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Drying Water and Alcohol through a Porous Medium Experiment


Department of Chemical Engineering and Materials Science University of California Davis





Drying Water and Ethanol through a Porous Medium!







By

Brett Koehn

For

Professors Powell and Tseregounis

















ECH 155: Chemical Engineering Laboratory





Group #1

Ethan Jensen, Chris Gee, and Zheyu Li



Experiment Performed: January 29, 2016



Report Submitted: February 9, 2016





TABLE OF CONTENTS:

Abstract……………………………………………………………………………………………3

Introduction………………………………………………………………………………………..3

Theory……………………………………………………………………………………………..5

Experimental Methods…………………………………………………………………….………7

            Figure 1……………………………………………………………………………………8

Results…………………………………………………………………………………………......9

            Figure 2…………………………………………………………………………………..11

            Figure3………………………………………………………………………………...…11

Discussion……………………………………………………………………………………..…12

Conclusion…………………………………………………………………………………….…14

Nomenclature Table……………………………………………………………………………...14

References………………………………………………………………………………………..15

Appendix A………………………………………………………………………………………16

            Figure 4…………………………………………………………………………………..16

            Figure 5…………………………………………………………………………………..17

            Figure 6…………………………………………………………………………………..18

            Figure 7…………………………………………………………………………………..19

            Figure 8…………………………………………………………………………………..20

            Figure 9…………………………………………………………………………………..21

            Figure 10…………………………………………………………………………………22

            Figure 11………………………………………………………………………………....23

            Figure 12………………………………………………………………………………....24

            Figure 13………………………………………………………………………………....25

            Figure 14………………………………………………………………………………....26

            Figure 15………………………………………………………………………………....27

            Figure 16………………………………………………………………………………....28

            Table 1……………………………………………………………………………….......28

            Table 2……………………………………………………………………………….......29

            Table 3……………………………………………………………………………….......29

            Table 4……………………………………………………………………………….......37

            Table 5……………………………………………………………………………….......52

            Table 6……………………………………………………………………………….......52

            Table 7……………………………………………………………………………….......53

            Table 8……………………………………………………………………………….......55

            Table 9……………………………………………………………………………….......56

            Table 10……………………………………………………………………………….....57

            Table 11……………………………………………………………………………….....58

            Table 12……………………………………………………………………………….....59

            Table 13……………………………………………………………………………….....60

            Table 14……………………………………………………………………………….....61

            Table 15……………………………………………………………………………….....62

            Table 16……………………………………………………………………………….....63

            Table 17……………………………………………………………………………….....66

            Table 19……………………………………………………………………………….....67

            Table 20……………………………………………………………………………….....68

            Table 21……………………………………………………………………………….....69

            Table 22……………………………………………………………………………….....70

            Table 23……………………………………………………………………………….....71

            Table 24……………………………………………………………………………….....72

            Table 25……………………………………………………………………………….....73

            Table 26……………………………………………………………………………….....75

            Table 27……………………………………………………………………………….....76

            Table 28……………………………………………………………………………….....78

Appendix B………………………………………………………………………………............80

            Figure 17………………………………………………………………………………....80

            Figure 18………………………………………………………………………………....81

Appendix C………………………………………………………………………………............82

            Figure 19………………………………………………………………………………....82

Abstract:

            This experiment analyzed how the drying of a liquid is affected by a porous media. Drying in a porous media has four periods which can be analyzed: The start-up, constant rate, first falling rate, and second falling rate periods. In order to analyze these periods, we filled up trays of ethanol and water, and then dried them and measured the loss in mass versus time. Next we plotted the loss in mass versus time to find a drying rate.

We then used the mass versus time plot along with an average saturation versus drying rate plot to find the constant rate periods. We found constant rate periods for every trial. The drying rate in the constant rate period was used to find the heat transfer coefficients. The h values were 26.3±3.4, 34.4±4.5, 23.2±3.0, 48.5±6.3, 38.9±5.1, 20.5±2.7, and 8.1±1.1 watts per meters squared per degree Kelvin, and the htheory values were 20.4±.61, 20.9±.62, 19.8±.59, 20.9±.63, 20.8±.62, 19.7±.59, 18.9±.57 watts per meters squared per degree Kelvin.

