1.861 3.722 5.584 7.445 9.306
Time (min)
8. Return to Excel and the Results and Scale-up worksheet. Record the predicted filtration time
(9.1 min) and average flux (395 L/m2h) in the Predicted Performance (rows 49-50), as shown
below.
9. Click the Add to Report button for Scale-up Filtration to save the details and results of this
prediction to the Report worksheet. Click on the Report worksheet to view the saved
information and results.
2. Click the Add Expt button to unhide the columns for a fourth experiment.
3. Fill in the inputs for the fourth experiment, as shown below. In this case, select Impose Profile
from the drop list for the Pressure Difference, which will enable a column for the pressure
profile in the table with filtrate data. Also, change the Experiment Name to ‘Expt 4 (DPM)’.
4. Scroll down as needed to see the Filtrate Data & Pressure Profile table. Remove any existing
data in the table for this experiment. The raw data file [raw_data_filtration_exercise.xlsx]
provides the measured data for this experiment. Copy the data from the Variable Pressure
Experiment worksheet and paste the data into the white cells for ‘Expt 4 (DPM)’ in the Filtrate
Data & Pressure Profile table.
5. From the Dynochem Ribbon in Excel, click on the Open in Fitting icon ( ). If the model
contains no errors it will ‘parse’ successfully, then click the OK button and the model will open in
the Fitting module.
6. Select the data for only the Expt 4 (DPM): Imposed pressure profile, as shown below.
Tip: The ‘initial guess’ may be edited prior to fitting. A good starting point for the initial guess is
25 for the ‘LN_media_res’ and ‘LN_spec_cake_res_0’ and 0.5 for the ‘compress_index’.
8. Press play ( ) and monitor fitting progress in the Fitting Results panel.
When you see the Fitting Complete message, click OK. Review the parameter values and
confidence intervals displayed in the top left of the Fitting Results panel and ensure that the
confidence intervals are of the order of tens of percent or less. These statistics indicate that the
parameters have been estimated well from the data.
Tip: Click the icon while in Fitting to see more detailed statistics describing the fit. If you
would like to export a detailed fitting report into your Excel model, click the button in the
Fitting toolbar. This will add a new worksheet to your file.
9. Press the Save button ( ). This automatically updates the scenarios sheet of the model in
Excel with the parameter values you have fitted (the scenarios sheet is hidden by default in the
toolbox).
10. Return to Excel and click on the Results and Scale-up worksheet. The ‘LN_media_res’,
‘LN_spec_cake_res_0’, and ‘compressibility index’ for ‘Expt 4 (DPM)’ should match the values
that you fitted in the prior step. As you can see, these results are similar to the values that you
fitted for the three constant pressure experiments, Expt 1, 2, & 3.
Note: The plot in the Check Model Graphs, does not show the model prediction (solid line) for
any experiment with an imposed pressure profile (Observation #4). For experiments with an
imposed pressure profile, you must use the Simulator to produce a graph of the experimental
data versus the model prediction.
11. Click the Add to Report button for the ‘Expt 4 (DPM)’ experiment to save the details and results
of this experiment to the Report worksheet.
12. Review the Report worksheet with the saved details and results from this exercise. In particular,
the ‘Specific Cake Resistance at 1 bar’, ‘Compressibility Index’, and ‘Medium Resistance’ are
similar to the values that you fitted for the three constant pressure experiments, Expt 1, 2, & 3.