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Manufacture of Methyl Ethyl Ketone form

Secondary Butyl Alcohol

PROJECT REPORT

Name : Dilip Kumar Verma

Roll number : 11/S-11/535

Registration Number : S/111/15/21

Title of the problem : Design a plant to produce 5000 tons per annum Methyl ethyl

ketone using Secondary butyl alcohol

INDIAN INSTITUTE OF CHEMICAL ENGINEERS


KOLKATA-700032.INDIA

1
Manufacture of Methyl Ethyl Ketone form
Secondary Butyl Alcohol

PROJECT REPORT

Name : Dilip Kumar Verma

Roll number : 11/S-11/535

Registration Number : S/111/15/21

Title of the problem : Design a plant to produce 5000 tons per annum Methyl ethyl

ketone using Secondary butyl alcohol

INDIAN INSTITUTE OF CHEMICAL ENGINEERS


KOLKATA-700032.INDIA

2
INDIAN INSTITUTE OF CHEMICAL ENGINEERS
Jadavpur University Campus, Kolkata - 700032.INDIA

BONAFIDE CERTIFICATE
This is certify that dissertation of the project work (MEK).

MANUFACTURE OF METHYLE ETHYEL KYTONE

Submitted by…………………………………………………………is aRecord of


bona fide work carried out by him, as a partial fulfillment of theRequirements for
the award of the degree of Bachelor of Technology in Chemical engineering of
Indian institute of chemical engineers, Kolkata.

……………………. …………………………….
Membership.Head of Department.

Place. Kolkata
Date:
Certified that the candidate ………………………………………………….was
Examined by us in the PROJECT WORK and VIVA VOCE examination held
On……………………

……………………. …………………...
Internal Examiner External Examiner

3
ABSTRACT

Thus the project based on manufacturing of MEK 5000 tons per year includes.
1. Material balance

2. Energy balance

3. Factor for selecting the process

4. Design of equipment such as

a) Condenser

b) Absorption

5. Cost estimation
In carrying out this project we applied
a) Chemical process calculation

b) Process equipment and design concepts

c) Application of heat and mass balance principle

d) Economic
Thus the project covers all aspects required for the manufacturing of MEK and
Could be implemented in reality.

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Contents
Manufacture of Methyl Ethyl Ketone form Secondary Butyl Alcohol ......................................................... 1
PROJECT REPORT ..................................................................................................................................... 1
Manufacture of Methyl Ethyl Ketone form Secondary Butyl Alcohol ......................................................... 2
PROJECT REPORT ..................................................................................................................................... 2
ABSTRACT ..................................................................................................................................................... 4
NOMENCULTURE ..................................................................................................................................... 7
INTRODUCTION ........................................................................................................................................ 9
METHYL ETHYL KETONE:- ................................................................................................................ 9
PHYSICAL AND CHEMICAL PROPERTIES OF MEK ......................................................................... 11
PHYSICAL PROPERTIES:- .................................................................................................................. 11
CHEMICAL PROPERTIES:-................................................................................................................. 13
Miscellaneous Reactions......................................................................................................................... 13
USES:- .................................................................................................................................................... 15
ECONOMIC ASPECT:- ......................................................................................................................... 15
TOXICOLOGY: ......................................................................................................................................... 17
PROCESS SELECTION AND DETAILS ................................................................................................. 18
PROCESSES MANUFACTURING METHODS .................................................................................. 18
PROCESS SELECTION ........................................................................................................................ 18
PROCESS DESCRIPTION .................................................................................................................... 19
RAW MATERIAL REQUIRMENT ...................................................................................................... 20
Major raw materials required:................................................................................................................. 20
VAPOR PHASE DEHYDROGENTAION OF 2-BUTANOL: ............................................................. 21
LIQUID PHASE OXIDATION OF BUTANE: ..................................................................................... 22
DIRECT OXIDATION OF N-BUTENES, HOECHST-WACKER PROCESS: ................................... 22
DIRECT OXIDATION N-BUTENES, MARUZEN PROCESS: .......................................................... 23
PROCESS SELECTION: ....................................................................................................................... 23
MATERIAL BALANCE ............................................................................................................................ 26
BASIS: .................................................................................................................................................... 26
REACTOR.............................................................................................................................................. 26
CONDENSER ........................................................................................................................................ 28
SEPARATOR ......................................................................................................................................... 28
ABSORBER ........................................................................................................................................... 29
MEK balance: ......................................................................................................................................... 29
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EXTRACTOR ........................................................................................................................................ 31
MEK PRODUCT DISTILLATION COLUMN ..................................................................................... 32
Material balance.......................................................................................................................................... 34
REACTOR.............................................................................................................................................. 34
CONDENSER ........................................................................................................................................ 35
SEPARATOR ......................................................................................................................................... 36
ABSORBER ........................................................................................................................................... 36
EXTRACTOR ........................................................................................................................................ 37
SOLVENT RECOVERY DISTILLATION COLUMN ......................................................................... 37
MEK PRODUCT DISTILLATION COLUMN ..................................................................................... 38
ENERGY BALANCE ............................................................................................................................ 39
PIPING AND INSTRUMENTATION ....................................................................................................... 79
AUTOMATION CONTROL: ................................................................................................................ 79
FLOW CONTROL: ................................................................................................................................ 79
INSTRUMENTATION AND CONTROL OBJECTIVES: ................................................................... 79
TERMINOLOGY ................................................................................................................................... 83
PROPERTIES ......................................................................................................................................... 83
Physical Properties.................................................................................................................................. 83
Chemical Properties ................................................................................................................................ 84
HEALTH EFFECTS AND TOXICITY INFORMATION ........................................................................ 85
General.................................................................................................................................................... 85
PERSONAL PROTECTIVE EQUIPMENT .......................................................................................... 85
STORAGE, HANDLING, LABELLING AND TRANSPORTATION .................................................... 86
Labelling .............................................................................................................................................. 86
Waste Disposal ........................................................................................................................................... 87
FIRE PREVENTION AND FIRE FIGHTING........................................................................................... 87
TRAINING AND HEALTH MONITORING ............................................................................................ 88
FIRST AID ............................................................................................................................................. 88
CONCLUSION........................................................................................................................................... 89

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NOMENCULTURE

Cp = Specific heat, kJ/kg K


Hr = Heat of formation, kJ/mole
m = Mass flow rate, kg/hr
λ = Latent heat of vaporization, kJ/kg
De= Equivalent Diameter, m
U = Overall Heat transfer coefficient, W/m2K
LMTD = Log mean temperature difference,°C
(∆T)ln = True mean temperature difference,°C
ρ =Density, kg/m3
µ = Viscosity, kg/m.sec
K = Thermal conductivity, W/m K
h = Heat transfer coefficient, W/m2K
Nnu = Nusselt number
NRe = Reynolds number
NPr = Prandlt Number
Uc = Clean overall coefficient, W/m2K
C = Corrosion allowance, m
Rc = Crown Radius, m
R1 = Knuckle Radius, m
ya = Gasket seating stress, kgf/m2
Am = Area of the bolt, m2
Wm = Weight of material, kg
Wi = Weight of insulating material, kg
Wt = Total weight, kg
HTU = Height Transfer Unit, m
NTU = Number of Transfer Unit
Np = Number if theoretical plates
7
A = Absorption factor
G = Mass velocity, kg/hr.m2
αAB = Relative volatility
Rm = Reflux Ratio
V = Vapor flow rate, m3/sec
L = Liquid flow rate, m3/sec
Unf = Flooding velocity, m/sec

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INTRODUCTION

Methyl ethyl alcohol, also known as 2-butanone is a colorless organic liquid with an acetone like

odor and a low boiling point. It has very good solvent properties, a fast evaporation rate, and is

miscible with organic Solvents. MEK is an excellent solvent for a variety of resin systems used

in the preparation of paints and lacquers.

The molecular formula of methyl ethyl ketone is CH3COCH2CH3 and its molecular structure is

represented as:

METHYL ETHYL KETONE:-

Ketones are organic compounds containing one or more carbonyl groups bound to two carbon

atoms and are represented by the general formula:

R --- CO --- R’

Based on the hydrocarbon ( R , R’ ) groups attached to the carbonyl group, ketones can be

classified. MEK has the molecular structure: CH3 – CO – C2H5.It is asymmetric or mixed

aliphatic ketone. It’s IUPAC name is 2-butanone.

2-Butanone ,methyl ethyl ketone, MEK, is the 2nd link in the homologous series ofaliphatic

ketones and next to acetone, the most important commercially produced ketone.It is

commercially produced by dehydrogenation of the secondary butyl alcohol. It isanalogus to the

production of actone by dehydrogenation of isopropyl alcohol on copperor zinc or bronze

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catalyst at 400 – 5000C. At 80-95% sec butylalcohol conversion, MEKselectivity is greater than

95%. Butenes (dehydration) and higher ketones (auto condensation) are the by-products.Methyl

Ethyl Ketone (MEK) is a low –boiling, chemically stable compound also knownas 2- butanone.

MEK is a flammable, colourless liquid possessing a typical ketonic odor.It has very good solvent

properties, a fast evaporation rate, and is miscible with organic solvents. MEK is an excellent

solvent for a variety of resin systems used in thePreparation of paints and lacquers.Interest in

MEK as a solvent for paints and adhesives has been growing in recentyears. It has broad

applications as solvent for nitrocellulose, cellulose acetatebutyrate,ethylcellulose, acrylic resins,

vinyl acetate and vinyl chloride – vinyl acetate copolymers.Moreover, MEK can be used as an

activator for oxidative reactions, as a selectiveextractant, as a special solvent for dewaxing

mineral oil fractions and as a chemicalintermediate.

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PHYSICAL AND CHEMICAL PROPERTIES OF MEK

PHYSICAL PROPERTIES:-

MEK is a low boiling solvent with an atmospheric boiling point of 175.3 0F

(79.60C). Methyl Ethyl Ketone (MEK) is a chemically stable compound also known as 2-

butanone. MEK is a flammable, colourless liquid possessing a typical ketonic odor. It hasvery

good solvent properties, a fast evaporation rate, and is miscible with organicsolvents. MEK is an

excellent solvent for a variety of resin systems used in thepreparation of paints and lacquers. It is

highly miscible with water and manyconventional organic solvents and forms azeotrope with

number of organic solvents.

Some of the physical properties are listed below:

1. Physical Properties of MEK (all values are at 200C, except where noted)

2. Boiling point at 1 atm, 0C …………………………………………………………..79.6

3. Azeotrope with water , bp, 0C ………………………………………………………73.4

4. Wt.% ketone in vapor……………………………………………………………….. 88.7

5. Autoignition temperature, 0C………………………………………………….…… 515.6

6. Coefficient of cubic expansion, per 0C …………………………………………...0.00119

7. Critical pressure, atm ……………………………………………………………………43

8. Critical temperature , 0C ……………………………………………………….………260

9. Density, g/mL at 200C……………………………………………………………... 0.8037

10. Dielectric constant …………………………………………………………………...18.51

11. Dipole moment, debye units………………………………………………………….. 2.74


12.
Electrical conductivity, mho…………………………………………………….. 5.0 x 10-8

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13. Explosive limits in air, vol.%

14. Upper ……………………………………………………………………………………10

15. Lower …………………………………………………………………………………...1.8

16. Flash point, 0C

17. Tag open Cup ………………………………………………………………………….1.11

18. Tag Closed Cup……………………………………………………………………… -2.22

19. Freezing point, 0C……………………………………………………………………. -86.3

20. Heat of combustion, cal/g……………………………………………………………. 8084

21. Heat of fusion, cal/g …………………………………………………………………...24.7

22. Heat of vaporization, cal/g ……………………………………………………………..106

23. Molecular weight ………………………………………………...…………………72.104

24. Refractive index nD……………………………………………….………………..1.3791

25. Solubility, wt. %

26. Ketone in water ………………………………………………………………………26.3

27. Water in ketone ………………………………………………………………………11.8

28. Solubility parameter ……………………………………………………………………9.3

29. Specific heat, cal/g 0C……………………………………………………………….. 0.549

30. Surface tension, dyn/cm ……………………………………………………………….24.6

31. Thermal conductivity, cal/cm2 .s. (0C/cm) …………………………………….3.58 x 10-4

32. Vapor pressure, mmHg ………………………………………………………………80.21

33. Viscosity, cP…………………………………………………………………………0.43

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CHEMICAL PROPERTIES:-

Methyl Ethyl ketone can be widely utilized in chemical synthesis. Its reactivity

centers around the carbonyl group and its adjacent hydrogen atoms. Condensation,

ammonolysis, halogenations, and oxidation can be carried out under the proper

conditions. Some typical reactions are described below.

