Distillation Column Design in Separating Ethanol-Water Mixture

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    University of California,

    Los Angeles

    Winter 2000

    Distillation Column Design In Separating

    Ethanol-Water Mixture

    Marie Dang

    Sandy Lao

    Hang-Tam Nguyen

    ChE 108A Project

    Professor Choi

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    2

    Table of Contents

    Introduction 3

    Procedure 4

    Calculation 5

    Result 9

    Discussion 11

    Conclusion 13

    Contribution 14

    Index 15

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    Introduction

    A conventional azeotropic distillation uses entrainer such as benzene to purify products.

    Thus a distillation process without entrainer will cost more and one would need to adjust

    the process variables to minimize the cost. This project focuses on designing a system

    consisting of two distillation columns to obtain 99.9 wt% ethanol from a feed stream that

    composed of 40 wt% ethanol, 60 wt% water, at a total flow rate of 100kg/hr. The feed

    enters the first column at 25 C and 1 atm. For the basic case design, the first column will

    contain 60 stages, with a feed stage at 58 and the recycle-in stage is 10. The top pressure

    is 0.10 atm and the bottom pressure is 0.12 atm. We use total condenser with a distillate

    rate of 410 kg/hr with a reflux ratio of 25. The pumps output pressure is 1.1 atm. As for

    the second distillation column, the number of stages is 90 and the feed stage is at tray 10.

    The top pressure is 1.0 atm and the bottom pressure is 1.1 atm. Again, we use the total

    condenser with a distillate rate of 370 kg/hr and a reflux ratio of 25.

    With the above parameters in mind, we utilize PRO/II with the NRTL thermodynamic

    model to design and simulate the base case design. By adjusting the following variables,

    we can come up with the best separation process design.

    1. Number of trays of column 12. Number of trays of column 23. Position of the feed tray for column 14. Position of the feed tray for column 25. Reflux ratio of column 1

    6. Reflux ratio of column 27. Position of the recycle-in stage for column 18. Flow rate of the recycle stream

    We then came up with three different designs in which we minimize the material cost.

    The ultimate goal is to obtain a final design, which is economically the best, or at the

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    very least, has significant improvement from the basic design. The first design, which is

    denoted as Optimal 2, uses 15 and 39 trays for the two columns with a saving in cost of

    13.6% in comparison to the base cost. The second design, Hang1, requires 37 and 40

    trays for the two columns and saving us 83% less in comparison to the Base Run cost.

    Our last run, Sandy2, which uses 32 and 26 trays, saves us 28% less to theBase Run case.

    Procedure

    For the Basic run, which involves two distillation columns, ProII is utilized to quickly

    calculate the features of each tray of the distillation column and generate a report for each

    run. First the basic run design is schematically drawn with ProII. The conditions are

    then entered into each column and initial estimates are provided. Note that the initial

    estimates for each stream coming in and out of the distillation reflect the overall

    component mass balance around the each unit. Once the basic run is generated, we can

    adjust the variables to come up with the better designs, which we could evaluate based on

    the economic analysis. By comparing the different cases we would be able to select

    which of the potential candidate designs would be the best. We note that this may not be

    the most optimal design but it is certainly presents improvement from the base design and

    that its set of costs are within reasonable tolerances. Thus by minimizing the number of

    trays of each column, the reflux ratio of the condensers, and the recycle flow rate, we can

    reduce the expense considerably. The choice of a design is based on the total annualized

    costs which would consists of both capital costs and operating costs, and the balanced

    minimum of the two would lead to the optimal design.

