ANKARA 2013

GAZİ UNIVERSITY ENGINEERING FACULTY

DEPARTMENT OF CHEMICAL ENGINEERING

KM451E CHEMICAL ENGINEERING DESIGN I

ASSIGMENT IV: DISTILLATION COLUMN DESIGN

DELIVERED DATE : 30.12.2013 DELIVERED TO : PROF. DR. BEKİR ZÜHTÜ UYSAL

: RES. ASIST. MELDA ESKİTOROS

09114003 EMRE AKASLAN

i

ABSTRACT

In this report, the aim is to design the optimum economical distillation column for seperation

of acetone, ethanol and water mixture. This mixture is desired to be distilled to 99.9 % pure

components.

The feed of first distillation column is 190 000 kg/h. We used four distillation columns to

distillate mesitylene, n-buthanol, water, ethanol and acetone and we done detailed calculation

and found optimum Rd/Rdmin parameter for third column. We used partial condensers for

first, second and third column and we used total condenser for last column.

The third (designed column) column’ s feed is 351 kmol/h. The mole fraction in feed acetone

is 0.1118, ethanol is 0.0470 and water is 0.8412. We selected heavy component as water and

light component as ethanol. Water is distilled to 99.99% outlet composition from the bottom

of distillation column. Distillate of column is fed to the last column which is binary

distillation column. The products of this column are 99.9% acetone and 99.9% ethanol.

Calculations are done by using these decisions.

Three different calculation methods are employed.

ChemCad Simulation program

Microsoft excel program

GWBasic Software program

ChemCad simulation program is run after deciding on distillation columns arrangement. In

calculations the temperatures of exit streams from program are used for determining the

physicochemical properties of components and in rough calculations taken ideal number of

plates are used to calculate pressure drops. Pressure drop is found as about 0.18 atm.

After detailed calculations, we found optimum Rd/Rdmin value as 1.1 and on this way we

found Total Annual Cost as 2 452 259 TL/yr for using steam cost as 40 TL/ton. Then we done

a calculation again to see effect steam cost on Total Annual Cost. Taking steam cost as 16

TL/ton we found Total Annual Cost as 1 442 001 TL/yr. We discussed this results.

GWBasic Software program is run to check the results of ChemCad and excel program for

optimum value. We compared them and it is seen that the results for ideal number of plates

are same.

ii

INDEX

ABSTRACT ................................................................................................................................ i

INDEX ....................................................................................................................................... ii

FIGURE AND TABLE LIST ................................................................................................... iv

1. INTRODUCTION .................................................................................................................. 1

1.1. Bioacetone ....................................................................................................................... 2

1.1.1. Bioacetone Production .............................................................................................. 2

1.2. Bioethanol ........................................................................................................................ 3

1.2.1. Bioethanol Production .............................................................................................. 3

1.3. Biobuthanol ..................................................................................................................... 4

1.3.1. Biobuthanol Production ............................................................................................ 4

1.4. Distillation ....................................................................................................................... 5

1.4.1. Basic Components of Distillation Columns .............................................................. 5

1.4.1.1. Trays ................................................................................................................... 7

1.4.2. Continuous Distillation ........................................................................................... 10

1.4.2.1. Reflux Considerations ...................................................................................... 11

1.4.2.2. Selection of Column Pressure .......................................................................... 12

1.2.2.3. Dew Points and Bubble Points ......................................................................... 12

1.4.3. Multicomponent Distillation ................................................................................... 13

1.4.3.1. Key Components .............................................................................................. 14

1.4.3.2. Number and Sequencing of Columns ............................................................... 14

1.5. Distillation Column Design ........................................................................................... 15

2. PROBLEM STATEMENT .................................................................................................. 16

3. METHOD OF CALCULATIONS ...................................................................................... 17

3.1. Assumptions .................................................................................................................. 26

4. SAMPLE CALCULATIONS .............................................................................................. 27

5. RESULTS ............................................................................................................................ 56

6. DISCUSSION ...................................................................................................................... 59

7. CONCLUSION .................................................................................................................... 62

8. SYMBOLS ........................................................................................................................... 63

9. REFERENCES ..................................................................................................................... 65

APPENDIX-A: PHYSIOCHEMICAL PROPERTIES OF COMPONENTS .......................... 67

APPENDIX-B: FIGURES WHICH ARE USED ON CALCULATIONS .............................. 69

iii

APPENDIX-C: GWBASIC PROGRAM RESULTS .............................................................. 74

APPENDIX-D: CHEMCAD RESULTS ................................................................................. 76

APPENDIX-E: ECONOMICAL RESULTS ........................................................................... 81

APPENDIX-F: CHEMCAD, EXCEL AND GW BASIC RESULTS COMPARATIONS .... 83

APPENDIX-G: EXCEL RESULTS ........................................................................................ 84

APPENDIX-H: DETAILED FLOW CHART ......................................................................... 96

 

1. INTR

Figure

In this

distillati

column

the last

optimum

Figure

RODUCTI

1: Basic Flo

project, to

ion column

is seperatin

one is sepe

m paramete

2: Detailed

ON

owchart for

distillate m

ns, one heat

ng mesithyl

erating etha

rs.

Flowchart

r Distillation

mesithylene

t exchanger

lene, second

anol. We do

for Third (D

n System

e, n-buthano

r and pump

d is seperati

one detailed

Designed) C

ol, water, e

ps are used

ing buthano

d calculation

Column

ethanol, ace

d shown in

ol, third is se

ns for third

etone mixtu

Figure 1. T

eperating w

d column an

1

ure; four

The first

water and

nd found

2  

As seen from Figure 2. For distillation column partial reboiler, partial condenser, pump for

reboiler and pump for condenser are used. Water, ethanol and acetone mixture is seperated

with third column and optimum parameters are found.

1.1. Bioacetone

Bioacetone is an organic solvent which is produced using fermentation processes. Using the

microorganism, Clostridium acetobutylicum, acetone is produced from starch. From the

1930’s to the 1960’s, this was the primary method of acetone production. However, in the mid

1960’s, the chemical pathway for acetone production became less expensive and thus more

efficient. Now, due to dwindling petroleum supplies and changes in public positions, the

process is shifting back to the use of fermentative means in order to produce bioacetone.