Self-Condensation:

Aldol condensation of 2 moles of MEK yields a hydroxy ketone, which readilydehydrates to an

unsaturated ketone:

O CH3 O

2CH3CCH2CH3 CH3CH2CCH3CCH2CH3

CH3 O

CH3CH2C==CHCCH2CH3+H2O

Condensation with other Compounds:

Reaction with aldehydes gives higher ketones, as well as ketals and cyclic compounds,depending

on reaction conditions. β - ii ketones are produced by the condensation ofMEK with aliphatic

esters. MEK condenses with glycols and organic oxides to givederivatives of dioxolane. sec-

Butyl amine is formed by reacting MEK with aqueousammonia and hydrogen:

O Ni NH2

CH3CCH2CH3+NH3+H2 CH3CHCH2CH3+H2O

An excess of MEK in this reaction will produce di-sec-butylamine.Reacting MEK with acetylene

gives methyl pentynol, a hypnotic compound:…...,O CH3

CH3CCH2+HC CH CH3CH2CCOH CH

Miscellaneous Reactions

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Oxidation of MEK with oxygen produces diacetyl, a flavouring material. Chlorinationyields

mixtures of several monochloro and dichloro derivatives in various percentagesdepending on

reaction conditions. The reaction of MEK with hydrogen peroxide gives amixture of peroxides

and hydro peroxides which is used to cure polyester resins at roomtemperature:

O OH

CH3CCH2CH3 + H2O2 CH3CCH2CH3

OOH

This initial addition product is the unstable precursor of seven stable peroxides andhydro

peroxides. Of these, 2,2 –dihydroperoxy-2,2’-dibutyl peroxide is present in thelargest amount

(about 45%) in the peroxide mixture: CH3 CH3

HOOC – OO – COOH

C2H5 C2H5

MEK peroxides are widely used as catalysts for the polymerisation of polyesterresins at room

temperature. The condensation product of MEK and m-phenyl diamine isan efficient curing

agent for epoxy resins. MEK and cobalt acetate function together as aspecific catalyst for single-

stage oxidation of p-xylene to terephthalic acid. Aliphaticmonoketones, such as MEK also

function as catalysts in the polymerisation ofpolyethylene terephthalate where, it is claimed, they

speed condensation times and causeless yellowing of the polymer than antimony trioxide. MEK

is also used in thepreparation of complex catalysts used in the syndiotacicpolymerisation of α-

olefinssuch as propylene.Phenol, glyoxal, formaldehyde, acetaldehyde, furfuraldehyde, and other

chemicalscan be reacted with MEK to form resins useful for adhesives, coatings, molded

products,and electrical insulation. MEK reacts with acrylonitrile to produce a dinitrile, which

uponhydrogenation produces amines.

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USES:-

More than half the MEK produced in the United States finds application insurface coatings end

uses. Significant volumes are also used in the production ofadhesives, magnetic tapes, printing

inks, solvent extraction, cleaning fluids, dewaxingagents, and dyes.In surface coatings MEK is

widely used as a component in vinyl lacquer solventsystems. Its active solvency for vinyl acetate

and vinyl chloride – vinyl acetatecopolymers makes it possible to formulate high solids lacquers

containing large amountsof economical hydrocarbon diluents. In addition, it is a strong, active

solvent fornitrocellulose and is extensively used in furniture and automotive lacquers. The

lowspecific gravity of MEK enables formulators to produce larger volumes of base lacquersor

thinners per pound than is possible with heavier solvents. MEK is also a coatingssolvent for

many resin systems including alkyds and air-dried epoxies. It performs extremely well in fast

drying traffic paints and has become an important component inplacing air pollution regulated

solvents, such as toluene, which are frequently used inthese alkyd formulations.

MEK is a dewaxing agent in the refining of lubricating oils and is asolvent for adhesives, rubber,

cement, printing inks, paint removers and cleaningsolutions. It is used in vegetable oil extraction

process and in azeotropicseparation schemes in refinery.

ECONOMIC ASPECT:-

Demand for MEK has increased at a rate of 6.5% per year and is continued to grow

at about this rate in future. Apparently the long term decrease in demand owing to

increase in solventless coatings has not materialized .

The percentage sales distribution for MEK is as follows :

Paints, lacquers, printing inks, aluminium foils – 40%.

Coating and printing of plastics – 20%

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Chemical industry, pharmaceutical industry – 13%

Adhesives – 11%

Miscellaneous – 16%

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TOXICOLOGY:

The inhalation of MEK vapours has narcotic effects. The vapour irritates the eyes

and the nasal and pharyngeal membranes. Frequent and prolonged contact with MEKcauses skin

moisture loss and slight irritation .Sensitive persons may develop demitasses.Liquid MEK

temporarily irritates eyes and corneas .MEK is usually absorbed throughthe respiratory track. It

may also be absorbed through the skin.The odour threshold for MEK is 10 ppm .

Toxic concentration for water organisms :Average lethal concentration for fish – 5600 mg / lit

Maximum permissible concentration for pseudomonas putida – 1150 mg / lit

Maximum permissible concentration for scendesmusquadricanda – 120 mg / lit

Maximum permissible concentration for small crabs -- 2500 mg / lit

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PROCESS SELECTION AND DETAILS

PROCESSES MANUFACTURING METHODS

There are a few processes listed below for the production of MEK.

1. Vapour phase dehydrogenation of 2- Butanol.

2. Liquid phase oxidation of n-Butane.

3. Direct oxidation of n-Butanes, Hoechst-Wacker process.

4. Direct oxidation of n-Butanes, Maruzen process

PROCESS SELECTION

The vapour phase dehydrogenation process gives high conversion of 2-butanol and high

selectivity of MEK of about 95 mole%. Other advantages of this process include better yield,

longer catalyst life, simple production separation and lower energy consumption.In

dehydrogenation process, hydrogen as a by product is obtained that can be used as a furnace

fuel.In dehydrogenation process, there is the feasibility of separating the MEK from the reaction

products.The dehydrogenation process can easily be carried out at moderate temperature and at

atmospheric pressure.In dehydrogenation process, 90% of MEK can easily be converted to

MEK.Selective oxidation process requires controlled conditions so it becomes

uneconomical.Chromic acid and sulphuric acid in aqueous acetone is required for selective

oxidation of butanol while only brass is required for dehydrogenation of butanol.

Of all the processes, it has been found that “dehydrogenation of secondary butyl alcohol” has

more advantages and is more economical compared to other processes, so this process has been

selected for plant design.

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PROCESS DESCRIPTION

The cold feed of secondary butyl alcohol from feed tank is initially preheated in steam heater.

The preheated alcohol is taken to vaporizer and further superheated by the high temperature

reaction products discharged from reactor and gets vaporized. The alcohol vapors leaving from

vaporizer enter into a knockout drum to separate liquid alcohol and vapors entrained liquid. The

separated liquid is recycled back to vaporizer. The dry vapors of secondary butyl alcohol leaving

from the knockout drum are heated up to 500°C in super heaters and enter the reactor containing

catalytic bed of Zinc oxide.

In reactor, temperature is maintained between 400-550°C at which secondary butyl alcohol starts

dehydrated and produce methyl ethyl ketone and hydrogen. 90% of the feed is converted into

methyl ethyl ketone.The dehydrogenation reaction of SBA is as shown

ZnO

CH3CH2-CHOH-CH3 CH3CH2-CO-CH3 + H2

The dehydrogenation reaction is endothermic and reversible; therefore a considerable amount of

heat is to be supplied. Hence, a multi-tube reactor is selected. In order to utilize the heat energy

and lower the temperature of the gaseous reaction products (contain MEK, unreacted secondary

butyl alcohol vapors and hydrogen); it is routed to vaporizer to preheat the feed. The reaction

products are then cooled in condenser. 80-85% of MEK and the unreacted secondary butyl

alcohol vapors get condensed in condenser. Outlet from condenser is taken to a separator where

liquid and gas get separated.The uncondensed vapors and non-condensable hydrogen from the

separator is taken to absorption column to separate hydrogen from the alcohol vapors. In

absorption column, aqueous ethanol is used as absorbent. Around 98% of MEK and secondary

19
butyl alcohol vapors are absorbed in aqueous ethanol. The hydrogen off gas from the top of the

absorber is dried and used as furnace fuel.

The aqueous solution contains MEK and secondary butyl alcohol from the absorber is pumped

into an extraction column where 95% of MEK and alcohol is extracted into trichloroethane

(TCE). The raffinate is recycled back to absorber and the extract is passed to solvent recovery

distillation column. In solvent recovery distillation column, 99.9% MEK and alcohol are

separated from the solvent asdistillate and the residue containing TCE and traces of MEK and

alcohol are recycled back to extraction column.

The distillate from solvent recovery distillation column and the condensed MEK from condenser

are taken to product distillation column where the final purification occurs. In distillation

column, 99.9% pure methyl ethyl ketone is distilled as final product. The product MEK is cooled

and stored in product storage tank. The residue from distillation column bottom is mainly

contains unreacted secondary butyl alcohol which is recycled back to feed storage tank.

RAW MATERIAL REQUIRMENT

Plant capacity: 5000 tons Methyl ethyl ketone (99.9%) per annum

To produce 5000 tons per annum methyl ethyl ketone, the required secondary butyl alcohol is

5860 tons per annum (90% Conversion is considered)

Major raw materials required:

1. Secondary butyl alcohol

2. Trichloroethane

3. Aqueous ethanol

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4. Utilities:

5. Cooling water

6. Steam

7. Flue gas

There are a few processes listed below for the production of MEK.

1) Vapor phase dehydrogenation of 2- Butanol.

2) Liquid phase oxidation of n-Butane.

3) Direct oxidation of n-Butanes, Hoechst-Wacker process.

4) Direct oxidation of n-Butanes, Maruzen process.

VAPOR PHASE DEHYDROGENTAION OF 2-BUTANOL:

MEK is prepared by vapor phase dehydrogenation of 2-butanol. A 2 step process from butanes,

which are first hydrated to give 2-butanol, is used. The dehydrogenation of2-butanol is an

exothermic reaction (51 KJ/Kgmol). The reaction is as follows.

CH3OHCHCH3 CH3 –COC2H5

The equilibrium constant for 2-butanol cab be calculated as follows:

logKp = -2790/T + 1.51 *log T + 1.856

Where T = reaction temperature, K

Kp= equilibrium constant, bar.

The MEK concentration in the reaction mixture increases and reaches its maximum

atapproximately 3500C. Copper, Zinc or Bronze are used as catalysts in gas

phasedehydrogenation. Commercially used catalysts are reactivated by oxidation, after 3 to

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6months use. They have a life expectance of several years.Sec-butyl alcohol is dehydrogenated

in a multiple tube reactor, the reaction heatbeing supplied by heat transfer oil. The reaction

products leave the reactor as gas and aresplit into crude MEK and hydrogen on cooling. The

hydrogen is purified by furthercooling. The crude MEK is separated from uncreated reactants

and by-products bydistillation.