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    Calculation

    Sample Calculation for Determination of Column Size (Case Sandy2 Column 1)

    From the generated report for PROII simulation run, we first locate the vapor and liquid

    flow rates for tray #2 and the bottom tray. We picked tray #2 as our top tray because this

    is the actual first tray in the column. We also find the density (Rho) for both vapor and

    liquid at the top and bottom. Summarizing these results provided by PROII:

    L'(kg/hr) V' (kg/hr)

    RhoL(kg/m^3)

    RhoV(kg/m^3)

    Top (Tray #2) 10554 10660 783.806 0.17735

    Bottom 60.09 4187 986.644 0.07937

    Then we determine Flv, which is defined by the following relation:

    5.0

    '

    '

    =

    L

    g

    lvV

    LF

    For the top tray:

    )(014893.0

    806.783

    17735.0

    10660

    10554)(

    5.0

    unitlesstopFlv =

    =

    )(000129.0644.986

    07937.0

    4187

    09.60)(

    5.0

    unitlessbottomFlv =

    =

    Now we pick 24 tray spacing and turn to Figure 4.4 in out textbook Systematic Methods

    of Chemical Process Design and find Csb in ft/s.

    s

    fttopCsb 39.0)( = and s

    ftbottomCsb 4.0)( =

    Updating our table:

    L'(kg/hr) V' (kg/hr)

    RhoL(kg/m^3)

    RhoV(kg/m^3)

    Flv (nounit) Csb (ft/s)

    Top (Tray #2) 10554 10660 783.806 0.17735 0.014893 0.39

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    Bottom 60.09 4187 986.644 0.07937 0.000129 0.4

    We now calculate the flooding velocity Unfgiven by the expression:

    2.0

    5.0

    20

    =

    g

    gL

    nf CsbU

    Where is the surface tension in dynes/cm. For the first column, we use the surface

    tension of ethanol at the top since it is mostly ethanol, and the surface tension of water at

    the bottom. For the second column, we use the surface tension of ethanol for both top

    and bottom. Note here that the ethanol surface tension used, is at 50C, as opposed to

    about 80C, which is the actual temperature of ethanol at the streams since this is the

    highest temperature that we can find. And for water, we used the surface tension at 30C

    while the actual stream is at 29C.

    ( )cm

    dynesCC ethanolethanol 475.88)50(80 =

    According to CRC Handbook of Chemistry, 80th

    edition,1999-2000.

    s

    m

    ft

    m

    s

    ftTopUnf 869.5

    3048.0

    475.88

    20

    17735.0

    17735.0806.78339.0)(

    2.05.0

    =

    =

    s

    m

    ft

    m

    s

    ftBottomUnf 544.10

    3048.0

    2.71

    20

    07937.0

    07937.0644.98640.0)(

    2.05.0

    =

    =

    Now we assume that we want to operate the column at 80% flooding, then the diameter

    of the column is given by the expression:

    ))((8.0

    '4

    gnfU

    VD

    =

    ( ) ( ) cmdynes

    CC waterwater 2.712930 =

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    Where is the fraction of the area available for vapor flow and since we picked the

    cheaper sieve tray, is 0.75.

    m

    m

    kg

    s

    m

    s

    hr

    hr

    kg

    TopD 457.2

    )17735.0)(75.0()869.5)(14.3(8.0

    3600)10660(4

    )(

    3

    =

    =

    m

    m

    kg

    s

    m

    s

    hr

    hr

    kg

    BottomD 717.1

    )07937.0)(75.0()544.10)(14.3(8.0

    3600)4187(4

    )(

    3

    =

    =

    mtopDbottomDD .457.2))(),(max((max) ==

    And we take this to be the diameter of our column. Summarizing the results:

    L'(kg/hr)

    V'(kg/hr)

    RhoL(kg/m^3)

    RhoV(kg/m^3) Flv (no unit) Csb (ft/s) Unf (m/s) D (m)

    Top 10554 10660 783.806 0.17735 0.014893 0.39 5.869 2.457

    Bottom 60.09 4187 986.644 0.07937 0.000129 0.4 10.544 1.717D(max)= 2.457 meters

    We perform the same calculation for column 2 as well, except that for column 2, we use

    the surface tension of ethanol for both top and bottom trays.

    To determine the column height, we use a rough approximation of the tray spacing of 0.6

    meter. So the total tray stack height would be:

    mnstacktrayH 6.0*)1()( =

    where n = number of trays, so for column 1:

    mmCH 6.186.0*)132()1( ==

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    Adding this to the extra feed space (1.5mX2 feed stages for column1), Disengagement

    space 1.5m), and skirt height (1.5m), gives the total height of the column.