Acetone, or 2-propanone, is a common industrial solvent and chemical precursor. It is

generally utilized as a solvent in plastics, coatings, and various pharmaceuticals. Classified as

a ketone, it is employed as a chemical precursor with ketone properties. It can be found in

products such as methyl methacrylate, acetone cyanohydrins, and Vitamin C. Common

household uses are in nail polish remover and paint thinners. Acetone is also used in

superglue as a solvent to prevent setting. Evaporation of the solvent causes the solidification

of the glue. [1]

1.1.1. Bioacetone Production

Bioacetone is produced using the ABE fermentation process. ABE stands for acetone-butanol-

ethanol and is the fermentative process used to create all three. ABE fermentation occurs in

anaerobic conditions and is carried out by bacteria from the Clostridia class. The most popular

strain of Clostridia used is Clostridium acetobutylicum, which yields the solvents in a 3:6:1

ratio. The ratio is representative of 3 parts acetone, 6 parts butanol, and 1 part ethanol. It can

be shifted with the aid of genetic and metabolic engineering by heightening the activity of the

enzymes responsible for each conversion. Once produced, the solvents must be separated,

both from the bacteria and from each other. This process is still under investigation for the

most efficient method. [1]

3  

1.2. Bioethanol

The principle fuel used as a petrol substitute for road transport vehicles is bioethanol.

Bioethanol fuel is mainly produced by the sugar fermentation process, although it can also be

manufactured by the chemical process of reacting ethylene with steam.

The main sources of sugar required to produce ethanol come from fuel or energy crops. These

crops are grown specifically for energy use and include corn, maize and wheat crops, waste

straw, willow and popular trees, sawdust, reed canary grass, cord grasses, jerusalem artichoke,

myscanthus and sorghum plants. There is also ongoing research and development into the use

of municipal solid wastes to produce ethanol fuel.

Ethanol or ethyl alcohol (C2H5OH) is a clear colorless liquid, it is biodegradable, low in

toxicity and causes little environmental pollution if spilt. Ethanol burns to produce carbon

dioxide and water. Ethanol is a high octane fuel and has replaced lead as an octane enhancer

in petrol. By blending ethanol with gasoline we can also oxygenate the fuel mixture so it

burns more completely and reduces polluting emissions. Ethanol fuel blends are widely sold

in the United States. The most common blend is 10% ethanol and 90% petrol (E10). Vehicle

engines require no modifications to run on E10 and vehicle warranties are unaffected also.

Only flexible fuel vehicles can run on up to 85% ethanol and 15% petrol blends (E85). [2]

1.2.1. Bioethanol Production

Ethanol can be produced from biomass by the hydrolysis and sugar fermentation processes.

Biomass wastes contain a complex mixture of carbohydrate polymers from the plant cell walls

known as cellulose, hemi cellulose and lignin. In order to produce sugars from the biomass,

the biomass is pre-treated with acids or enzymes in order to reduce the size of the feedstock

and to open up the plant structure. The cellulose and the hemi cellulose portions are broken

down (hydrolysed) by enzymes or dilute acids into sucrose sugar that is then fermented into

ethanol. The lignin which is also present in the biomass is normally used as a fuel for the

ethanol production plants boilers. There are three principle methods of extracting sugars from

biomass. These are concentrated acid hydrolysis, dilute acid hydrolysis and enzymatic

hydrolysis. [2]

4  

1.3. Biobuthanol

Biobutanol, which is also sometimes called biogasoline, is an alcohol that is produced from

biomass feedstocks. Butanol is a 4-carbon alcohol that is currently used as an industrial

solvent in many wood finishing products. Biobutanol can be utilized in internal combustion

engines as both a gasoline additive and or a fuel blend with gasoline. The energy content of

biobutanol is 10% less than that of regular gasoline. This is not as bad as energy density of

ethanol is 40% lower. Since biobutanol is more chemically similar to gasoline than ethanol, it

can be integrated into regular internal combustion engines easier than ethanol. Its

bioproduction route was halted in the 1960s due to high production price with respect to

production from petroeum. New technology advancements and an increase in petroleum

prices are making bioproduction of butanol more competitive and safer. Biobutanol has

displayed the potential to reduce the carbon emissions by 85 percent when compared to

gasoline, making it a superior alternative to gasoline and a gasoline-ethanol blended fuel. [3]

1.3.1. Biobuthanol Production

Biobutanol is made via fermentation of biomasses from substrates ranging from corn grain,

corn stovers and other feedstocks. Microbes, specifically of the Clostridium acetobutylicum,

are introduced to the sugars produced from the biomass. These sugars are broken down into

various alcohols, which include ethanol and butanol. Unfortunately, a rise in alcohol

concentration causes the butanol to be toxic to the microorganisms, killing them off after a

period of time. This made the fermentation process expensive and unrealistic when compared

to the petroleum costs of the late 50’s. Luckily, new technological advances and the discovery

of new microbes have improved the efficiency and cost of the fermentation process

tremendously. Through genetic engineering, researchers have been able to modify the most

efficient microbes to be able to withstand high alcohol concentrations. New modifications are

constantly being researched, including the modification to enzymes and genes involved in

butanol formation from biomass fermentation.

A promising trend is a slew of recent ethanol fermentation plants purchases by biobutanol

companies. These ethanol plants are being retrofitted with advanced separation systems to

allow them to produce biobutanol. Since biobutanol has inherently higher value vs.

bioethanol, the trend of the plant conversions is likely to continue.

5  

Aside from fermentation, a handful of companies are pursuing pyrolysis biobutanol. This

route can convert waste biomass or crop waste into biobutanol. [3]

1.4. Distillation

Whenever two materials at any temperature possessed a marked difference in their vapor

pressures, this difference could be made the basis of a method of separation of the two; and if

one or both of the substances were recovered by condensation, the process is called

distillation. Equilibrium is established at any temperature between a liquid or a mixture of

liquids held in a containing vessel, and the vapor existing above it.