LIQUID PHASE OXIDATION OF BUTANE:

MEK is produced as a by-product in the liquid phase oxidation of n-butane toacetic acid.

Autoxidation of n-butane of n-butane takes place in the liquid phaseaccording to the radical

mechanism yielding MEK as an intermediate and acetic acid asend product. MEK and acetic

acid (mass ratio 0.2: 1.0) are obtained by non-catalyzedliquid phase oxidation at 1800C and 53

bars with remixing. Continuous oxidation underplug flow conditions at 1500C, 65 bars and a

residence time of 2- 7 minutes forms MEKand acetic acid at a mass ratio of 3:1. this process has

slight economic advantage over thedehydrogenation of 2-butanol. But the key factor is

availability and price of butane.

DIRECT OXIDATION OF N-BUTENES, HOECHST-WACKER PROCESS:

In direct oxidation of n-butanes by Hoechst-wacker process, oxygen istransferred in a

homogenous phase on to n-butanes using redox salt pair, PdCl2 / CuCl2.

n – C4 H8 + ½ O2 CH3 – CO – C2H5

95% conversion of n-butanes can be obtained with the MEK selectivity of about 86%.The main

disadvantage of this product is the formation of chlorinated butanones and bbutryaldehydeand

corrosion caused due to free acids.

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DIRECT OXIDATION N-BUTENES, MARUZEN PROCESS:

The Maruzen process is similar to the Hoechst-Wacker process except thatoxygen is transferred

by an aqueous solution of palladium sulfate and ferric sulfate. Thismethod is attractive

commercial route to get MEK via direct oxidation of n-butenes, but itis patented and very less

information is available about this process. This process isgenerally not accepted due to

formation of undesirable by products.

PROCESS SELECTION:

Commercially, MEK is predominantly produced by the catalytic dehydrogenation of SBA in

vapor phase over ZnO or Brass catalyst. It can, however be produced by theselective direct

oxidation of the olefin in a variety of processes, including the Hoechst-Wacker-type process

employing a palladium(II) catalyst.Most MEK (88%) is produced today by dehydrogenation of

2-butanol. 2-butanolcan be easily produced by the hydration of n-butenes(from petrochemically

produced C4raffinates). The remaining MEK is produced by process in which liquid butane

iscatalytically cracked giving both acetic acid and MEK.The vapor phase dehydrogenation

process gives high conversion of 2-butanol andhigh selectivity of MEK of about 95 mole%.

Other advantages of this process includebetter yield, longer catalyst life, simple production

separation and lower energyconsumption.

MEK is produced as by product from liquid phase oxidation of n-butenes toacetic acid. The

process has slight economic advantage over dehydrogenation of 2-butanol, but the key factor is

the availability and price of n-butanes.Of all the processes, it has been found that

dehydrogenation of 2-butabol has moreadvantages and is more economical compared to other

processes, so this process has beenselected for design in following text.

23
PROCESS DETAILS:

The cold feed of 2-butanol will be pumped from the feed tank to a steam heaterto a vertical

thermosyphon vaporizer in which alcohol is vaporized. The thermosyphonvaporizer will be

heated by reaction products discharged from the reactor. The wetalcohol vapor will be passed to

a knock out drum to remove any entrained liquid. Theliquid separated will be recycled and the

dry alcohol will be fed to the reactor via superheaters heated by flue gas. The super heaters will

be designed to raise the temperature of alcohol vapors to 5000C at which temperature the vapors

enter the reactor.The dehydrogenation reaction of SBA is as shown

OH

CH2 – CH – C2H5 H2C – CO – C2H5 + H2

The dehydrogenation reaction is endothermic and reversible and therefore aconsiderable amount

of heat is to be supplied and hence, a multi-tube reactor is selected.The gaseous reaction products

discharged from the reactor at a minimum of4000C will be passed on to the thermosyphon

vaporizer in order to initiate the preheatingof alcohol reactor feed. The reaction products will be

cooled to near saturation in thevaporizer so that they will enter the water condenser at 150 0C.

There about 80% MEKand alcohol will be condensed and sent to the storage while the remainder

will leave thisunit as saturated vapor in non-condensable hydrogen.

This vapor will be fed to the bottom of the packed bed absorption column whereMEK and 2-

butanol will be absorbed in water. The water will be recycled from theextraction column and its

rate will be controlled to provide an aqueous effluentcontaining 10% MEK. The hydrogen

discharged from the top of the absorber will bedried and fed to the furnace.The aqueous effluent

from the absorber will be pumped into an extraction columnwhere it will be contacted with

1,1,2-Trichlorethane to extract MEK and alcohol. Inexcess of about 95% of the MEK and

24
alcohol will be extracted and remainder will bere-circulated back to the absorber.The

trichloroethane extract phase will be pumped to a distillation unit for theseparation unit for the

separation of solvent, which is recycled. The distillate from thiscolumn will be MEK and

alcohol, which will be, mixed liquid product form thecondenser and this will be treated in a

MEK product still for the purification ofMEK. The alcohol discharged from the bottom of this

column will be replaced back toalcohol feed tank. The MEK product will be cooled and stored.

25
MATERIAL BALANCE

BASIS:

The required Secondary butyl alcohol is taken as “W”Kg per hr.

Name Molecular weight (Kg / kmole)

Secondary Butyl alcohol 74

Methyl ethyl ketone 72

Hydrogen 2

REACTOR

Stoichiometric reaction of dehydrogenation of secondary butyl alcohol is as follows,

C4H10O C4H8O + H2

(74 Kg/kmole) (72 Kg/kmole) (2 Kg/kmole)

Reaction Conversion = 90%

From the reaction,

74 kg of secondary butyl alcohol produces 72 kg of MEK and 2 kg of H2.

With 90% conversion, W kg/ hr of SBA produces,

= (72/74) ×0.9× W = 0.876W Kg/hr of MEK

= (2/74) × 0.9 × W = 0.0243W Kg/hr of H2

= 0.1W kg/hr of unreacted SBA

26
MEK = 0.876W (Kg/hr)

H2 = 0.0243W (Kg/hr)

Unreacted SBA = 0.1W (Kg/hr)

Reactor

Secondary butyl alcohol


W Kg/hr

27
CONDENSER

In condenser, 80% of methyl ethyl ketone and unreacted SBA getscondensed. Condenser outlet
is two phased flow- contains condensed liquid anduncondensed/non condensable vapors.

MEK = 0.876W (Kg/hr) Liquid Phase:


H2 = 0.0243W (Kg/hr) MEK = 0.7W (Kg/hr)
Unreacted SBA = 0.1W (Kg/hr) SBA = 0.08W (Kg/hr)

Vapor phase:

MEK = 0.176W (Kg/hr)

H2 = 0.0243W (Kg/hr)

SBA = 0.02W (Kg/hr)

SEPARATOR

The condensed liquid and uncondensed vapors get separated in separator. The separated vapor
goes to absorber and the liquid is taken to product distillation column.

Vapor phase:

MEK = 0.176W (Kg/hr)

H2 = 0.0243W (Kg/hr)
Liquid Phase:
SBA = 0.02W
MEK = 0.7W (Kg/hr)

SBA = 0.08W (Kg/hr)

Vapor phase:

MEK = 0.176W (Kg/hr)

H2 = 0.0243W (Kg/hr) Liquid Phase:

SBA = 0.02W MEK = 0.7W (Kg/hr)

SBA = 0.08W (Kg/hr)

28
ABSORBER

Aqueous ethanol is used as absorbent. 98% of MEK and SBA areabsorbed in absorption
column.The raffinate from the extraction column contain
ns 99.5 wt% ethanol and 0.5wt% MEK is recycled back to absorber.Recycleflow rate is
controlled to provide an aqueous solution containing 10% MEK at absorberbottom outlet.

Absorber bottom outlet = A Kg/hr


MEK in absorber outlet = 0.1A Kg/hr
Amount of absorbent = E Kg/hr

MEK = 0.0035W (Kg/hr)

H2 = 0.0243W (Kg/hr)

Absorbent (E):

Ethanol = 99.5%

MEK = 0.176W (Kg/hr) MEK =0.5%

H2 = 0.0243W (Kg/hr) = 0.005E

SBA = 0.02W(Kg/hr)

MEK = 0.1805W (Kg/hr)

SBA = 0.02W (Kg/hr)

Ethanol = 1.606W (Kg/hr)


MEK balance:

MEK in = MEK out


0.176W+0.005E = 0.0035W + 0.1A
Solving for A,
A = 1.725W + 0.05E --------------------------- (1)
Overall balance:
29
0.176W + 0.0243W + 0.02W + E = 1.725W + 0.05E +0.0035W +0.0243W
Solving for E,
E = 1.614W ----------------------------- (2)
Amount of MEK in absorbent = 0.005×1.614W
= 0.0081W
Amount of ethanol in absorbent = 0.995×1.614W
= 1.606W

Using (2) in equation (1),


Absorber bottom solution, A = 1.805W

Absorber bottom solution contains,


MEK = 0.1805W
Ethanol = 1.606W
SBA = 0.02W

30
EXTRACTOR

In extraction column, trichloroethane is used to extract MEK and alcohol from the absorbent.

95% of the MEK and alcohol is extracted and remainder isrecirculated back to the absorber.

Trichloroethane
T (kg/hr)

MEK = 0.1805W (Kg/hr)


MEK = 0.0081W (Kg/hr)
SBA = 0.02W (Kg/hr)
Extractor Ethanol = 1.606W (Kg/hr)
Ethanol = 1.606W (Kg/hr)

Extract = X kg/hr
(MEK in Extract = 20%)

MEK balance:
0.1805W = 0.0081W + 0.2X
Solving for X in terms of SBA,
The amount of extract leaving from extractor, X = 0.862W
The composition of X is,
MEK = 0.172W
TCE = 0.67W
SBA = 0.02 W
Overall balance to find out the required TCE:
1.806W + T = 1.614W + 0.862W
T = 0.670W
31
SOLVENT RECOVERY DISTILLATION COLUMN
The extracted solution from extractor is distilled in solvent recovery distillation column to

separate solvent and MEK. Efficiency of the column is 99.9%

Distillate

MEK = 0.171W

SBA = 0.019W

MEK = 0.172W

SBA = 0.02W

TCE = 0.67W

Residue:

MEK = 0.001W

SBA = 0.001W

TCE = 0.67W

MEK PRODUCT DISTILLATION COLUMN

The distillate form solvent recovery column and the condensed liquid from separator are treated

in product distillation column. 99.9% pure methyl ethyl ketone is distilled.