    )()()()()( skirtHentDisengagemHspacefeedHstacktrayHcolumnH +++=

    Thus for column 1,

    mmmmmcolumnH 6.245.15.10.36.18)1( =+++=

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    Results

    Data Result

    As can see from the generated graph of the basic run, Figure 1 attached on the next page,

    we notice the excess number of trays in both columns one and two were used to obtain a

    100% pure ethanol. Thus this is a significant source of waste posed by the extra trays.

    The dimensions are also quite large. The diameters are 2.47 and 1.45 meters for column

    one and two ofBasic Run respectively. The lengths are 42.9 and 59.4 meters for column

    one and two. The number of trays is 60 and 90 for columns one and two. The feed enters

    at stage 58 for the first column, and at stage 10 for the entering recycle stream. For the

    second column, the feed enters at stage 10. The final product purity is 100% ethanol.

    However, we only need 99.9% ethanol, therefore we can reduce the amount of trays and

    reflux ratio.

    Foroptimal 2 case, the number of tray is reduced to 20 for the first column and 39 for the

    second column. The reflux ratio is also decreased to 25 and 18. With such a drastic cut

    in the tray number, the length column went down to 18.9 and 28.8 meters respectively.

    The diameter stays relatively the same, 2.47 and 1.24 meters. Here the feed enters at

    stage 18 and the recycle stream was introduced in stage 2. For the second column, the

    feed enters at stage 5.

    For the Hang1 case, the number of tray is 37 and 40 for the two columns. The reflux

    ratio is 4 and 2.5. As for the dimensions, the diameters are 1.08 and 0.52, however, the

    column heights reduced to 15.9 and 30.6 meters. Thus, the first column is only almost

    half of the second column in diameter. The feed enters at stage 25 and 2 for the entering

    recycle stream for the first column. For column two, the stream enters at second stage.

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    Since we have looked at the two extremes of number of tray and the lowest reflux ratio,

    now on the final optimal case, we try to even out the number of tray in both columns with

    the lowest reflux ratio possible to see if this would lower our overall cost.

    For the last case, Sandy2 case, the tray numbers are 32 and 26 for the two columns. The

    diameters are 2.46 and 0.95 meters. The heights are 26.10 and 21.0 meters respectively

    for the two columns. The reflux ratios are 25 and 10. For the entering streams of the first

    column, the feed enters at stage 22 and the recycle stream at 2. As of the second column,

    the stream enters at stage 2. Thus the following Table1 summarizes four different trials to

    provide a quick comparison between different runs.

    Runs Columns Num. OfTrays

    Diameter(m)

    Height(m)

    RefluxRatio

    Condenser HeatDuty (M*KJ/HR)

    Reboiler HeatDuty (M*KJ/HR)

    Pump Work(KW)

    Basic Run Column1 60 2.47 42.9 25 -10.258 10.2103 0.0142

    Column2 90 1.45 59.4 25 -8.6674 8.7227

    Optimal 2 Column1 20 2.47 18.9 25 -10.2793 10.2357 0.0142

    Column2 39 1.24 28.8 18 -6.3485 6.4039

    Hang1 Column1 37 1.08 29.1 4 -1.9542 1.9109 0.0142

    Column2 40 0.52 29.4 2.5 -1.1541 1.2093

    Sandy2 Column1 32 2.46 26.1 25 -10.0178 9.9747 0.0142

    Column2 26 0.95 21.0 10 -3.5678 3.6229

    Cost Analysis Results

    This section focuses on the economic factor in designing a separation process. According

    to the Basic Run, which would cost roughly 16 million dollars to purify 40% ethanol to

    99.9% pure. Comparing this cost value to the optimal runs, we see a significant

    improvement. For Optimal2 case, the NPV(cost) is only 13.8million dollars. Yet for

    Hang1 case, the cost is now only 2.7 million dollars. Thus we have saved around 82.9%

    of theBasic Run. Table 2 below summarizes the different types of cost for each run.