We also used a plot of loss in mass versus the square root of time to find the second falling rate. The Keff and Deff values from the second falling rate period were .018±8.2E5 and .0436±.009 watts per meters per degree Kelvin and .00014±2.6E6 and .000013±3.9E6 centimeters squared per second respectively. We found that very small beads must be used to examine the second falling rate.

Introduction:

The process of drying involves the dynamics of heat and mass transfer. These two dynamics happen simultaneously during drying. Also, the phases of liquid and gas are always involved. For special cases, the solid phase can also be involved. For example, consider a bowl of vegetable soup being heated in a microwave. The rate at which liquid evaporates from the bowl will be dependent on the solid vegetables, the soup broth, and the vapor particles above the soup. Drying dynamics can be studied by analyzing the corresponding phases involved.

            Drying undergoes four different periods which are, in chronological order, the start-up, constant rate, first falling rate and second falling rate periods. These periods may be seen in the results section where average saturation is plotted against drying rate. The start-up period is when the gas-liquid interface and uniform dryer temperatures are reaching equilibrium. The constant rate period is when the liquid is still above the porous medium of beads, and therefore drying is controlled by external heat and mass transfer. The first period falling rate occurs when the partial of pressure of the liquid is not equal to the vapor pressure at the gas-liquid interface. This period happens quickly. The second falling rate period is when the liquid level is so low that the dried vapor must travel through the dry porous medium.

            Drying is an important aspect of many of industrial processes. In the pharmaceutical industry several different types of dryers are used to remove moistures or impurities from pure powders.

The food and dairy industries are dependent on freeze drying, which is a process that removes or dries the ice of a product that is frozen rapidly.

Understanding the dynamics of drying allows industries to maximize the efficiency of their drying processes. According to Carranza, drying can be maximized by using dry air to influence the concentration gradient across the gas-liquid interface. Drying will be the quickest if the gas at the liquid-gas interface is constantly being renewed.


Theory:

             Drying through a porous medium is dependent largely on the two parameters porosity and saturation. Porosity is


where ε is porosity, Vγ is the volume of the gas in milliliters, Vβ is the volume of the liquid in milliliters, and VT is total volume of the tray in milliliters. Saturation is

where S is the average saturation.

The complex dynamics of drying behave specifically during the four periods. The start-up periods, and first falling rate periods are too complex to analyze quantitatively. Therefore, we only analyzed them qualitatively. The start-up period is assumed to quasi-steady state. Also, the temperature of the wet porous medium, Ta is assumed to be less than the drier temperature, . Furthermore, we assumed that the gas-liquid interface or simply interfacial temperature, Ti, is equal to the wet-bulb temperature, which is less than Ta.

We assumed that the constant rate period obeys the equation

because the fluid evaporates from the wet porous media since the drier is at a higher temperature than the wet porous media. H is the heat transfer coefficient in watts per meters squared per degree Kelvin Δhvap is the liquid heat of vaporization in joules per mole, A is the area of the gas-liquid interface in meters squared, and dm/dt is the mass drying rate of liquid in grams per second. The theoretical heat transfer coefficient can be found through boundary layer analysis,

where kair is the thermal conductivity of air in watts per meter Kelvin, L is the height of the tray in meters,  is the width of the insulation in meters, Npr is the Prandtl number, and NRe is the Reynolds number which is defined as

where u is the velocity of flowing air in meters per second, DH is the hydraulic diameter in meters, and ν is the kinematic viscosity of air in meters squared per second.

            The Nusselt number is

where NNu  is the nusselt number, havg is the heat transfer coefficient average over the gas-liquid interface, L is the same as DH.

            The second falling rate has heat transfer defined by

where Z is the height of glass beads in the tray in meters, z(t) is the height of the liquid level in meters, and Keff is the effective thermal conductivity in watts per meter per degree Kelvin.

            We also know that diffusive transport dominates diffusive transport because of the quasi-steady state assumption. Therefore,

where Naz is the average molar flux of vapor in moles per meters squared per seconds, c is the liquid concentration in moles per meters cubed, Xea is the mole fraction of evaporated liquid at gas-liquid interface, Xa is the mole fraction of liquid in the air above the tray, Deff is the effective diffusivity, and MWA is the molecular weight of the liquid.