32
Feed
From separator:
MEK = 0.7W
SBA = 0.08W
From solvent recovery column:
MEK = 0.171W
SBA = 0.019W

MEK = 0.87W

SBA = 0.001W

MEK = 0.871W

SBA = 0.099W

MEK = 0.001W

SBA = 0.098W
Amount of SBA required (W)

0.87W = 571 Kg/hr of MEK


W = 656.3 Kg/hr
1% loss of SBA is considered in knockout drum. So total SBA required at vaporizer inlet is,
= 1.01×656.3
=662.86 Kg/hr

*Using the value of W = 656.3 in material balance across the equipment; we will get the mass
flow of the different streams.
33
Material balance

REACTOR

MEK = 575 Kg/hr

H2 = 15.75 (Kg/hr)

Unreacted SBA = 65.63 (Kg/hr)

Secondary butyl alcohol


656.3 Kg/hr

Material Reactor in (Kg/hr) Reactor Out (Kg/hr)


Secondary butyl alcohol 656.3 65.63
Methyl ethyl ketone - 575
Hydrogen - 15.75
Total mass 656.3 656.3

34
CONDENSER

MEK = 575 Kg/hr


Liquid Phase:
H2 = 15.75 Kg/hr
MEK = 459.4 Kg/hr
Unreacted SBA = 65.63 Kg/hr
SBA = 52.5Kg/hr

Vapor phase:

MEK = 115.5Kg/hr

H2 = 15.75 Kg/hr

SBA = 13.13 Kg/hr

Condenser Out (Kg/hr)


Material Condenser in Liquid phase Vapor Phase
(Kg/hr)
Secondary butyl 65.63 52.5 13.13
alcohol
Methyl ethyl 575 459.4 115.5
ketone
Hydrogen 15.75 - 15.75
Total mass 656.3

35
SEPARATOR

Vapor phase:

MEK = 115.5 (Kg/hr)


Liquid Phase:
H2 = 15.75 (Kg/hr)
MEK = 459.4 (Kg/hr)
SBA = 13.13(Kg/hr)
SBA = 52.5 (Kg/hr)

Vapor phase:

MEK = 115.5 (Kg/hr)

H2 = 15.75 (Kg/hr)
Liquid Phase:
SBA = 13.13(Kg/hr)
MEK = 459.4 (Kg/hr)

SBA = 52.5 (Kg/hr)

ABSORBER

MEK = 2.3 Kg/hr

H2 = 15.75Kg/hr

Ethanol = 1054 Kg/hr

MEK = 5.32 Kg/hr

MEK = 115.5 Kg/hr

H2 = 15.75 Kg/hr

SBA = 13.13Kg/hr

MEK =118.5Kg/hr

SBA =13.13 Kg/hr

Ethanol = 1054 Kg/hr

36
EXTRACTOR

Trichloroethane
439.7 kg/hr
MEK =118.5Kg/hr

SBA =13.13 Kg/hr


Ethanol = 1054 Kg/hr
Ethanol = 1054 Kg/hr Extractor
MEK = 5.32 Kg/hr

Total Extract = 565.7 kg/hr


( MEK in extract = 112.88 Kg/hr

TCE = 439.7 Kg/hr

SBA = 13.13 Kg/hr )

SOLVENT RECOVERY DISTILLATION COLUMN

Distillate

MEK = 112.23 kg/hr

SBA = 12.47 Kg/hr

MEK = 112.88 Kg/hr

TCE = 439.7 Kg/hr

SBA = 13.13 Kg/hr

Residue:

MEK = 0.66 Kg/hr

SBA = 0.66 Kg/hr

TCE = 439.7 Kg/hr

37
MEK PRODUCT DISTILLATION COLUMN

Feed
From separator:
MEK = 459.41 Kg/hr
SBA = 52.5 Kg/hr
From solvent recovery column:
MEK = 112.23 Kg/hr
SBA = 12.47 Kg/hr
MEK = 571 Kg/hr

SBA = 0.66 Kg/hr

MEK = 571.64 Kg/hr

SBA = 64.97 Kg/hr

MEK = 0.64 Kg/hr

SBA = 64.32 Kg/hr

38
ENERGY BALANCE

Feed Preheater
Total secondary butyl alcohol = 662.86 Kg/hr
Feed inlet temperature = 298K
Feed outlet temperature = 373 K
Specific heat of SBA = 2.67 KJ/Kg K
Heat duty of preheater = m × Cp × ΔT
Q = 662.86 × 2.67 × (373-298)
=132737.7 KJ/hr------------------ 1
Steam Requirement
Steam inlet temperature = 413K
Condensate Outlet temperature = 363 K
Latent heat of steam @ 413K = 2133 KJ/Kg
Specific heat @ 413K =2.26 KJ/Kg K
Heat energy of steam in = m (λ + CpΔT)
= m [2133 + (2.26×140)]
= 2449.4m
Heat energy of steam condensate out = m ×4.2 × 90
= 378m
Heat given by steam = 2449.4m - 378m
=2071.4m -------------------------- 2
Equating (1) & (2)
Steam required, m = 132737.7 / 2071.4
m =64 Kg/hr
Vaporizer
SBA inlet temperature = 373K
SBA vapor outlet temperature = 385K
SBA Latent heat of vaporization = 562.6 KJ/Kg
39
Heat energy of SBA entering into vaporizer = m × Cp × ΔT
= 176983.62 KJ/hr------------------ (1)
Heat energy of SBA leaving the vaporizer= m (λ + CpΔT)
= 662.86 (562.6+2.67×110)
= 567607 KJ/hr--------------------- (2)
Heat added to vaporize SBA = 2-1
Q added =390623.4 KJ/hr --------------------- (3)
Heating medium in vaporizer = Reaction product leaving the reactor @ 633K
Temperature of reaction products leaving the vaporizer = T2
Heat energy of reaction product entering vaporizer
= mMEKCpΔT + mSBACpΔT + m Hydrogen CpΔT
QMEK = 575×2.3× (633-T2)
=1322.5(633-T2)
QSBA = 65.63×2.03× (633-T2)
= 133.23× (633-T2)
Q Hydrogen = 15.75×14.7× (633-T2)
=231.52× (633-T2)
Qtotal = 1687.25× (633-T2)---------- (4)
Equating (3) & (4)
T2 = 401.5K
Q total = 390598.38 KJ/hr
Super Heater-I
In S.H-I, the SBA vapors are heated to 573K from 385K. Flue gas is available at 673K.
Heat duty of super heater-I = 656.3×2.03× (573-385)
Q = 250470.33 KJ/hr

Flue gas requirement:


Flue gas inlet temperature = 673K
Flue gas outlet temperature = 423K
40
M fluegas× 1.172 × (673-423) = 250470.33
M fluegas = 854.85 Kg/hr

Super Heater-II
In S.H-II, the SBA vapors are heated to 773K from 573K.
Heat duty of super heater-I = 656.3×2.03× (773-573)
Q = 266457.8 KJ/hr

Flue gas requirement:


Flue gas inlet temperature = 813K
Flue gas outlet temperature = 673K
M fluegas× 1.172 × (813-673) = 266457.8
M fluegas = 1623.95 Kg/hr

Reactor
Dehydrogenation of secondary butyl alcohol is an endothermic reaction. Conversion is
considered as 90%
C4H10O C4H8O + H2
Heat of reaction (ΔHR):

ΔfH°MEK = -238.5 kJ/mol


ΔfH°SBA = -293 kJ/mol
ΔfH°Hydrogen = 0 kJ/mol
ΔH°R = (-238.5+0) – (-293)
= +55 kJ/mol (or) 55000 kJ/kmole
= 656.3 Kg/hr or8.88 kmole/hr
= 55000×8.88×0.9
ΔH°R= 439560 KJ/hr
41
Total heat balance, Q = Q1– Q2
Q1 = (m × Cp × ΔT + ΔH°R)
= 656.3× 2.03×500 + 439560
= 1105704.5 KJ/hr
Q2 = m × Cp avg × ΔT
= 656.3× 2.6×360
= 614296.8 KJ/hr
Q = 491407.7 KJ/hr
Flue gas required
M fluegas× 1.172 × (813-673) = 491407.7
M fluegas = 2995 Kg/hr
Condenser
The reaction products from vaporizer enter into condenser to cool down the temperature from
401.5K to 310K. 80% of MEK and SBA get condensed in condenser.
Heat loss due to condensation
Qc = Mmek(Cp×ΔT +λmek) + MSBA(Cp×ΔT+λSBA) + MHYDROGEN(Cp×ΔT)
λmek = 486 KJ/Kg
λSBA = 649 KJ/Kg
Qc = 459.4× ((2.3×91.5) +486) + 52.5× ((2.03×91.5) +649) +15.75×14.7×91.5
=319949.13+43824.11+21184.54 = 384957.78 KJ/hr
The liquid and vapors leaving the condenser is in equilibrium condition.
From T-X-Y diagram, at mole fraction X=0.8 of the condensate, the temperature of liquid and
vapor are obtained.
Liquid temperature = 305K
Vapor temperature = 338K
Heat duty to reduce vapor temperature from 401.5K to 338K
Q1 = 511.92×2.6× (401.5-338)
= 84518 KJ/hr
Total heat loss, Q = Qc + Q1

42
= 384957.78 + 84518
= 469475.78 KJ/hr

Cooling water required


CWS temperature = 297K
CWR temperature = 305K
Mass flow of CW = 469475.78 / (4.186×8)
= 14019.22 Kg/hr
Absorber
Heat of absorption = Mmek× λmek + MSBA ×λSBA
=(115.5×486) + (13.13×649)
= 64654.37 KJ/hr
Heat loss in cooling gases from 338K to 299K
= (2.3×1.7×39) + (15.75×14.7×39)
= 9182 KJ/hr
Total heat released = 64654.37 + 9182
= 738336.37 KJ/hr
Heat gained by absorption operation
= [(115.5×2.3) + (13.13×2.67) + (1054×2.5)] × (T-299)
=2935.71× (T-299)
2942.61× (T-299) = 738336.37
To = 324.15K

43
Solvent recovery column
Feed:
MEK = 112.88 Kg/hr
SBA = 13.13 Kg/hr
TCE = 439.7 Kg/hr
Total, F = 565.71 Kg/hr
Feed temperature is 28°C
Enthalpy of Feed, HF = [ (112.88×2.3) + (13.13×2.67) + (439.7×1.1) ] × (28)
= 21793.83 KJ/hr
Distillate:
MEK = 112.23 Kg/hr
SBA = 12.47 Kg/hr
Distillate temperature from T-x-y diagram, 81°C
Enthalpy of distillate, HD=23605.34 KJ/hr
Residue:
MEK = 0.66Kg/hr
SBA = 0.66 Kg/hr
TCE = 439.7 Kg/hr
Residue temperature is 115°C
Enthalpy of residue, HR = 56000 KJ/hr

Overhead condenser:
Heat load on condenser, QC =V×λ
V = (1+R) D
R = 2Rm
Rm = 0.3 (from x-y diagram)
R = 0.6
V = 199.5 Kg/hr
44
Qc = 100208.85 KJ/hr
Cooling water requirement:
Mw = 100208.85/(4.186×8)
=2992.3 Kg/hr

Reboiler:
QB = Qc + HR- HF
= 131941.5 KJ/hr
Steam requirement:
Heat energy of steam in = m (λ + CpΔT)
= m [2133 + (2.26 ×140)]
= 2449.4m
Heat energy of steam condensate out = m × 4.2 × 90
= 378m
Heat given by steam = 2449.4m - 378m
= 2071.4m
Steam required, m = 131941.5 / 2071.4
m = 63.69 Kg/hr
Product MEK distillation column
Feed:
MEK = 571.64 Kg/hr
SBA = 64.97 Kg/hr
Enthalpy of Feed, HF = [ (571.64×2.3) + (64.97×2.67) ]× (25)
= 37206.05 KJ/hr
Distillate:
MEK = 571 Kg/hr
SBA = 0.66 Kg/hr
Distillate temperature from T-x-y diagram, 79°C
Enthalpy of distillate, HD= 103889.9 KJ/hr
45
Residue:
MEK = 0.64Kg/hr
SBA = 64.32 Kg/hr
Residue temperature is 102°C
Enthalpy of residue, HR = 17667.05 KJ/hr
Overhead condenser:
Heat load on condenser, QC =V×λ
Qc = 277934.34 KJ/hr
Cooling water requirement:
Mw = 277934.34 / (4.186×8)
=8299.5 Kg/hr

Reboiler:
QB = Qc + HR- HF
= 258395.34 KJ/hr
Steam requirement:
Heat energy of steam in = m (λ + CpΔT)
= m [2133 + (2.26 ×140)]
= 2449.4m
Heat energy of steam condensate out = m × 4.2 × 90
= 378m
Heat given by steam = 2449.4m - 378m
= 2071.4m
Steam required, m = 258395.34 / 2071.4
m = 125 Kg/hr