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    Runs Total

    Capital

    Cost ($)

    Total

    Annualize

    Utility Cost

    ($)

    NPV (Cost)

    ($)

    % Saved NPV

    (Cost)

    Basic Run 1254360 4918508 15980036 0

    Optimal2 615332 4353813 13802432 13.62702812

    Hang1 322485 817055 2733632 82.89345531

    Sandy2 621785 3597620 11483816 28.1364823

    We can see that the costs of all optimal runs are significantly less than that of the Basic

    Run. However, each of the trials has its own advantage and disadvantage as will be

    discussed in detail in the next section.

    The following Table 3 presents a rough calculation of the profit we would have obtained

    if the designs were to implement. Note that this represents a very crude calculation of the

    profit just so we would have an idea if this is actually profitable investment. We see that

    all the trials seem to yield reasonable gain. Even theBasic Run, which costs much higher

    than the other three optimal runs, brings 35 fold profits for a 10 years period. This

    indicates that either the retail-selling price is too high ($30/L of ethanol) or that the

    process does bring considerable gain. Either way, this evaluation confirms that the

    Hang1 run is still the best in term of economic factor.

    Profit Evaluation

    Basic Run Optimal2 Hang1 Sandy2

    Fixed Capital 1254360 615332 322485 621785

    Working Capital (0.20 f.c) 250872 123066.4 64497 124357

    Fixed and Working Capital 1505232 738398.4 386982 746142

    Product Rate (lb) 699031.77 699031.77 699031.77 699031.77

    Raw Material ($0.08/lb prod) 55922.54 55922.54 55922.54 55922.54

    Utilities ($0.012/lb prod) 8388.381 8388.381 8388.381 8388.381

    Labor ($0.015/lb prod) 0.015 10485.48 10485.48 10485.48

    Maintenance (0.06yr f.c.) 75261.6 36919.92 19349.1 37307.1

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    Supplies (0.02yr f.c.) 25087.2 12306.64 6449.7 12435.7

    Depreciation (straightline over ~10yrs) 125436 61533.2 32248.5 62178.5

    Taxes, insurance (0.03/year) 37630.8 18459.96 9674.55 18653.55

    Total Manufacturing Cost ($0.131/lb) 91573.16 91573.16 91573.16 91573.16

    Gross Sales 11982762 11982762 11982762 11982762

    Gross Profit (GS-TM) 11891189 11891189 11891189 11891189

    SARE Expenses (0.10sales tax) 1198276 1198276 1198276 1198276

    Net Profit Before Taxes (GP-SARE) 10692913 10692913 10692913 10692913

    Taxes (0.50 net profit) 5346456 5346456 5346456 5346456

    Net Profit after Taxes 5346456 5346456 5346456 5346456

    Return on Investment (ROI) (net income/ f&w cap) 35519% 72406% 138158% 71655%

    Payout Time (total cap./net annual profit) 0.1391369 0.0686598 0.0360817 0.0693757

    *Assume ethanol costs $30/Liter From Sigma

    Discussion

    Data Discussion

    As can see from Figure 1, the purity of ethanol actually reaches 100% long before the

    tray number reaches 60 trays for the first column of the Basic Run. Thus this indicates

    that there are significant number of excess trays in the first column. The extra number of

    tray would cost us an additional cost to operate this design. In order to reduce the cost

    yet at the same time achieving the ultimate goal, of producing 99.9% ethanol, the stage

    number can be cut down to the minimum amount. However, if we push for the border

    line amount of tray number, the ethanol purity might not reach 99.9%, thus adding an

    extra 5% of tray number would serve our purpose adequately. The lowest number of tray

    would give the lowest design dimensions, thus would lower the construction cost of such

    a design. For the optimized runs, we not only push for the lowest number of tray number

    but also minimizing the reflux ratio as well as the dimensions of the design. The same

    purpose would serve for having the lowest reflux ratio, this would give a lower cost for

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    the feeding steam entering the column. Also the feed tray number plays an important role

    in maximizing the design. The recycle stream and the stream from the first column to

    second column need to feed in at the top tray. This makes sense because the ethanol

    concentration in these two stream are saturated with ethanol, thus having them fed in the

    top trays would separate the water out more efficiently. With all these considerations in

    mind, we eventually derive the three optimal runs. The first run, Optimal 2, aims for the

    lowest possible distillation tray-number for the second column, yet still produces 99.9%

    ethanol. Since the number of tray for the second column is too high for theBasic Run,

    minimizing this would considerably lower the cost of building such a tall column.