There are a variety of configurations for distillation columns, each designed to perform

specific types of separations. A simplified way of classifying distillation columns is to look at

how they are operated. In this manner, the two major types are batch and continuous columns.

In a batch operation, the feed to the column is introduced batch-wise. That is, the column is

charged with a ‘batch’ and then the distillation process is conducted. When the desired

separation is achieved, a next batch of feed is introduced. In contrast, continuous columns

process a continuous feed stream. No interruptions occur unless there is a problem or upsets

with the column or surrounding process units. They are capable of handling high throughputs

and are the more common of the two types. The following discussions focus on continuous

columns. [4]

1.4.1. Basic Components of Distillation Columns

There are several important components in a distillation column, each of which is used either

to transfer heat energy or enhance mass transfer. The major components in a typical

distillation are:

A vertical shell where the separation of liquid components is carried out,

Column internals such as tray, plates and/or packing which are used to enhance

component separations,

A reboiler to provide the necessary vaporization for the distillation process, a

condenser to cool and condense the vapor leaving the top of the column,

A reflux drum to hold the condensed vapor from the top of the column. The liquid

(reflux) is recycled back to the column.

 

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9: Distillati

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11  

1.4.2.1. Reflux Considerations

The reflux ratio, R, is normally defined as:

     

         

The number of stages required for a given separation will be dependent on the reflux ratio

used.

In an operating column the effective reflux ratio will be increased by vapor condensed within

the column due to heat leakage through the walls. With a well-lagged column the heat loss

will be small and no allowance is normally made for this increased flow in design

calculations. If a column is poorly insulated, changes in the internal reflux due to sudden

changes in the external conditions, such as a sudden rain storm, can have a noticeable effect

on the column operation and control.

Total Reflux: Total reflux is the condition when all the condensate is returned to the column

as reflux: no product is taken off and there is no feed.

At total reflux the number of stages required for a given separation is the minimum at which it

is theoretically possible to achieve the separation. Though not a practical operating condition,

it is a useful guide to the likely number of stages that will be needed. The testing of columns

is conveniently carried out at total reflux.

Minimum Reflux: As the reflux ratio is reduced a pinch point will occur at which the

separation can only be achieved with an infinite number of stages. This sets the minimum

possible reflux ratio for the specified separation.

Optimum Reflux Ratio: Practical reflux ratios will lie somewhere between the minimum for

the specified separation and total reflux. The designer must select a value at which the

specified separation is achieved at minimum cost. Increasing the reflux reduces the number of

stages required, and hence the capital cost, but increases the service requirements (steam and

water) and the operating costs. The optimum reflux ratio will be that which gives the lowest

annual operating cost. No hard and fast rules can be given for the selection of the design

reflux ratio, but for many systems the optimum will lie between 1.2 to 1.5 times the minimum

reflux ratio.

12  

For new designs, where the ratio cannot be decided on from past experience, the effect of

reflux ratio on the number of stages can be investigated using the short-cut design methods.

This will usually indicate the best of value to use in more rigorous design methods.

At low reflux ratios the calculated number of stages will be very dependent on the accuracy of

the vapor-liquid equilibrium data available. If the data are suspect a higher than normal ratio

should be selected to give more confidence in the design.

1.4.2.2. Selection of Column Pressure

Except when distilling heat-sensitive materials, the main consideration when selecting the

column operating-pressure will be to ensure that the dew point of the distillate is above that

which can be easily obtained with the plant cooling water. The maximum, summer,

temperature of cooling water is usually taken as 30°C. If this means that high pressures will

be needed, the provision of refrigerated brine cooling should be considered. Vacuum

operation is used to reduce the column temperatures for the distillation of heat-sensitive

materials and where very high temperatures would otherwise be needed to distilled relatively

non-volatile materials.

When calculating the stage and reflux requirements it is usual to take the operating pressure as

constant throughout the column. In vacuum columns, the column pressure drop will be a

significant fraction of the total pressure and the change in pressure up the column should be

allowed for when calculating the stage temperatures. This may require a trial and error

calculation, as clearly the pressure drop cannot be estimated before an estimate of the number

of stages is made.

1.2.2.3. Dew Points and Bubble Points

To estimate the stage, and the condenser and reboiler temperatures, procedures are required

for calculating dew and bubble points. By definition, a saturated liquid is at its bubble point

(any rise in temperature will cause a bubble of vapor to form), and a saturated vapor is at its

dew point (any drop in temperature will cause a drop of liquid to form).

Dew points and bubble points can be calculated from knowledge of the vapor-liquid

equilibrium for the system. For multicomponent mixtures the temperature that satisfies these

equations, at a given system pressure, must be found by trial and error. For binary systems the

13  

equations can be solved more readily because the component compositions are not

independent; fixing one fixes the other.

1.4.3. Multicomponent Distillation

The problem of determining the stage and reflux requirements for multicomponent

distillations is much more complex than for binary mixtures. With a multicomponent mixture,

fixing one component composition does not uniquely determine the other component

compositions and the stage temperature. Also when the feed contains more than two

components it is not possible to specify the complete composition of the top and bottom

products independently. The separation between the top and bottom products is specified by

setting limits on two “key” components, between which it is desired to make the separation.

The complexity of multicomponent distillation calculations can be appreciated by considering

a typical problem. The normal procedure is to solve the MESH equations stage-by-stage, from

the top and bottom of the column toward the feed point. For such a calculation to be exact the

compositions obtained from both the bottom up and top-down calculations must mesh at the

feed point and match the feed composition. But the calculated compositions will depend on

the compositions assumed for the top and bottom products at the commencement of the

calculations. Though it is possible to match the key components, the other components will

not match unless the designer was particularly fortunate in choosing the trial top and bottom

compositions. For a completely rigorous solution the compositions must be adjusted and the

calculations repeated until a satisfactory mesh at the feed point is obtained. Clearly, the

greater the number of components, the more difficult the problem. Trial-and error calculations

will be needed to determine the stage temperatures. For other than ideal mixtures, the

calculations will be further complicated by the fact that the component volatilities will be

functions of the unknown stage compositions. If more than a few stages are required, stage-

by-stage calculations are complex and tedious.