46
DESIGN OF CONDESER
Amount of heat removed by condenser
Q = 469475.78 KJ/hr
Amount of cooling water required
Inlet cooling water temp = 24°C
Outlet cooling water temp = 32°C
Mass flow of CW = 469475.78 / (4.186× 8)
= 14019.22 Kg/hr
LMTD: (COUNTER CURRENT FLOW)
Th1=128.5°C Th2= 37°C
Tc2 = 32°C Tc1 =24°C
LMTD = (128.5-32) – (37-24) / ln ((128.5-32) / (37-24))
= (96.5-13) / ln (96.5 / 13)
= 83.5 / ln 7.423
= 41.75°C
True temperature difference
S = (Tc2– Tc1) / (Th1- Tc1) = (32 – 24 ) / (128.5 – 24)= 8 / 104.5
= 0.077
R = (Th1 - Tc2) / (Tc2- Tc1)= (128.5 – 32) / (32 - 24) = 96.5 / 8
= 12
From graph Ft = 12 × 0.077 = 0.924
ΔTln = 41.75 × 0.924
=38.58°C
Assume Overall heat transfer coefficient = 581.5 W / m2°C
TO FIND NUMBER OF TUBS:
BWG = 16
Tube outer diameter (OD) = 3/4 ’’ = 0.0191 m
Tube Inner diameter (ID) =0.620” = 0.0157m
Length of tube = 8ft= 2.44m
47
Outer surface area of each tube =πDL
= (22 /7) × 0.0191 × 2.44m
= 0.146m2
HEAT TRANSFER AREA:
Q = UAΔTln
U assumed = 581.5 W/m2 °C
469475.78 = 581.5 × 38.58 ×A
A = 20.93m2
NUMBER OF TUBE = Heat transfer area / Outer surface area of each tube
Nt = 20.93 / 0.146
= 143.36
Near tube count = 150tubes
Pitch (triangular) = 15 /16 inch
Number of shell pass = 1
Number of tube pass = 4
Shell side condensing vapor
Tube side cooling water
TUBE SIDE
Cooling water mean temperature = 28°C
Water properties at this temperature
Density = 993Kg / m3
Viscosity = 0.85Cp
Thermal conductivity =0.620W / m2°C
Water flow rate = 14019.22 / 993*3600 = 0.004 m3/sec
Flow area = (Nt/n)× π/4 ×Di2
=0.0027m2/pass

Linear velocity of water = water flow rate/flow area


= 0.004/0.0027= 1.48 m/sec (greater than the min of 1m/s)
48
Tube side heat transfer co-efficient
Mass flow rate of water, Gt = 1.48×993 = 1469.64 Kg/m2s
NRe = (Di×Gt) / µ
= (0.0157×1469.64) / 0.85×10-3
= 27145.1
Npr = (Cp×µ) / k
= (4186×0.85×10-3) / 0.623
= 5.711
(hi×Di) / K = 0.023 (NRe)0.8 × (Npr)0.33
hi = [ 0.023×(27145.1)0.8× (5.711)0.33× 0.623 ] / 0.0157
hi = 5714.58 W/m2 °C
hio = hi× (Di/Do) = 5714.58×0.8266= 4723.67W/m2 °C
Shell side heat transfer co-efficient

NRe = 4Γ / µ = (4/µ) × W / ((Ntubes)0.67 × L)


= (4×18.23) / (0.0027×(150)0.67×2.44)
= 386

Nu = 1.51 ×[ (Do3×ρ2×g)/ µ2)0.33 (NRe)-0.33 ]


= 159.85
hoD/K = 159.85
ho = (159.85×0.14) / 0.0191
=1171.68 W/m2 °C

1/Uo = 1/ho + 1/hio + wall resistance + fouling factor


1/Uo = (1/1171.68) + (1/4723.67) + 4.1×10-5 + 5.3×10-4
= 0.001636
Uo = 611.5 W/m2 °C
Uo >Uassumed

49
Pressure drop calculations
Tube side:
NRe= 27145.1
f = 0.079(Re)-0.25=0.079(27145.1)-0.25
= 6.155×10-3
F = friction factor
Pressure Drop along the pipe length
(Δp)L = (ΔH)L×ρ×g
= 4fLVp2 /2g(ID) ×ρ×g
= (4×6.155×10-3× 2.44×1469.642×9.81) / 2×9.81×0.0157×1000
= 4.128KPa
Pressure Drop in the end zone
(Δp)e = 2.5×ρ×Vp2/2 = (2.5×993×1.469642) / 2
=2.68KPa
Total Pressure Drop in the pipe = (Δp)total= (4.128KPa+2.68KPa)2
= 13.616KPa ˂ 70KPa
Shell side: Kern’s method
Baffle spacing (B) = Ds = 340mm
C1 = 0.0254 – 0.0191 = 0.0063
PT= pitch =0.0 254m
ashell=shell diameter×C1×B /PT= (0.34×0.0063×0.34) /0.0 254
= 0.0287 m2

De = 4((PT /2)×0.86PT–(1 / 2) × (π/4)× (OD)2) / πdo/2

= 4((0.0254)2/ 2) ×0.86 – (π / 8)×(0.0191)2)/ π(0.0191) / 2

De =18.29mm

Gs = Superficial velocity in shell side =mshell/ ashell

=18.23 / 0.155 = 117.61Kg/m2s

NRe =GsDc / µ = (117.61×0.0139) / 0.85×10-3


50
= 1923.26

f = 1.87(1923)-.2= 0.412

Shell side pressure drop = (Δp)s=((4f(Nb+1)DsGs2g) / (2gDe×ρvapor))×0.5

No of baffles, Nb = L/Ls

(ΔP)s=0.5{[4× (0.412)×26×0.34×(18.23)2×9.81] / (2×9.81×0.01829×2.48)}

= 23.74 Kpa (less than the acceptable pressure drop 70Kpa)

Total pressure drop = Shell side pressure drop + Tube side pressure drop
= 37.35Kpa (less than the acceptable pressure drop 70Kpa)

MECHENICAL DESIGN:

Shell side:

Material – carbon steel

No. of shell – 1

No. of pass – 4

Fluid – condensing vapor

Inlet temperature = 128.5°C

Outlet temperature = 37°C

Internal diameter of shell (Ds) = 0.34m

Working pressure (P) =1×105 N/m2

Design pressure (Pd) = 1.1×105N/m2

Permissible strength for carbon steel = 95N/mm2

Tube side:

Number of tube = 150

Outside diameter = 0.0191m; Inner diameter = 0.01587m

51
Length of tube = 8ft = 2.44m

Pitch Δlar= 25.4×10-3m

Feed = Cooling water

Inlet temperature = 24°C

Outlet temperature = 32°C

Working pressure (P) =1×105 N/m2

Design pressure (Pd) = 1.1×105N/m2

Shell side:

ts= (PDi / 2fJ-P)

ts= shell thickness

Pd = Design pressure = 0.11N/mm2

Di = Inside diameter of shell = 340mm

f = allowable stress value = 95N/mm2

J = joint factor = 0.85

ts=0.11(340) / ( 2(95)(0.85) – (0.11))

= 0.23mm

Minimum shell thickness = 6mm

Corrosion allowance = 3mm

Thickness of shell ( ts) = 6+3 = 9mm (including corrosion allowance)

Approx. = 10mm
Head: (Torrispherical head)
th= (PRcW / 2fJ)
th=thichness of head
W = 1 / 4 (3+(Rc / Rk)1/2 )
Rc= crown radius = outer diameter of shell = 340mm

52
Rk = knuchle radius = 0.06Rc
W = 1 / 4 (3+(Rc / 0.06Rc)1/2 ) = 1.77
th= (0.11) (340)(1.77) / 2(95)(0.85) = 0.41mm
Minimum shell thichness = 6mm

Corrosion allowance = 3mm

Total shell thickness = 6+3 =9mm (Near 10mm)


Baffle arrangement:
Type – Transverse baffle (Baffle cut = 25%)
No. of baffle = 25
Baffle spacing = 97.8mm
Thickness of baffle = 6mm
Height of baffle = 0.75×baffle spacing
= 73.35mm =7.3cm
THERODS AND SPACERS:
Forshell ID = 0.5m, no. of tie roads = 2
Diameter of the rods = 10mm
Spacer diameter = 8mm
Flange:
Loose type except tap joint flange.

Design pressure = 0.11N/mm2


Flange material IS:2004 – 1962 class 2
Bolting steel: Asbestos composition
Shell side diameter = 340mm
Shell side thickness = 10mm
Outside diameter of shell = 340+ (10) (2) = 360
Determination of gasket width:
do / di = ((y-pm)/(y-p(m+1))1/2
y =yield stress

53
m = gasket factor
Gasket material chosen is asbestos with a suitable binder for the operating conditions.
Thickness = 10mm
m = 2.75
y = 2.60(9.81) = 25.5N/mm2
do / di = ((25.5 - 0.11(2.75) / (25.5 – 0.11(2.75+1))1/2
= 1.0004
di = in side diameter of gasket = outside diameter of shell
= 360+5
= 365mm
do = outside diameter of the gasket
= 1.004(365) = 366.46mm
Minimum gasket width = (365 – 365) / 2 =0.73mm
But minimum gasket width = 6mm
G = 365+2(6) = 377mm
G = diameter at the location of gasket load reaction.
Calculation of minimum bolting area:
Minimum bolting area (Am) = Ag = Wg/ Sg
Sg= tensile strength of bolt material (MN/m2)
Consider, 5% Cr-Mo steel, as design material for bolt
At = 128.5°C
Sg=138×106N/m2Am= (0.6037×106) / 138×106 = 4.375×10-4m2
Calculation for optimum bolt size:
g1= go / 0.707 = 1.41go
g1=thickness of the hub at the back of the flange
go=thickness of the hub at the small end =10+2.5 = 12.5mm
Selecting bolt size M18×2
R = Radial distance from bolt circle to the connection of hub & back of flange
R = 0.027
54
C = Bolt circle diameter = ID + 2(1.41(go+R)
C = Bolt circle diameter = ID + 2(1.41(0.0125) +0.027)
= 0.340 +2[(1.41)(0.0125)+0.027]
= 0.429m
Estimation of bolt load:
Bolt due to design pressure(H) = πG2P / 4
H = π (377)2 (0.11) / 4 = 0.0491×106N
Load to keep the joint tight under operating conditions.
Hp= πg (2b)mp
b = Gasket width = 6mm = 0.006m
Hp= π (0.377) (2) (0.006) (2.75) (0.11×106) = 4.3×103 N
Total operating load (Wo) H+Hp= 0.0491×106N+4.3×103 N
= 0.0534×106N
Load to seat gasket under bolt – up condition = Wg
Wg= π g b y
= π× 0.377×0.006×25.5×106
= 0.18128×106N
Wg>Wo
Wg is the controlling load
Controlling load = 0.18128×106N
Actual flange outside diameter (A) = C + bolt diameter + 0.02
= 0.43m + 0.018 + .002
= 0.468m
Check for gasket width:
Ab= minimum bolt area = 44×1.54×10-4m2
AbSg/ πGN = (44×1.54×10-4) 3.8×10-4 / 3.14(0.377)(0.012)
= 18.1N/mm2
2y = 2×25.5 =51N/mm2
2y>AbSg/ πGN
55
Bolting condition is satisfied.