            The dry and wet bulb relationship is described by Bird’s Transport Phenomena as

where Nsc is the Schmidt number Cpf is the heat capacity of air, Pavap is the vapor pressure of liquid, P is the pressure inside the dryer, and Twb is the temperature of the wet bulb.

            The theoretical calculation of the diffusivity is

where Dtheory is diffusivity of water or ethanol in the porous medium in centimeters squared per seconds, DAB is the standard diffusivity of water or ethanol.

Experimental Methods:

            We began this experiment by coming in on Thursday January 28, 2016 to prepare a dish containing glass beads and water. We measured the mass and volume of the tray, the mass of beads, and mass of liquid. We converted the masses of liquids and beads to volumes. We then calculated the porosity. This dish had a large diameter and small height. Furthermore, this dish was suspended in the dryer. This dish was dried overnight, and a remote computer recorded the data. We set dryer to an air flow of 3 and let this dish dry overnight.

Figure 1: The drying duct we used for this experiment. The knobs on the side adjust the airflow and temperature (the temperature knob was broken). The glass window is where the water and ethanol sample were inserted and removed.

            The following day, we again calculated the porosity of trays filled with glass beads and liquids by the same method described in the paragraph above. However, for liquid we used both water and ethanol. We ran two trials for water, and four trials for ethanol. For the water trials we used 4 millimeter and 500 micron beads, and these trials will be referred to as trials 1 and 2 respectively. For the ethanol trials we used 4 millimeter, 500 micron, 1 millimeter, and 6 millimeters beads, and these trials will be referred to as trials 3, 4, 5, and 6 respectively. We wanted to choose a vast array of bead sizes so we would get varying diffusivities and heat transfer coefficients. The overnight water trial will be referred to as trial 7. We measured the mass every 10 minutes and 5 minutes for water and ethanol trials respectively. We removed the trays and weighed them on a balance, then another group member would record the data in excel. We also measured the wet and dry bulb temperatures every hour.

            We then plotted the mass versus time and the change in mass over the change in time versus saturation. We then searched the mass versus time plots (figure 2, 4, 6, 9, 11, 13, and 15) to find a linear fit. We also searched the change in mass over the change in time versus average saturation plots (figure 3, 5, 7, 10, 12, 14, and 16) to find a flat period. Using this information we found in these two plots together, we estimated where the constant rate period was. We then fit this period linearly on the mass versus time plot to obtain a dm/dt value for the constant rate period. We then used this fit to find in accordance with equation 3 to find the experimental heat transfer coefficient h, which is shown in appendix B. We also found htheory by performing a boundary layer analysis and solving equation 4, which is also shown in appendix B. In equation 4 the Reynolds number was calculated inside the duct, and we looked up the Prandtl number.

            We then plotted the mass versus the square root time. We then examined this plot and the average saturation plot to estimate the second falling rate. We then linearly fitted the second falling rate period to obtain another dm/dt value. We then were able calculate Keff from equation 7, which is shown in appendix B. We were also to calculate Deff from equation 9, and Dtheory form equation 10.

Results:

            The constant rate period was generally similar for all of our trials. For trial 1 (water with 4 millimeter beads), the drying rate was squirrely, but it oscillated around a rate of 8.78E-4 grams per second. For trial 2 (water with 500 micron beads), the drying rate was also initially squirrely, but it eventually stabilized to a rate of .001 grams per second. Trial 3 (ethanol with 4 millimeter beads) had a constant rate period that lasted nearly the entirety of the trial. This constant rate period also slowly decreased through the length of the trial. Trial 4 (ethanol with 500 micron beads), had a very quick constant rate period with squirrelly data. However, the drying rate did oscillate around 0.0038 grams per second. Trial 5 (ethanol with 1 millimeter beads) and Trial 6 (ethanol with 6 millimeter beads) both had a relatively long and stable constant periods. Trial 7 (overnight water with 3 millimeter beads) initially had a stable constant drying rate, but it eventually had an oscillating rate.

            The second falling rate varied greatly for each of our trials. The second falling rate was not clear for trial 1. We did not finish this trial, and a second falling rate did seem to be forming as we approached the end of the trial. However, we did not believe this drop off in drying rate was conclusive enough, as the drying rate could have stabilized, and the water sample could have still been in the constant rate period. The second falling rate was visible for trial 2. This trial showed a linear fit to the tail end of the mass versus square root of time plot. Furthermore, the drying rate versus average saturation plot showed a quick and steady drop off at the end of the trial. The third trial slowly decreased during the constant rate period, and displayed a miniature second falling rate. However this was not enough data to analyze. The fourth trial had a second falling rate which first rose and then fell. The fifth trial had a steadily decreasing second falling rate. The sixth and seventh trials were not fully completed, and therefore no second falling rate was observed.