The short-cut methods available can be divided into two classes:

1. Simplification of the rigorous stage-by-stage procedures to enable the calculations to be

done by hand, or graphically.

2. Empirical methods, which are based on the performance of operating columns, or the

results of rigorous designs.

14  

1.4.3.1. Key Components

Before commencing the column design, the designer must select the two “key” components

between which it is desired to make the separation. The light key will be the component that it

is desired to keep out of the bottom product, and the heavy key the component to be kept out

of the top product. Specifications will be set on the maximum concentrations of the keys in

the top and bottom products. The keys are known as “adjacent keys” if they are “adjacent” in

a listing of the components in order of volatility, and “split keys” if some other component

lies between them in the order; they will usually be adjacent.

Which components are the key components will normally be clear, but sometimes,

particularly if close boiling isomers are present, judgments must be used in their selection.

If any uncertainty exists, trial calculations should be made using different components as the

keys to determine the pair that requires the largest number of stages for separation (the worst

case). The Fenske equation can be used for these calculations.

The “non-key” components that appear in both top and bottom products are known as

“distributed” components; and those that are not present, to any significant extent, in one or

other product, are known as “non-distributed” components.

1.4.3.2. Number and Sequencing of Columns

In multicomponent distillations it is not possible to obtain more than one pure component, one

sharp separation, in a single column. If a multicomponent feed is to be split into two or more

virtually pure products, several columns will be needed. Impure products can be taken off as

side streams; and the removal of a side stream from a stage where a minor component is

concentrated will reduce the concentration of that component in the main product.

For separation of N components, with one essentially pure component taken overhead, or

from the bottom of each column, (N-1) columns will be needed to obtain complete separation

of all components. For example, to separate a mixture of benzene, toluene and xylene two

columns are needed (3-1). Benzene is taken overhead from the first column and the bottom

product, essentially free of benzene, is fed to the second column. This column separates the

toluene and xylene.

15  

The order in which the components are separated will determine the capital and operating

costs. Where there are several components the number of possible sequences can be very

large; for example, with five components the number is 14, whereas with ten components it is

near 5000. When designing systems that require the separation of several components,

efficient procedures are needed to determine the optimum sequence of separation.

1.5. Distillation Column Design

The design of a distillation column can be divided into the following steps:

1. Specify the degree of separation required: set product specifications.

2. Select the operating conditions: batch or continuous; operating pressure.

3. Select the type of contacting device: plates or packing.

4. Determine the stage and reflux requirements: the number of equilibrium stages.

5. Size the column: diameter, number of real stages.

6. Design the column internals: plates, distributors, packing supports.

7. Mechanical design: vessel and internal fittings.

The principal step will be to determine the stage and reflux requirements. This is a relatively

simple procedure when the feed is a binary mixture, but a complex and difficult task when the

feed contains more than two components (multicomponent systems). [6]

16  

2. PROBLEM STATEMENT

Bio-technology is gaining increasing importance due to the limited reserves of fossil fuels

which have been used substantially in the last decades to produce practically all the chemicals

that our modern world needs. Our company, which sees the necessity to shift to bio-

technology, decided to produce acetone, buthanol and ethanol from starch via ABE

fermentation process that uses bacterial anaerobic fermentation.

The products are recovered from fermentation medium by extraction using mesitylene as the

solvent. The extract phase is avaible at room temperature and atmospheric pressure, and has

the following composition;

Components wt%

Acetone 1.2

Butanol 2.4

Ethanol 0.4

Water 2.8

Mesitylene 93.2

It is desired to produce acetone, butanol and ethanol, each with 99 % purity, by distillation.

Our engineering group is expected to recommend as a reasonable layout for this separation

and is particularly responsible for the design of the 190 ton/h distillation column.

17  

3. METHOD OF CALCULATIONS [7]

Decide on heavy key and light key,

Decide on distillation column arrangement,

Run ChemCad Simulation,

Find number of theoretical plates (N) and feed plate location for column,

Calculate average densitiy of feed streams,

Calculate pressure drop and feed plate pressure for column;

∆ (1)

Material balance calculations for column;

Calculate molar flow rate of each component in inlet stream;

(2)

Calculate distillate and bottom flow rates with total material balance for water

(3)

(4)

Determine mole fractions in distillate and bottom

(5)

Assume water mole fraction in distillate

1 (6)

Get operating temperature of condenser and reboiler from Chemcad

Calculate vapor pressures for each component from Antoine Equation

  (7)

Determine dew and bubble point by using excel trial and error method

Calculate partial pressures for each components

(8)

Determine total pressure

∑ (9)

Calculate relative volatilities for column

∝ (10)

Calculate average volatilities

∝ ∝ ∝ (11)

18  

Determine q value,

  1      , 0     

Calculate value

∑∝

∝1 (12)

Calculate RD min

∑∝

∝   1 (13)

Determine number of theoretical stages including partial reboiler from Fenske

Equation

1∝

(14)

Calculate number of theoretical plates from Gilliland Correlation

  (15)

1.

. √ (16)

(17)

Determine total column efficiency from O’Connell Correlation

∑

(18)

51 32.5 ∝ (19)

Determine actual number of plate

(20)

Determine ideal number of plates in stripping and enriching section from Kirkbride

Correlation

0.206 (21)

1 (22)

(23)

Calculate height of the column

3.25 1 (24)

19  

Calculate mass flow rate of distillate and bottom

∑ (25)

  (26)

(27)

Calculate Lo

(28)

Calculate Vn+1

(29)

Calculate Lm

(30)

Calculate Vm+1

(31)

Calculate average density of vapor

 

  (32)

Diameter calculations for bottom and top

Calculate FLV for top of the column

(33)

Calculate FLV for bottom of the column

(34)

Find KF  from Figure 11.