Flange Moment calculations:


For operating conditions:
WQ = W1 +W2 +W3
W1 = (π/4) B2 P = Hydrostatic end force on area inside of flange.
W2 = H-W1
W3= gasket load = WQ - H = Hp
B= outside shell diameter = 360 mm
W1 = π/4 (0.360)2 x 0.11 x 106 = 0.0448 x 106 N
W2 = H- W1=(0.0491 – 0.0448) x 106 =0.0026 x 106 N
W3 = 4.3 x 103 N
WQ=( 0.0448+ 0.0026 + .0043 ) x 106
= 0.0513x 106 N
Mo = Total flange moment = W1 a1 + W2 a2 + W3 a3
a1 = (C –B) / 2; a2 = (a1 + a3) / 2; a3 = (C –G) / 2
C=0.429; B=0.360; G=0.377
a1 = (0.429 – 0.360) / 2 = 0.0345
a3 = (C – G) / 2 = 0.429 – 0.377 = 0.026
a2 = (a1 + a3) / 2= 0.0345 +0.026 = 0.0303
Mo=[ 0.0448 ( 0.0345) + 0.0022 ( 0.0303) +0.0043 (0.026) ] x 106
=1.724 x 103 J
For bolting up condition:
Mg = Total bolting Moment =W a3
W =[(Am +Ab) / 2]Sg .
Am =2.869 x 10-3
Ab= 44 x 1.5 4x 10-4 = 67.76 x 10-4
Sg= 138 x 106
W= (2.869 x 10-3 + 67.76 x 10-4) x 138 x 106
56
= 0.666 x 106
Mg = 0.666x 106 x 0.026 = 0.017 x 106 J
Mg> Mo
Mg is the moment under operating conditions
M= Mg = 0.017 x 106 J
Calculation of the flange thickness:
t2 = (MCFY / BSFO)
CF= Bolt pitch correction factor = [Bs/ (2d + t)]1/2
Bs= Bolt spacing = (π C / n) = (0.429x22 / 22x7) = 0.06128 m

n= number of bolts = 22
Let CF = 1
SFO = Nominal design stresses for the flange material at design temperature.
SFO = 100 x 106 N
M = 0.017 x 106 J
B = 0.360 m.
K = (A / B) = (Flange diameter / Inner Shell diameter)
= 0.468 / 0.360
= 1.3
Y=8
t = √ (0.017 x 106 x 1 x 8) / (0.360x100x106 = 0.061 m
d = 18 x 2 = 36mm
CF =√ [0.06128 / (2(36 x 10-3) + 0.061)]
= 0.68
CF = (0.83)2
t = 0.061 x 0.83 = 0.0506 m
t = 50mm = 0.05m
Tube sheet thickness :(Cylindrical Shell).
T1s = Gc√ (KP / f)
57
Gc= mean gasket diameter for cover = 0.377
P = design pressure.
K = factor = 0.25 (when cover is bolted with full faced gasket)
F = permissible stress at design temperature.
t1s = 0.377 √ (0.25 x 0.11 x 106) / ( 95 x 106) = 0.0064 m
Channel and channel Cover
th=Gc√ (KP/f) ( K = 0.3 for ring type gasket)
= 0.377√[(0.3 x 0.11)/ 95]
= 0.007 m = 7 mm
Consider corrosion allowance = 4 mm.
th=0.004 + 0.007 = 0.011 m.
Saddle support:
Material: Low carbon steel
Total length of shell: 2.44 m
Diameter of shell: 0.360 mm
Knuckle radius = 0.06 x 0.360 = 0.0216 m = ro
Total depth of head (H)=√ (Doro/2)
= √ (0.360 x 0.0216 /2)
= 0.0235 m
Weight of the shell and its contents = 1875 kg = W
R=D/2=0.360 / 2 = 0.18m = 180 mm
Distance of saddle center line from shell end = A =0.5R=0.09 m.
Longitudinal Bending Moment
M1 = QA [1-(1-A/L+ (R2-H2)/ (2AL))/ (1+4H/ (3L))]
Q = [W (L+4H/3)] / 2
= 1875(2.44 + 4 x 0.1398/3)/2
= 2462.25 kg / m
M1 = [2462.25x0.2 { 1- (1-0.2/2.44+(0.182-0.062352)/(2x2.44x0.2)) }]
. /[(1+4x0.06235/(3x2.44))]
58
= 8.55kg-m
Bending moment at center of the span
M2 = QL/4[(1+2(R2-H2)/L)/ (1+4H/(3L))-4A/L]
M2 = 785.416 kg-m
Stresses in shell at the saddle
(a) At the topmost fibre of the cross section
f1 =M1/(k1π R2 t) k1=k2=1
=8.55/(3.14 x 0.182 x 0.01)= 8404.104 kg/m2
The stresses are well within the permissible values.
Stress in the shell at mid-point
f2 =M2/ (k2π R2 t)
= 160.8 kg/cm2
Axial stress in the shell due to internal pressure
fp= PD/4t
= 0.11 x 106 x 0.340/ (4 x 0.01)
= 93.5 kg/cm2
f2 + fp = 254.3 kg/cm2
The sum f2 and fp is well within the permissible values.

59
ABSORBER
Gas Inlet:
MEK = 115.5Kg/hr
SBA = 13.13Kg/hr
H2 = 15.75Kg/hr
Gas out:
MEK = 2.3Kg/hr
H2 = 15.75Kg/hr
Liquid inlet:
MEK = 5.32 Kg/hr
Aq.ethanol = 1054Kg/hr
Liquid outlet:
MEK = 118.5 Kg/hr
SBA = 13.13 Kg/hr
Aq.ethanol = 1054Kg/hr
At absorber top:
(L/G)× (ρg/ρl)0.5= (1059.32/18.05)× (1.25/797)
= 0.092
At absorber bottom:
(L/G)× (ρg/ρl)0.5= (1185.63/144.38)×(1.7/818)
= 0.017

60
Flow parameter (L/G)× (ρg/ρl)0.5is greater at top of the absorber. So flooding conditions are
considered at top and the percentage is 80%

From Generalized pressure drop correlation chart, at 0.5 inch of water/ ft pressure drop,
G2Fp(ρw/ρl)µL0.2/(ρg×ρl×g) = 0.05

Packing material is 1/2” Raschig rings and packing factor Fp from design data table

61
Fp= 2100m-1; surface area, a=368m2/m3
G2×2100×1.25× (0.0011)0.2/(1.25×797×9.81) = 0.05
G2=0.727 Kg/m2s
Superficial mass flow rate of gas, G = 0.85Kg/m2s
Cross sectional area, Ac = Gt/G
Ac = 0.26m2
(π/4)×Dc2 = 0.26
Diameter, Dc =0.58m
Dc/dp = 0.58/0.013 = 44.6 (greater than the minimum ratio of 10)
Wetting rate:
Lw = L/(Ac×ρl×a)
= 1059.32/ (0.26×797×368)
= 0.138 m2/hr
= 1.4 ft2/hr (greater than 0.85ft2/hr)

62
Pressure drop:
ΔP = C2×10C3Utl ×Utg2
= 0.02×10(0.9×0.0041) × 2.62
= 13.63 mm H2O/meter packing
Height of the absorber:
Z = HTU×NTU
HTU = HG+ (mG/L) HL
HG = 0.029×Ψ×D1.11×Z0.33×Scg0.5 / (Lf1f2f3)0.5
ScG= gas-phase Schimidt number (dimensionless number)
= µG/ρgDg = 0.45
ψ =Correlation parameter
For 80% flooding, ψ = 60
f1= (µL/µw) 0.16, with µW=1.0 mPa.s
f2 = (ρw/ρL) 1.25 with ρw=1000 kg/m3
f3 = (σw/σl) 0.8, with σw = 72.8 mN/m
f1= 1.015
f2 = 1.32
f3 = 0.9
HG = 0.029×60× (0.58)1.11×Z0.33× (0.45)0.5 / (1.13×1.015×1.32×0.9)0.5
HG= 0.54 Z0.33
HL = (φC/3.28) × (µL/ρLDL) 0.5× (Z/3.05)0.15
φ = Correlation parameter for given packing, m
C = correlation factor for high gas rates
µL =liquid viscosity, Pa.s
ρL =Liquid density , kg/m3
DL =liquid –diffusion coefficient, m2 /s
Z =height of packing,m

φ = 0.03
63
µL = 1.09cP
C = 0.6
HL = (φC/3.28) × (µL/ρLDL) 0.5× (Z/3.05)0.15
= (0.03×0.6/3.28)× [(0.0011/797×35)]0.5 × (Z/3.05)0.15
= 0.148Z0.15

HTU = 0.54 Z0.33 + (mG/L) 0.148Z0.15


NTU Calculations:
NTU = ∫ [dY / (Y-Y*)] – [½ ln {(1+ Yb) / (1+ Yt)}] Yt

Y Y* 1/(Y-Y*)
0.05 0.043 142.86
0.1 0.07 33.33
0.15 0.11 25
0.2 0.165 28.6
0.25 0.19 16.67
0.34 0.26 12.5
0.4 0.3 10

Plotting a graph of 1/(Y – Y*) Vs Y,


Area under the curve from Yt to Yb = ∫ [dY / (Y-Y*) ] = 4.5
And the value of [ ln{(1+ Yb)(1+ Yt)}/2] = 0.12
NTU = 4.5 – 0.12 = 4.38
(m× G/ L)avg = 0.2
Z = HTU ×NTU
= (0.54Z0.33 + 0.3Z0.15)×4.38
= 2.365Z0.33 + 1.3Z0.15
By trial and error method, Z = 6 meter

64
MECHENICAL DESIGN:
Material used = carbon steel
Thickness of the shell = ts
ts = (PD / 2fJ-P)+C
D –inner diameter of the column = 0.58m
Working pressure = 1.013×105N/m2
Design pressure =1.1143×105 N/m2
Permissible stress, f =95×106 N/m2
Joint efficiency, J= 0.85
Corrosion allowance = 5mm
ts = (1.1143×105×1/2×95×106×0.85-1.1143×106)
ts = 5.69mm = 6mm (approx.)
Outer diameter of the column Do = 0.592m
DESIGN OF GASKET AND BOLT SIZE CALCULATIONS:
Width of the gasket, N = 10mm
Gasket material – ASBESTOS
Gasket factor, m =2
Minimum design seating stress y =11.2N/mm2
Basic gasket seating widthbo = N/2 = 10/2 = 5mm
Effective gasket seating width, b= 5.6mm
BOLT LOAD CALCULATIONS:
Wm1 = π×b×G×Y
G = Mean diameter = (Dfi + Dfo) / 2 = 0.586m
Wm1= 115407.31 N

Under operating condition,


Wm2 = (π×2b×G×m×P) +(π/4×G2 ×P)
= 346305.225 N
Bolt material: HOT ROLLED CARBON STEEL
65
Bolt area:
Am1 = Wm1/Sa
Am2 = Wm2/Sb
Sa – Nominal bolt stress at design temperature = 58.7×106N/m2
Sb – Nominal bolt stress at ambient temperature = 56.2×106N/m2
Am1 = (115407.31/58.7×106) = 0.002 m2
Am2 = (346305.225/56.2×106) = 0.006m2
Actual bolt area:
Ab = 2πYGN/Sa
= 2×3.14×11.2×586×10/ (56.2×106)
= 0.0073m2 (Ab>Am)
No of Bolts = Mean diameter/ 2.5×bo
= 0.586/(2.5×0.005)
=47 bolts

To find size of the bolts larger bolt area is considered.


Diameter of bolt = ((0.0073×4)/3.14) 0.5
=96 mm

Flange Thickness:
tf =G×(P/Kf)0.5 + C
K = 1/ (0.3+ (1.5WmhG)/H×G)
Hydrostatic end force H = π/4 × G2×P
=51.25 Kw
Radial distance from gasket load to bolt circle,
hG= 0.015m
Wm = 346305.225 N
66
K = 1.19
tf = 23mm
HEAD DESIGN: FLANGED AND SHALLOW
Material – stainless steel
Permissible stress, f = 130N/mm2
Design pressure, p= 1.1143×105 N/m2
Stress identification factor, W = 1/4× (3+ (Rc/R1))
Crown radius, Rc = 0.5 m
Knuckle radius, R1 = 6% of Di = 0.03m
W = 2.83
Thickness of head, th = (P×Rc×W)/2×f
= 4.45mm = 5mm (approx.)