            The h values were 26.3±3.4, 34.4±4.5, 23.2±3.0, 48.5±6.3, 38.9±5.1, 20.5±2.7, and 8.1±1.1 watts per meters squared per degree Kelvin for trials 1 through 7 respectively. The htheory values were 20.4±.61, 20.9±.62, 19.8±.59, 20.9±.63, 20.8±.62, 19.7±.59, 18.9±.57 watts per meters squared per degree Kelvin for trials 1 through 7 respectively.
            The Keff values were .018±8.2E5 and .0436±.009 watts per meters per degree Kelvin for trials 2 and 5 respectively. The Deff values were .00014±2.6E6 and .000013±3.9E6 centimeters squared per second for trials 2 and 5 respectively. The Dtheory values were 1.5E-5±9E7 and 9.2E-6±5.5E7 centimeters squared per second for trials 2 and 5 respectively.


Figure 2: A plot displaying the loss of mass versus time for ethanol in trial 5. The linear fit of trial 5 for the constant rate period is shown in red. The fit is close to linear because we used a large amount of ethanol.

Figure 3: The constant rate curve for trial 5. The period is close to constant because we used a large amount of ethanol.

Discussion:

            The plots of mass versus time do no display perfectly linear fits because of error. First off, there was error when measuring the loss of liquid mass, because the scales could only measure to a tenth of a gram. Secondly, there was error in the time because the stop watch only measured to a second. Also, the time measurements were actually estimates because there was pause between the recording of the measurements of mass and time. In addition, the constant rate period was estimated by myself, which is a source of human error. Furthermore, the water plots of mass versus time (figures 4 and 6) show more linear fits when compared to the ethanol plots (figures 2,9,11 and 13), because the ethanol trays were removed from the dryer more often. Therefore, the ethanol samples were cooling for twice as long outside of dryer when compared to the water samples.

            For figures 3, 5, 7, 10, 12, and 14 no perfect constant rate periods were displayed because of the constraint of having to remove the trays from the dryer. However, the overnight water tray did display a semi-constant period when compared to the other trials (figure 16). This constant rate period was interrupted, because when we began to take measurements of other tray the next morning, we bumped the tray a large number of times. This skewed the drying rate of the overnight trial and ruined its consistency.

            The Reynolds number had error in the uinf because the air flow meter only measured to one hundredth of meters per second, so the percent error was 1 percent. The L measurement because the tape ruler, because it only measured to a millimeter, so the percent error in length was negligible.

The h values have larger values than the theoretical because we were constantly weighing the tray samples. This caused an influx in disruption, which gave us h values that were larger than theory. Furthermore, the h values had error in the temperatures (negligible), area which came from ruler measurements (2 percent error), and change in mass over time measurements (10 percent error). The htheory had an error of 1 percent from the diameter measurement, 1 percent from the insulation measurement, and 1 percent from the Reynolds number.

            Trials 1 and 3 did not display second falling rates, instead they display slowly decreasing constant rate periods. This is because the gaps between the beads were too large, and therefore there was too much space to inhibit a mass transfer to create a second falling rate. Trials 2 and 5 had small enough beads to inhibit mass transfer, and display a second falling rate.

            The Deff  and Keff values were calculated from an array of values that occurred over the span of the second falling rate. This was then averaged and the standard deviation was taken to be the error. The discrepancy between Deff and Dtheory comes from several variables containing uncertainties in equations 8 and 9. The concentration of gas, height of liquid, porosity, dm/dt, partial pressures, area, Schmidt number, Prandtl number, and temperatures all contain uncertainties. Furthermore, the Deff values were much lower because the beads were not packed down, and the gas was constantly being disrupted when the trays were weighed. The discrepancies between Keff and theory come from many of the same uncertainties such as dm/dt, area, temperature, and height of liquid level.