Calculate entrainment velocity

(35)

Take design parameter (F*) between 0.75-0.80

Calculate linear velocity

∗ (36)

Calculate volumetric flow rate of vapor phase

(37)

Calculate total cross-sectional area of the column

.  

(38)

20  

Calculate diameter of the column

   

(39)

Cost of the plate column

Calculate column wall thickness

 

(40)

Calculate weight of shell

Calculate base cost

(41)

Determine material factors for the shell (FM)

Calculate cost of the shell of the column

(42)

Calculate base cost for the plate

340  . (43)

Calculate material factors for plates

(44)

Determine plate type factor (FRT)

Determine correction factor (FNR)

Calculate cost of the plates

(45)

Calculate cost of platform and ladder

(46)

Calculate total cost of the column

(47)

Calculate heat capacity of condenser

For partial condenser

(48)

Calculate mass flow rate of water

(49)

21  

Calculate ΔTLM

Δ (50)

Assume overall heat transfer coefficient

Calculate area of condenser

 Δ

(51)

Determine cost of condenser from Figure 12.

Calculate cost of water

Calculate heat capacity of partial reboiler

(52)

Calculate mass flow rate of steam

(53)

Determine steam properties (pressure and temperature of inlet and outlet)

Calculate ΔT

Δ (54)

Assume overall heat transfer coefficient

Calculate area of partial reboiler

 Δ

(55)

Determine cost of reboiler from Figure 12.

Calculate cost of steam

Calculate optimum pipe diameter

For turbulent flow and Di ≥ 0.0254m

, 0.363 . . (56)

Calculate volumetric flow rate

(57)

Calculate area of pump

, (58)

Calculate linear velocity

(59)

22  

Calculate Reynold Number

(60)

Calculate Wp

(61)

Calculate power of pump

(62)

Calculate cost of electricity

Determine cost of pump from Figure 13.

23  

Detailed Cost Calculations;

Direct Costs (DC)

1. Purchased Equipment Cost (Column + Condenser + Reboiler + Pump’s Costs) (64)

2. Installation, Including Insulation and Painting Cost = 0.50 x PEC (65)

3. Instrumentation and Controls, Installed = 0.25 x PEC (66)

4. Electrical, Installed= 0.20 x PEC (67)

5. Piping, Installed = 0.30 x PEC (68)

Direct Cost = Pec. + Ins. + Inst. + Elec. + Pip. (69)

Indirect Costs(IC)

1. Engineering and Supervision = 0.20 x DC (70)

2. Legal Expenses = X

3. Construction Expense and Contractor’s Fee= 0.20 x FCI (71)

4. Contingency = 0.05 x FCI (72)

Indirect Costs = Eng. & Sup. + Cons. & Cont. + Contin. (73)

Fixed Capital Investment = DC+IC (74)

Fixed Charges

1. Depreciation = (1/15) x FCI (15 years service life) (75)

2. Local Taxes = X

3. Insurance = 0.005 x FCI (76)

4. Rent = X

5. Financing = X

Fixed Cost = Dep. + Insr. (77)

Operating Costs

1. Raw Materials = X

2. Operating Labor = %25 Technician(1 Technician’s Salary = 2200TL), %10 Engineer (1

Engineer’s Salary = 3500TL)

(78)

3. Direct Supervisory and Clerical Labor =X

4. Utilities = (Cooling Water’s Cost + Electricity Cost for Pumps + Steam’s Cost) (79)

5. Maintenance and Repairs = 0.05 x FCI (80)

6. Operating Supplies = X

7. Laboratory Charges = X

8. Patents and Royalities = X

OC= Mant. & Rep. + Op. Lab. + Util. (81)

Total Annual Cost For System = Fixed Costs + Operating Costs (82)

 

P

Figu

Plate Desig

ure 10: Siev

Volumetr

Length of

Area of d

Net area

Area of h

Active are

Perforated

≅

Number o

For triang

gn; [7]

ve Tray Phe

ric flow rate

f weir

0.77

rain channe

0.12

0.88

oles

0.1

ea

0.76

d area

≅ 2

of holes

gular pitch

0.95 

enomena an

e for liquid p

el

 

nd Pressure R

phase

Relation

24

(86)

(87)

(88)

(89)

(90)

(91)

(92)

(93)

(94)

25  

Determine drag ratio (ψ) from Figure B.4

Liquid entrainment

(95)

Vapor velocity in holes

(96)

Determine dry orifice coefficient (Cvo) from Figure B.5

Pressure drop in dry plate

Δ 5.08ρ

ρu (97)

Bubble parameter

(98)

Determine bubble factor (Qp) from Figure B.6

Height of liquid above weir

66.6.

(99)

Bubbled liquid height

(100)

Total plate pressure drop

Δ Δ (101)

Pressure drop from bubbling

4.14 10 (102)

Check weeping from Figure B.7

Velocity of the liquid in the decent duct

(103)

The time passed during the stay of liquid in decent duct

(104)

Height of Foam on the Plate

(105)

Hydraulic Radius of the Bubbled

(106)

26  

(107)

Determine density of foam (ϕ) from Figure B.6

Velocity of bubbled mass

(108)

Reynolds module

(109)

Determine friction coefficient (f) from Figure B.8

Liquid gradient

∆ 100 (110)

Height of liquid in decent duct

(apron space) (111)

16.5 (112)

Check plate space assumption

hdc Pdry + hw + how + + hda (113)

For bubbling liquids:

(114)

For non-bubbling liquids:

0.9 (115)

3.1. Assumptions

hw= 0.05m

x 0.0001

F*=0.80

For partial condenser U=750 W/m2K

For partial reboiler U= 1200 W/m2K

Pump efficiency = 0.75

ld = 0.075 m

27  

4. SAMPLE CALCULATIONS

28  

29  

30  

31  

32  

33  

34  

35  

36  

37  

38  

39  

40  

41  

42  

43  

44  

45  

46  

47  

48  

49  

50  

51  

52  

53  

54  

55  

 

 

 