Nozzle thickness:
Material – SS
Dn =0.25m
Thickness,tn = (P×D×N)/ (2×f×J-P)
= 2.6mm = 3mm(approx.)
There for we can take the thickness of the nozzle as 3mm (No corrosion allowance because the
material is stainless steel)

67
STRESS ANALYSIS AND SHELL THICKNESS AT DIFFERENT HEIGHTS:
Axial stress due to pressure,fap =PDi /4(ts-C)
= (1.1143×105×1) / (4×(6×103-0.0008)
fap = 5.35×106N/m2
Stress due to dead load,
Compressive stress due to weight of shell unto ‘x’ distance,
Outer diameter = 0.012m
Density of shell material = 7700Kg/m3
fds = π/4(Do2-Di2) ×ρ×X / π/4×(Do2-Di2) =7700.08xKg/m2
Compressive stress due weight of installation at height x
Material of insulation – ASBESTOS
Thickness – 3cm
Density - 2200Kg/m3
Dins – diameter of insulation
Dm – mead diameter of vessel
Dins= Dm
fds = (π ×Dins×tins×ρins×x)/(π ×Pm×ts-C))

Compressive stress due weight of installation at height x


Material of insulation – ASBESTOS
Thickness – 3cm
Density - 2200Kg/m3
Dins – diameter of insulation
Dm – mead diameter of vessel
Dins = Dm
fds = (π ×Dins×tins×ρins×xφ)/(π×Pm×ts-C))
= (π×0.586×3×10-2×2200×X) / (π×1.1143× (6×10-3-0.0008))
= 12712.40N/m2
68
Compressive stress due to liquid in the column unto x
ρ1= 797kg/m3
fdliq= (π/4×0.5862×797) / (π/4×0.586×0.006)
= 77840.33 N/m2
Compressive stress due to attachments
1. Packing weight
2. Head weight
3. Ladder
Density of packing, = 705kg/m3 (Raching rings ceramics)
Packing weight = (π/4×Di2×x×ρ×9.81)
= π/4×0.5862×705×X×9.81 = 1864.33X N
Head weight = π/4×0.5862×797×X×9.81
= 2107.62X N
Weight of ladder =1600X kgs
fd (attachments) = (Packing weight+Head weight+Ladderweight) / π×Di×(ts-C)
= (1864.33X+2107.62X+100x) / (π×0.586×(0.006-0.0008))
= 425570.0X N
Stress due to wind:
fwx= Mw /2
Mw = 1.4×φ×Do×x2/2
Z = π/4×Do ×x2 /2 = 0.00234x2
Pressure due to wind Pw =0.05×V2w
Velocity of wind = 100km/hr
Pw = 500N/m2
fmw = (1.4×500×0.598×x2)/2 = 209.3x2
fmw = 209.3x2/ 0.00234 = 89444.4.58x2
To = find the value of x:
ftmax=95×106N/m2
ftmax= fwx+fap-fax
69
x = 10.5m
The x obtained is greater than the tower height; hence the shell thickness can withstand the
stress.
SUPPORT:
Skirt support is used.
Di = 0.58m
Do = 0.592m
H = 6m
ρs = 7700kg/m3
ρ1= 797kg/m3

Total weight :
= weight of steel +weight of attachments (liquid + packing + head + ladder
= π/4× (Do2-Di2)×H×ρs×9.81+π/4× (Di2×H×ρ1×0.77) +(π/4×Di2×H×ρp) +40660.5+1600H
= 65362.53 N
Diameter of skirt = 0.58m
Height of skirt = 1.5m
Wind of pressure = 500N/m2
Stress due to dead load:
fd = Total weight / (π×D×tsk)
= 65362.53/(π×0.58×tsk)
= 20816.09/tsk
Due to wind load
Pw = k×P1×h1×Do
K = 0.7
Pw = 4.32×106×N/m2
Bending moment due to wind at the base of the vessel,
Mw = P1w×h1/2
70
Mw = 4.32×106Nm
fwb=(5.44×106/tsk)
Stress due to seismic load:
Load F = C×W
W – total weight of the vessel =65362.53N
C – Seismic coefficient – 0.08
fsb= 2/3× (CWH / π×Rok×tsk)
fsb= 26644.598 /tsk
Maximum stress at the bottom of the skirt
fmax=(fwb orfsb) - fdb
(5.44×106)tsk-20816.09/tsk = 140×106
tsk = 0.0387m
tsk = 38.7mm

COST ESTIMATION AND ECONOMIC


Cost of MEK plant of capacity 35000 TPY in 1967 is $3.75×106 = Rs.1.875x 108
Therefore cost of 5000 TPY in 1967 is:
C1 = C2 (Q1/Q2)0.6
=1.875x 108(5000/35000)0.6
= Rs.1.61 x 107
Chemical Engineering Plant Cost Index: Cost index in 1967 = 110
Cost index in 2002 = 402

Thus, Present cost of Plant = (original cost) × (present cost index)/(past cost index) = (1.61 x
107) × (402/110) = Rs 5.88×107
i.e., Fixed Capital Cost (FCI) = Rs. 5.88×107

Estimation of Capital Investment Cost:


Direct Costs:
Material and labor involved in actual installation of complete facility (70-85% of fixed-
capital investment)
71
a) Equipment + installation + instrumentation + piping + electrical + insulation + painting (50-
60% of Fixed-capital investment)
Purchased equipment cost (PEC): (15-40% of Fixed-capital investment)
Consider purchased equipment cost = 25% of Fixed-capital investment

PEC = 25% of 5.88×107= Rs.1.47×107


Installation, including insulation and painting: (25-55% of purchased equipment cost.)
Consider the Installation cost = 40% of Purchased equipment cost
40% of 1.47×107= Rs.5.88×106
Instrumentation and controls, installed:
(6-30% of Purchased equipment cost.)
Consider the installation cost = 20% of Purchased equipment cost
= 20% of ×1.47×107= Rs.2.94×106
Piping installed:

(10-80% of Purchased equipment cost) Consider the piping cost = 40% Purchased equipment
cost
40% of Purchased equipment cost = 0.40 ×1.47×107
= Rs. 5.88×106
Electrical, installed:

(10-40% of Purchased equipment cost) Consider Electrical cost = 25% of Purchased equipment
cost
25% of 1.47×107= Rs.3.675×106
Buildings, process and Auxiliary:

(10-70% of Purchased equipment cost) Consider Buildings, process and auxiliary cost = 40% of
PEC
40% of 1.47×107= Rs. 5.88×106
Service facilities and yard improvements:
(40-100% of Purchased equipment cost)
Consider the cost of service facilities and yard improvement = 60% of PEC
60% of 1.47×107= Rs. 8.82×106
72
Land: (1-2% of fixed capital investment or 4-8% of Purchased equipment cost) Consider the cost
of land = 6% PEC = 6% of 1.47×107
= Rs. 0.882×106
Thus, Direct cost = Rs. 4.865×107 ----- (82.75% of FCI)

Indirect costs:
Expenses which are not directly involved with material and labor of actual installation of
complete facility (15-30% of Fixed-capital investment)
Engineering and Supervision: (5-30% of direct costs)
Consider the cost of engineering and supervision = 10% of Direct costs
Cost of engineering and supervision = 10% of 4.865×107
= Rs. 4.865×106

Construction Expense and Contractor’s fee: (6-30% of direct costs)


Consider the construction expense and contractor’s fee = 15% of Direct costs
=Rs.7.29×106
Contingency: (5-15% of Fixed-capital investment)
Consider the contingency cost = 10% of Fixed-capital investment
= 5.88×106
Thus, Indirect Costs = Rs. 1.8×107 --- (30% of FCI)

Fixed Capital Investment:


Fixed capital investment = Direct costs + Indirect costs
= 4.865×107 + 1.8×107
= 6.6×107
Fixed capital investment = Rs. 6.6×107
Working Capital:
(10-20% of Fixed-capital investment)
Consider the Working Capital = 15% of Fixed-capital investment

73
Working capital = 15% of 6.6×107= Rs.0.99 ×107
Total Capital Investment (TCI):
Total capital investment = Fixed capital investment + Working capital
= 6.6×107 + 0.99 ×107
Total capital investment = Rs. 7.5×107
Estimation of Total Product cost:
Manufacturing Cost = Direct production cost + Fixed charges + Plant overhead cost.

Fixed Charges: (10-20% total product cost)


Depreciation:

(Depends on life period, salvage value and method of calculation-about 13% of FCI for
machinery and equipment and 2-3% for Building Value for Buildings)

Consider depreciation = 13% of FCI for machinery and equipment and 3% for Building Value
for Buildings)
Depreciation = (0.13×5.88×107) + (0.03×5.88×106) = Rs. 7.82×106

74
Local Taxes:
(1-4% of fixed capital investment) Consider the local taxes = 3% of fixed capital
Local Taxes = 0.03×6.6×107
= Rs.1.98×106

Insurances:
(0.4-1% of fixed capital investment) Consider the Insurance = 0.7% of fixed capital investment
Insurance = 0.007×6.6×107= Rs. 0.462×106

Rent:
(8-12% of value of rented land and buildings)
Consider rent = 10% of value of rented land and buildings
= Rs. 0.67×106
Thus, Fixed Charges = Rs. 11×106
Direct Production Cost: (about 60% of total product cost)
Now we have Fixed charges = 10-20% of total product charges – (given)
Consider the Fixed charges = 15% of total product cost
Total product charge = fixed charges/15%
Total product charge = 11×106/15%

Total product charge = Rs. 7.3×107


Raw Materials: (10-50% of total product cost)
Consider the cost of raw materials = 25% of total product cost
Raw material cost = 25% of 7.3×107
Raw material cost = Rs. 1.825×107
Operating Labor (OL): (10-20% of total product cost)
Consider the cost of operating labor = 12% of total product cost
Operating labor cost = 12% of 7.3×107
=Rs. 8.76×106

75
Direct Supervisory and Clerical Labor (DS & CL): (10-25% of OL)
Consider the cost for Direct supervisory and clerical labor = 12% of OL
Direct supervisory and clerical labor cost = Rs. 1.05×106
Utilities: (10-20% of total product cost)
Consider the cost of Utilities = 12% of total product cost
Utilities cost= 12% of 7.3×107
Utilities cost = Rs. 8.76×106

Maintenance and repairs (M & R):


(2-10% of fixed capital investment)

Consider the maintenance and repair cost = 5% of fixed capital investment Maintenance and
repair cost = 0.05×6.6×107= Rs. 3.3×106
Operating Supplies: (10-20% of M & R or 0.5-1% of FCI)
Consider the cost of Operating supplies = 15% of M & R
Operating supplies cost = 15% of 3.3×106
= 0.495×106
Operating supplies cost = Rs. 0.495×106
Laboratory Charges: (10-20% of OL)
Consider the Laboratory charges = 15% of OL
Laboratory charges = 15% of 8.76×106
Laboratory charges = Rs. 1.34×106
Patent and Royalties: (0-6% of total product cost)
= 4% of total product cost
Patent and Royalties = 4% of 7.3×107
Patent and Royalties cost = Rs. 2.92×106
Thus, Direct Production Cost = Rs. 4.5×107 ----- (61.5% of TPC)

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Plant overhead Costs:
(50-70% of Operating labor, supervision, and maintenance or 5-15% of total product cost)