            The error in Dtheory came from assuming the error in the porosity was six percent, because porosity is defined by two volume measurements, which is six length measurements. This is shown in appendix C

Conclusion:

The values of h and Deff were large when compared to theory, because we were constantly disrupting the samples by measuring the masses. This would not be a problem if the dryer could measure the masses of multiple samples at the same time.

We were able to obtain constant rate periods for all of the trials because the constant rate period only depends on external forces of heating. However, we were not able to obtain second falling rates for all of the trials because we used beads which were too large. If we want more accurate data of the second falling rate we need to invest in a new dryer which can weigh multiple trays over time. We also need to even more trials with even smaller beads.

In the future, we shall invest in smaller beads up to 1 micron in diameter. This will allow us to analyze the second falling rate more accurately. Furthermore, with beads in 1 micron in size, we will also be able to analyze and examine the first falling rate.

Nomenclature Table:



References:


1.      Tseregounis, S., Powell, R., 2016, Drying Porous Media, ECH 155, University of California, Davis.


2.      Bird, R., Stewart, W., Lightfoot, E., 1960, Transport Phenomena, John Wiley & Sons Inc. New York.

3.      Whitaker, S., 1981, Fundamental Principles of Heat Transfer, R.E. Krieger Publishing Company, Malabar, Florida

4.      Pharmaceutical Dryers, Pharmacetuctical Machinery, Retrieved February 2, 2016 from http://www.pharmaceuticalmachinery.in/pharmaceutical_dryer.htm

5.      Freeze Dry Applications, Cuddon Freeze Dry, “ISO 9001 Bureau Veritas Certification”, Retrieved February 3, 2016 from http://www.cuddonfreezedry.com/applications/

6.      Carranza, J., Heat and Mass Transfer in Drying, Retrieved February 1, 2016 from http://ww.chemicalonline.com/doc/drying-technologies-in-the-chemical-industry0002#liquid

Appendix A: Raw Data


Figure 4: A plot displaying the loss of mass versus time for water in trial 1. The linear fit of trial 1 for the constant rate period is shown in red. The fit is close to linear because we used a large amount of water.

Figure 5: The constant rate curve for trial 1. The period is close to constant because we used a large amount of water.

Figure 6: A plot displaying the loss of mass versus time for water in trial 2. The linear fit of trial 2 for the constant rate period is shown in red. The fit is decently close to linear because we used a decent amount of water.

Figure 7: The constant rate curve for trial 2. The period is close to constant because we used a large amount of water.

Figure 8: A plot of the loss of mass versus square root of time during the second falling rate for trial 2. The second falling rate is the linear fit in red.

Figure 9: A plot displaying the loss of mass versus time for ethanol in trial 3. The linear fit of trial 3 for the constant rate period is shown in red.

Figure 10: The constant rate curve for trial 3.

Figure 11: A plot displaying the loss of mass versus time for ethanol in trial 4. The linear fit of trial 4 for the constant rate period is shown in red.

Figure 12: The constant rate curve for trial 4. The period is close to constant because we used a large amount of ethanol.

Figure 13: A plot displaying the loss of mass versus time for ethanol in trial 6. The linear fit of trial 6 for the constant rate period is shown in red. The fit is close to linear because we used a large amount of ethanol.

Figure 14: The constant rate curve for trial 6. The period is close to constant because we used a large amount of ethanol.

Figure 15: A plot displaying the loss of mass versus time for water in trial 7. The linear fit of trial 7 for the constant rate period is shown in red. The fit is close to linear because we used a large amount of water.

Figure 16: The constant rate curve for trial 7. The period is close to constant because we used a large amount of water. This was interrupted when we started bumping the tray.

Table 1: Overall Data

Side Length (m)
U(inf) [m/s]
Kine. visco at 70 deg F [m2/s]
NRe
0.277
0.9
1.52E-05
16362.46
Temperature
Time (min)
Dry Air (C)
Wet Bulb (C)
0
49
36
61
48
37
123
48.5
37
176
49
37.5
283
50
39
340
49.5
38
367
51
40
406
50
40

Table 2: Trial 7 Data A

Tray diameter [cm]
Tray height [cm]
Water/bead height [cm]
11.246
7.845
1.31
Mass of Tray
Mass of Tray+Beads
Total Mass
(g)
(g)
(g)
163.3
344.1
400.1



Table 3: Trial 7 Data B

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