56  

5. RESULTS

3rd Column

Feed, kmol/h 351 Distillate, kmol/h 55.71 Bottom, kmol/h 295.29

x(acetone),F 0.1118 x(acetone),D 0.7043 x(acetone),B 0

x(ethanol),F 0.047 x(ethanol),D 0.2956 x(ethanol),B 0.0001

x(water),F 0.8412 x(water),D 0.0001 x(water),B 0.9999

Partial Condenser Partial Reboiler Flows in Column

Operating

Temperature. oC 65.66 Operating Temperature.°C 104.36 Lo, kg/s 8.59

Operating Pressure. atm 1.15 Operating Pressure. atm 1.18 V1, kg/s 9.43

Duty. kW 3103.5 Duty. kW 3162.6 Lm, kg/s 10.92

U. W/m2-K 750 U. W/m2-K 1200 Vm, kg/s 9.42

m(water). kg/s 35.37 m(steam). kg/s 1.46

Column Properties Plate Properties

RDmin 9.697 Column Efficiency.Eo(%) 81 ΔPdry (cm liq. column) 2.389

RD/RDmin 1.1 Number of Plates 59 Δptotal (cm liq. column) 9.236

RD 10.67 Feed Plate 42 Weeping Yes

Nmin 20 Height.m 27.5 Number of holes 64106

Ntheoretical 47 Diameter.m 3.8

57  

Graph 1. TAC, OC, FC vs. RD/RD,min (Steam Cost: 40 TL/ton)

Table 1. Detailed Cost Analysis Results for Steam Cost 40 TL/ton

DETAILED COST ANALYSIS Direct costs Purchased Equipment 1 639 666 TL Installation 819 833 TL Instrumentation and Controls 409 917 TL Piping 491 900 TL Electrical, Installed 327 933 TL TOTAL DIRECT COST 3 689 909 TL Indirect Costs Engineering and Supervision 737 862 TL Construction Expense and Contractor's Fee 1 180 578 TL Contingency 295 144 TL TOTAL INDIRECT COST 2 213 586 TL FIXED-CAPITAL INVESTMENT(TL) 5 902 894 TL Depreciation 393 526 TL/yr Insurance 29 515 TL/yr FIXED-CHARGES 423 041 TL/yr Maintenance and Repairs 295 145 TL/yr Utilities 1 723 273 TL/yr OPERATING COST 2 029 218 TL/yr TOTAL ANNUAL COST(TL/year) 2 452 259 TL/yr

280000530000780000

1030000128000015300001780000203000022800002530000278000030300003280000353000037800004030000

1 1,1 1,2 1,3 1,4 1,5 1,6 1,7 1,8 1,9 2 2,1

COST (TL/yr)

RD/RDmin

TAC, OC, FC vs. RD/RDmin (Steam Cost: 40 TL/ton)

FC (TL/yr)

OC (TL/yr)

TAC (TL/yr)

58  

Graph 2. TAC, OC, FC vs. RD/RD,min (Steam Cost: 16 TL/ton)

Table 2. Detailed Cost Analysis Results for Steam Cost 16 TL/ton

DETAILED COST ANALYSIS Direct costs Purchased Equipment 1 639 666 TL Installation 819 833 TL Instrumentation and Controls 409 917 TL Piping 491 900 TL Electrical, Installed 327 933 TL TOTAL DIRECT COST 3 689 909 TL Indirect Costs Engineering and Supervision 737 862 TL Construction Expense and Contractor's Fee 1 180 578 TL Contingency 295 144 TL TOTAL INDIRECT COST 2 213 586 TL FIXED-CAPITAL INVESTMENT(TL) 5 902 894 TL Depreciation 393 526 TL/yr Insurance 29 515 TL/yr FIXED-CHARGES 423 041 TL/yr Maintenance and Repairs 295 145 TL/yr Utilities 713 015 TL/yr OPERATING COST 1 019 030 TL/yr TOTAL ANNUAL COST(TL/year) 1 442 001 TL/yr

340000

490000

640000

790000

940000

1090000

1240000

1390000

1540000

1690000

1840000

1990000

2140000

2290000

1 1,1 1,2 1,3 1,4 1,5 1,6 1,7 1,8 1,9 2 2,1

COST (TL/yr)

RD/RDmin

TAC, OC, FC vs. RD/RDmin (Steam Cost: 16 TL/ton)

FC (TL/yr)

OC (TL/yr)

TAC (TL/yr)

59  

6. DISCUSSION

In this project, the main aim was design the optimum economical distillation column for

seperation of acetone, ethanol and water mixture. This mixture is desired to be distilled to

99.9 % pure components.

The feed of first distillation column is 190 000 kg/h. We used four distillation columns to

distillate mesitylene, n-buthanol, water, ethanol and acetone and we done detailed calculation

and found optimum Rd/Rdmin parameter for third column. We used partial condensers for

first, second and third column and we used total condenser for last column.

On ChemCad we used 0.9999 light key split for first and second column and looked at third

column stages number than we used 0.99 and 0.999 light key split for first and second column

then we have seen that we must use extra one column for bottom product of third column to

seperate ethanol and water. But using 0.9999 light key split at first and second column is more

economic, because total number of stages of first, second and third column is lower than

adding extra one column.

The cause of using partial condenser is about cooling water cost. If we used total condenser

for first, second and third column in this system, the cooling water cost will increase, so we

just used total condenser for last column.

The third (designed column) column’ s feed is 351 kmol/h. The mole fraction in feed acetone

is 0.1118, ethanol is 0.0470 and water is 0.8412. We selected heavy component as water and

light component as ethanol. Water is distilled to 99.99% outlet composition from the bottom

of distillation column. Distillate of column is fed to the last column which is binary

distillation column. The products of this column are 99.9% acetone and 99.9% ethanol.

Calculations are done by using these decisions.

After distillation; acetone, ethanol and water’ s mole fractions are found as 0.7043, 0.2956,

0.0001 for distillate. About bottom they are found 0, 0.0001, 0.9999 by completing material

balance.

The efficiency of column is found about 80 %. On calculations q taken as “1” because feed

was saturated vapor.