    Having 20 trays in the first column and 39 trays in the second column results in a 99.9%

    ethanol release forOptimal2. However, as ProII iterates through the design, the system

    converges significantly slower than theBasic Run, this could be due to the high number

    of cycle the recycle stream has to reverse to the first column in order to obtain the desired

    purity. However, this trial was not considered to be a good design because the reflux

    ratio was quite high, causing a large heat duty amount in the reboiler and condenser, thus

    the cost of the feeding steam will be expensive.

    For the second run,Hang1, we minimize the reflux ratio with an intention that this would

    lower the utility cost of feeding steam into the columns. The reflux ratios are 4 and 2.5

    for the two columns. This design leads to only 1.9542 and 1.1541 MJ in heat duty of

    the condenser. Comparing this heat duty with that of the Basic Run, which is 10.258

    and 8.6674 MJ for the heat duty of the condenser. We see almost a 10 fold decrease in

    the heat duty. Thus the annualize utility cost of feeding steam is only $2,733,632, which

    is 83.39% less than the Basic Run for the NPV(cost). So far this design seems very

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    attractive in term of operating cost. However, there are drawbacks in having such a low

    reflux ratio design, the columns height is much higher in comparison to the previous

    runs. Now it requires more stage number to separate the mixtures to 99.9% ethanol. This

    however, is compromisable if our intention is to minimize the operation cost.

    As for our last design, Sandy2, we aim for the lowest number of trays in both columns,

    thus this would give us a relatively the same number of tray for both column. For this

    case the number of stage for column one is 32 while we only need 26 on the second

    column. This design might considered to be more advantageous over the previous two

    designs in term of space design, because the numbers of trays for both columns are close

    to each other. This offers a better design in the sense that construction would be much

    easier. The heights of both columns are not too tall or not too short in comparison to all

    the other runs. However, the reflux ratio is still high leading to a high utility cost. Once

    again, this demonstrates the need of priority when it comes to process design. If the

    intention is to save space and building columns that would fit in a designated area, this

    design would be more superior to the other two.

    Conclusion

    As can see from the three trials, low tray number does not necessarily mean that it is the

    better design, there are several other factors involve that can significantly affect the

    capacity of a design. The reflux ratio seems to dominate over all the other factors in term

    of cost. Thus the lower the reflux ratio, the lower the cost would be. However, too low

    of a reflux ratio would require higher distillation stage number. Thus when designing a

    separation process, one would need to consider how the space and location of where the

    columns are to be built and from there to determine the priorities in designing the

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    process. For our purpose, we try to obtain the lowest cost operation yet with a relatively

    not too high number of trays, thus, Hang1 run seems to serve our purpose. This design

    saves us $13 million in comparison to the Basic Run case. Thus it is important to have as

    low reflux ratio as possible yet with reasonable column height in order to maximize profit

    of a design.

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    Contribution

    Marie Dang: Runs column, designs an optimal case and analyzes that particular case as

    well as contributing in writing the report.

    Sandy Lao: Runs column, designs an optimal case, analyzes that particular case and

    participate in writing the report.

    Hang-Tam Nguyen: Runs the column, designs an optimal case, analyzes that particular

    case and writing the report.

    Table of Index

    1. First Report: Base Case Run Report

    2. Second Report: Optimal 2 Run Report

    3. Third Report: Optimal 3 Run Report

    4. Fourth Report: Sandy2 Run Report

    5. Dimensional Analysis Report For All Runs

    6. Cost Analysis Report For All Runs