We have done calculations for two situations. One of them is taking steam cost as 40 TL/ton

(for Turkey) and the other one is taking steam cost as 16 TL/ton (for U.S.A.). We want to see

60  

effect of steam cost to total annual cost. And the results show that for first situation there is no

optimum point on Graph 1. and for second situation we found an optimum value which is 1.1

Rd/Rd,min ratio on Graph 2. and we done calculations using this optimum point. When cost

of steam increases, total annual cost increases.

After calculation we found diameter of column as about 3.8 m, height of column as 27.5 m,

minimum reflux ratio as about 9.6 , minimum stage number as 20, theoretical stage number as

47 and actual number of stage found as 59.

On basic and chemcad program we found same minimum reflux as about 9.6, but the number

of minimum and theoretical stages we have very little error but it can negliable. It’s reason

maybe our calculation has mistake a little.

The condensers and reboilers are placed on two different platforms where condensers are on

higher level than reboilers. The reason of this arrangement is to save place. In order to transfer

the feed to the system and also, in order to transmit the exit stream from the condenser to the

column as a reflux, pumps are used. The reflux pump is placed near reboiler to decrease pump

power and as a result energy cost.

We used two pumps for column, one of them for partial condenser and one of them for partial

reboiler. But we have seen that after calculation, for partial reboiler the pump is not necessary.

Because it is gas phase and not need to use pump. Also after calculation the reboiler pump

power found as 0.04 kW, it shows if there is no pump for reboiler, system can keep working.

Any other reason; the power of reflux pump is higher than reboilers’ pump as a result of

higher difference between heights of condensers and reflux pump in second column.

For reboiler we used lower pressure steam, which is 3 bar 133 oC. It was enough for our

system and if we use higher pressure steam the utility cost will find bigger. It shows steam

choosing is also important thing for distillation system.

Also steam production is important for cost of steam. On Turkey, steam production from coal

is cheaper than steam production from natural gas. Steam which by produced from coal cost is

40 TL/ton and from natural gas steam cost is 50 TL/ton. So we choosed steam for system

which is produced from coal.

304 stainless steel is chosen as the material of construction, because for long service life and

protect material from corrosion, these type of materials are using distillation system.

61  

About plate, we used sieve type plate, because it’s efficiency is higher than other type of

plates, it is simple to produce and usefull for these type of distillation columns.

Around the distillation column there should be manholes which are used when there is need

for cleaning the plates or when there is a need for unexpected situation in the system and also,

the ladder is used to climb to the column and used to reach to the manholes.

After all calculations for Rd/Rd, min 1.1, we done economical calculations. We found total

direct cost as 3,689,909 TL, total indirect cost as 2,213,586 TL, fixed charges as 423,041

TL/yr, operating cost as 2,029,218 TL/yr, and finally total annual cost as 2,452,589 TL/yr for

Turkey. For U.S.A. we found operating cost as 1,019,030 TL/yr and total annual cost as

1,442,001 TL/yr because of steam cost.

62  

7. CONCLUSION

In this project, the distillation column is designed to get pure product of ethanol and acetone

about 99%.

After economic analysis, following datas found;

Purchased Equipment Cost: 1,639,666 TL

Direct Cost: 3,689,909 TL

Indirect Cost: 2,213,586 TL

Fixed Cost: 423,041 TL/yr

For Turkey;

Operating Cost: 2,029,218 TL/yr

Total Annual Cost: 2,452,589 TL/yr

For U.S.A.;

Operating Cost: 1,019,030 TL/yr

Total Annual Cost: 1,442,001 TL/yr

This project is acceptable to purification of ethanol, acetone and n- buthanol. These

components using and market is increasing day to day. So it will make profit.

63  

8. SYMBOLS

A,B,C : Antoine constants

At : Cross sectional area of column ,m2

B: Mass flow rate of bottom product, kmol/ h

c: corrosion allowance, mm

Cp : specific heat, kj/ kg K

dc: Column diameter, m

d h : Hole diameter, m

D: Mass flow rate of distillate product, kmol/ h

E0 : Efficiency of column

f: Material’s max. working stress

F: Mass flow rate of feed, kmol/ h

F*: Design parameter

FLV: Flow parameter

hW: Height of water on tray ,m

HK: heavy key

IR: Plate spacing in column

KF: Capacity paramater

LM: Mass of liquid

LK: Light key

N: Number of plates

N,act: number of actual tray

P: Maximum allowable pressure, Mpa

64  

Po: Partial pressure of each component, mmHg

PT: Total pressure, mmHg

q: Heat load, j/s

Q: Volumetric flow rate of vapor, m3/s

RD: Reflux ratio

RDmin: Minimum reflux ratio

T: Temperature, K

t: Shell thickness,m

U: Overall heat transfer coefficient, W/ m2 K

u: Actual vapor velocity, m/s

uF: Floading velocity,m/s

VM : Mass of vapor

yi : Mol fraction of each component in vapor

ZT: Height of column, m

α: Relative volalitiy

XiF: Mol fraction of each component in feed

xi: Mol fraction of each component in liquid

ΔP: Pressure drop, mmHg

μ: Viscosity, mPa.s or kg/m.s

ρV: Density of vapor, kg/m3

ρL: Density of liquid, kg/ m3

λ: Latent heat, kJ/gmol

65  

9. REFERENCES

[1] http://bioacetone.com (28.12.2013)

[2] http://www.esru.strath.ac.uk/EandE/Web_sites/02-03/biofuels/what_bioethanol.htm

(28.12.2013)

[3] http://www.biobutanol.com (28.12.2013)

[4] Cheremisinoff, N., P., “Handbook of Chemical Processing Equipment”, 1st ed.,

Butterworth-Heinemann Publications, WoBurn, USA, 2000.

[5] Walas, S.M., “Chemical Process Equipment - Selection and Design”, 1st ed., Butterworth-

Heinemann publications, Reed Publishing USA, 1990

[6] Sinnott, R.K., Coulson & Richardson’s Chemical Engineering Design, Volume 6, 4th

Edition, Elsevier Inc., 2005

[7] Uysal B.Z., ‘Akışkanlar Mekaniği’, Alp Yayınevi, 2. Baskı, Ankara, 2006

[8] Peters M.S., Timmerhaus K.D., West R.E.,’Plant Design and Economics for Chemical

Engineers’, University of Colorado, fifth edition, New York, 2002

[9] http://www.engineeringtoolbox.com/saturated-steam-properties-d_457.html (28.12.2013)

[10] Ethanol MSDS

[11] Water MSDS

[12] Acetone MSDS

66  

APPENDICES

67  

APPENDIX-A: PHYSIOCHEMICAL PROPERTIES OF COMPONENTS

Table 3. Properties of Ethanol [10]

Properties of Ethanol at 20°C

Molecular Weight (g/mol) 46.0414

Viscosity (kg/ms) 0.0012

Boiling Point (° C ) 78

Freezing/Melting Point (° C ) -114.1

Density (kg/m3) 0.790

Solubility Miscible

Table 4. Properties of Water [11]

Properties of Water at 20°C

Molecular Weight (g/mol) 18.02

Viscosity (kg/ms) 0.001002

Boiling Point (° C ) 100

Freezing/Melting Point (° C ) 0

Density (kg/m3) 1.00

Table 5. Properties of Acetone [12]

Properties of Acetone at 20°C

Molecular Weight (g/mol) 58.08

Viscosity (mPa.s) 0.32

Boiling Point (° C ) 56.2°C

Freezing/Melting Point (° C ) -95.35

Density (kg/m3) 0.79

Solubility Easily soluble in cold water, hot water.

Table 6. Antoine Constans for Each Components [7]

Antoine Constants, T in K and P in mmHg A B C Acetone 16,6513 2940,46 -35,93 Ethanol 18,9119 3803,98 -41,68 Water 18,3036 3816,44 -46,13

68  

Table 7. Saturated Steam Properties [9]

Absolute pressure 

Boiling point  Specific volume (steam)  Density (steam) Specific enthalpy of liquid water 

(sensible heat) Specific enthalpy of steam

(total heat) Latent heat of evaporization  Specific heat 

(bar)  (oC)  (m3/kg)  (kg/m3)  (kJ/kg)  (kcal/kg)  (kJ/kg)  (kcal/kg)  (kJ/kg)  (kcal/kg)  (kJ/kg K) 

1  99.63  1.694 0.590 417.51 99.72 2675.43 639.02 2257.92 539.30 2.0267 

1.2  104.81  1.428 0.700 439.36 104.94 2683.44 640.93 2244.08 535.99 2.0476 

1.4  109.32  1.236 0.809 458.42 109.49 2690.28 642.56 2231.86 533.07 2.0673 

1.5  111.37  1.159 0.863 467.13 111.57 2693.36 643.30 2226.23 531.73 2.0768 

1.6  113.32  1.091 0.916 475.38 113.54 2696.25 643.99 2220.87 530.45 2.0860 

1.7  115.17  1.031 0.970 483.22 115.42 2698.97 644.64 2215.75 529.22 2.0950 

1.8  116.93  0.977 1.023 490.70 117.20 2701.54 645.25 2210.84 528.05 2.1037 

1.9  118.62  0.929 1.076 497.85 118.91 2703.98 645.83 2206.13 526.92 2.1124 

2  120.23  0.885 1.129 504.71 120.55 2706.29 646.39 2201.59 525.84 2.1208 

2.2  123.27  0.810 1.235 517.63 123.63 2710.60 647.42 2192.98 523.78 2.1372 

2.4  126.09  0.746 1.340 529.64 126.50 2714.55 648.36 2184.91 521.86 2.1531 

2.6  128.73  0.693 1.444 540.88 129.19 2718.17 649.22 2177.30 520.04 2.1685 

2.8  131.20  0.646 1.548 551.45 131.71 2721.54 650.03 2170.08 518.32 2.1835 

3  133.54  0.606 1.651 561.44 134.10 2724.66 650.77 2163.22 516.68 2.1981 

3.5  138.87  0.524 1.908 584.28 139.55 2731.63 652.44 2147.35 512.89 2.2331 

4  143.63  0.462 2.163 604.68 144.43 2737.63 653.87 2132.95 509.45 2.2664 

4.5  147.92  0.414 2.417 623.17 148.84 2742.88 655.13 2119.71 506.29 2.2983 

5  151.85  0.375 2.669 640.12 152.89 2747.54 656.24 2107.42 503.35 2.3289 

5.5  155.47  0.342 2.920 655.81 156.64 2751.70 657.23 2095.90 500.60 2.3585 

6  158.84  0.315 3.170 670.43 160.13 2755.46 658.13 2085.03 498.00 2.3873 

6.5  161.99  0.292 3.419 684.14 163.40 2758.87 658.94 2074.73 495.54 2.4152 

7  164.96  0.273 3.667 697.07 166.49 2761.98 659.69 2064.92 493.20 2.4424 

7.5  167.76  0.255 3.915 709.30 169.41 2764.84 660.37 2055.53 490.96 2.4690 

8  170.42  0.240 4.162 720.94 172.19 2767.46 661.00 2046.53 488.80 2.4951 

8.5  172.94  0.227 4.409 732.03 174.84 2769.89 661.58 2037.86 486.73 2.5206 

9  175.36  0.215 4.655 742.64 177.38 2772.13 662.11 2029.49 484.74 2.5456 

9.5  177.67  0.204 4.901 752.82 179.81 2774.22 662.61 2021.40 482.80 2.5702 

10  179.88  0.194 5.147 762.60 182.14 2776.16 663.07 2013.56 480.93 2.5944 

30  233.84  0.067 15.009 1008.33 240.84 2802.27 669.31 1793.94 428.48 3.4069 

 

APPEN 

Figure

Figure

NDIX-B: FI

11: Capacit

12: Purchas

IGURES W

ty of Entrain

sed Cost of

WHICH AR

nment Diag

Fixed-Tube

RE USED O

gram [7]

e-Sheet Hea