Includes for the following: General plant upkeep and overhead, payroll overhead, packaging,
medical services, safety and protection, restaurants, recreation, salvage, laboratories, and storage
facilities.
Consider the plant overhead cost = 60% of OL, DS & CL, and M & R Plant overhead cost
= 60% of ((8.76×106) + (3.3×106) + (1.05×106))
Plant overhead cost = Rs. 7.866×106
Thus, Manufacture cost = Direct production cost + Fixed charges + Plant overhead costs.
Manufacture cost = (4.5×107) + (11×106) + (7.866×106)

Manufacture cost = Rs. 5.4×107


General Expenses: Administrative costs + distribution and selling costs + research and
development costs
A. Administrative costs :( 2-6% of total product cost)
Consider the Administrative costs = 5% of total product cost
Administrative costs = Rs. 3.65×106
B.Distribution and Selling costs: (2-20% of total product cost); includes costs for sales offices,
salesmen, shipping, and advertising.
= 15% of total product cost
Distribution and selling costs = Rs.1.095×107
Research and Development costs: (about 5% of total product cost)
Research and Development costs = 5% of 7.3×107
Research and Development costs = Rs.3.65×106
Financing (interest): (0-10% of total capital investment)
Consider interest = 5% of total capital investment
= 5% of 7.5×107
Interest = Rs.3.75×107
Thus, General Expenses = Rs. 5.575×107
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Total Product cost: Manufacture cost + General Expenses

Total product cost = Rs. 10.975×107


Gross Earnings/Income:
Wholesale Selling Price of MEK per kg = Rs.40
Total Income = Selling price × Quantity of product manufactured

Total Income = Rs.13×107


Gross income = Total Income – Total Product Cost
= (13×107) – (10.975×107)

Gross Income = Rs. 2.025×107


Let the Tax rate be 45% (common)
Net Profit = Gross income - Taxes = Gross income× (1- Tax rate)
Net profit = 2.025×107 (1-0.45)

Net profit = Rs. 1.115×107


Rate of Return:
Rate of return = Net profit×100/Total Capital Investment
Rate of Return = 1.115×107 ×100/ (7.5×107)
Rate of Return = 14.85%
Payback period = TCI/Net profit
= 6.72 years

78
PIPING ANDINSTRUMENTATION

The main objective in the of the plant is to produce a particular product of given quality.
Instrumentation involves provision of controller to certain equipment’s to measure flow rate,
temperature, pressure etc. to maintain quality of the product.
The profit made by company also depend on the production cost. Therefore the purchase
instrumentation is justified because it gives product of uniform and better quality and makes the
operation uniform and smooth. Moreover, an efficiently controlled plant means high safety. In
chemical industry, this is a very important condition.
The most commonly encountered problem in chemical industry is the regulator type
problem, in which the set point is constant and we compensate the offset as rapidly as possible
without instability.
The function fulfilled by an instrument may be;
 Indicating
 Recording
 Controlling

AUTOMATION CONTROL:
Improvement in automatic instrumentation and control generally has lagged behind the
petroleum and petrochemical industry, probably because of more difficult measurement
requirements. However recent dramatic increases in feed stock, quality control and other cost
coupled with lower prices on computer have greatly increased the incentive for computer
controls.
Most plant eventually improves their control by installing conventional pneumatic and more
recently electronic controller on measure flow and temperature loops. This type of control is still
needed by most plants today.

FLOW CONTROL:
Flow control is usually associated with inventory contrary controlling storage or other equipment
to provide flow control on a compressor or pump running at a fixed speed and supplying a rear
constant volume output. A bypass control would be used .

INSTRUMENTATION AND CONTROL OBJECTIVES:


The following factors have been taken under consideration while preparing the process control
schemes:

79
1. Safe plant operation:
a) To keep the process variables within known safe operating limits.
b) To keep dangerous situation as they develop and to provide alarms to provide alarms
and automatic shutdown system.
c) To provide interlocks and alarms to prevent dangerous operating procedures.

2. Production rate:
To achieve the design product output.
3. Product quality:
To maintain the product composition within the specified quality standards.
4. Cost:
Operate at the lowest production cost, commensurate with the other objectives.
These are not separate objectives and have been considered together. The
order in which they are listed is not meant to imply the precedence of any objective
over another, other than that of putting safety first. Product quality, production rate
the cost of production rate cost of production will be dependent on sales
requirements.

COST ESTIMATION AND ECONOMICS


Paints and coatings continue to consume the majority of MEK.
Worldwide, approximately 44% of MEK was consumed for this application in 2014.
There will be little change in the world MEK market breakdown by 2019.
However, there are slight regional variations.
Although adhesives make up only 17% of the MEK market, this application will
experience the highest growth rate during 2014–19.
Historically, MEK capacity was concentrated in the three major regions (United
States, Western Europe, and Japan); these regions accounted for 75% of total MEK
Capacity in 2003. In 2014, the United States was no longer a producer and Western
Europe and Japan together accounted for about 43% of global MEK capacity. China
alone made up 38% of total world capacity in 2014
80
POLLUTION CONTROL AND SAFETY
SAFETY FOR METHYL ETHYL KETONE
Methyl ethyl ketone (MEK) is a clear, colorless, volatile, highly flammable liquid with an

acetone-like odour. It is stable under ordinary conditions but can form peroxides on prolonged

storage; these may be explosive.

 To maintain a safe working environment in the plant standard operating procedures will

be used in the plant.

 To develop awareness and provide knowledge about MEK, Secondary butyl alcohol,

Ethanol, Hydrogen and TCE, MSDS information boards, Information boards about health

and environment hazards/permissive working limits will be installed in the plant.

 Danger and toxic symbol plates will be mounted at critical work places.

 Flame and fire detectors will be installed to alert the workers in case of leakage or fire.

Fire extinguishers/Fire hydrants/Deluge system will be implemented at different locations

of the plant to fight the fire in case of accidents.

 Escape routes will be clearly mentioned in the plant.

 Installation of safety showers in the plant

0.1

This Indian Standard was adopted by the Bureau of Indian Standards on 17 August 1987, after
the draft finalized by the Chemical Hazards Sectional Committee had been approved by the
Chemical Division Council.
0.2

Methyl ethyl ketone is used as solvent for variety of resinous materials, such as vinyl films,
glyptal resins, adhesives, printing inks, lacquers, lubricant oil, refining and cleaning fluids. It is
used as a catalyst carrier, in vegetable oil extraction processes, in preparation of flavours,
antioxidants, perfumes, in the manufacture of n amyl ketone and methyl ethyl ketone peroxides.
81
0.3

In the preparation of this code, considerable assistance has been derived from the following
publications.

a. Dangerous Properties of Industrial Materials, third Edition, by N. Irving Sax, Reinhold


Publishing Corporation, 1957.
b. Material Safety Data Sheet (No. 303) Published by Materials Information Service,
General Electric Company USA 1979.
c. Manual for Handling and Disposal with Toxicity and Hazard Data. Published by
International Technical Information Institute, Japan, 1981.

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SCOPE

This standard describes properties of methyl ethyl ketone, the nature of hazards associated with it
and essential information on storage, handling, packing, labelling, disposal of waste, cleaning of
spillages, training of personnel, personal protective equipment and first aid.
This code, however, does not deal with the specifications for design of buildings, chemical
engineering plants, storage vessels and equipment for operations control.

TERMINOLOGY

For the purpose of this standard, the definitions given in IS : 4155-1966* and IS : 4167-1981†
shall apply.

PROPERTIES

General Information—Methyl ethyl ketone is a colourless, mobile, volatile liquid with acetone
type odour. It is flammable liquid with dangerous risk of fire and explosion, if not properly
handled.
Common Name—MEK
Chemical Name—Methyl ethyl ketone, 2-butanone
EmpiricalFormula—C4H8O

Structural formula—
Molecular Weight—72·12

Physical Properties

1) Description, Colour, Odour, Physical State—Methyl ethyl ketone is a colourless,


transparent liquid with acetone like odour. The technical grade may have slight yellowish
tinge.
2) Boiling Point (at 1 atm)—80°C
3) Specific Gravity—(20/20°C)—0·806
4) Vapour Pressure (at 25°C)—100 mm of mercury
5) Miscibility / Solubility in Common Solvents—It is soluble in water and miscible with
ethanol and ether.
6) Vapour Density—2·41

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Chemical Properties

Reactivity—Methyl ethyl ketone, with a strong oxidizing agent, can cause spontaneous ignition
and violent reaction. Its oxidation in air can give oxides of carbon and nitrogen. Direct
oxidationcan lead to peroxide formation. It undergoes reactions typical of carbonyl groups. It
condenses with variety of reagents. Methyl ethyl ketone reacts violently with certain transition
metal oxides, for example, chromium oxide.‘Methyl ethyl ketone reacts with oxidizing agents,
strong acids mixtures of strong bases and chlorinated solvents and potassium t-butoxide’

1) Stability at High Temperature


2) Autoignition temperature = 516°C
3) Light Sensitivity—No

Fire and Explosion Hazard Properties

1) Flash Point (Closed-up)—(–) 6·7°C


2) Flammability—Lower flammable limit in air 1·8 percent by volume and upper
flammable limit in air 10·0 percent by volume. Classified as flammable.

Corrosion Properties—It has no corrosion properties.

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HEALTH EFFECTS AND TOXICITY INFORMATION
General

1) PEL (TLV)—200 ppm (590 mg/m3)


2) TDL Oral—LD50 : 3400 mg/kg
3) STEL—300 ppm (885 mg/m3)

Health Effects

1) Methyl ethyl ketone is neither highly toxic nor it exhibits cumulative toxological
properties. It is slightly more toxic than acetone. Inhalation of vapours over prolonged
periods may irritate the mucous membrane and cause nausea and eventually loss of
consciousness.
2) Eyes—Eye contact causes irritation and burning sensation of the eyelids.
3) Ingestion—Ingestion causes irritation to the digestive tract. Larger quantities (25 g) can
cause narcosis.
4) Skin Contact—It can be absorbed through skin which defats and irritates the skin. When
methyl ethyl ketone is mixed with normal hexane, it causes synergistics effect.
5) Medical Monitoring—Provide regular medical monitoring, including blood cell count of
those exposed to in a material in the work place.

PERSONAL PROTECTIVE EQUIPMENT

Personal protective equipment should include general purpose breathing apparatus, rubber gloves
and protective clothing to avoid contact with liquid. Safety goggles or face shields should be
used to prevent splashing of the liquid into the eyes.

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STORAGE, HANDLING, LABELLING AND TRANSPORTATION

6) Storage—Storage under roof is preferable in all seasons. The drums should be tightly
closed and should not be exposed to sources of heat such as walls of boiler room and
kitchen. Storage place should be well ventilated and provided with fire-proof electrical
fittings and spark resistant tools. Do not store methyl ethyl ketone near strong oxidizing
agents. ‘NO SMOKING’ sign should be displayed in the storage area.
7) Handling—Wear neoprene rubber gloves, protective clothing and face shield while
handling this material. Use general purpose breathing apparatus.

Labelling

Use of hazard warning symbols/labels in plant area are recomended;

Cautionary and warning notice may also be displayed:

1) NO SMOKING
2) NO NAKED FLAME
3) AVOID SPILLAGE

SPILLAGE/LEAKAGE AND WASTE DISPOSAL


Spills and Leakages
If spills and leaks occur, shut off all sources of ignition or remove them from the area as early as
possible. Only persons provided with adequate personal protective equipment should remain in
the area.Spills, unless very large, should be absorbed on paper or other absorbent material.Scrape
up with a non-sparking scoop and place in a covered metal container for disposal. Those
involved in clean up should use protective equipment. Dispose of the scrap by burning in a
remote open pit or depositing in a sanitary land-fill. Do not dump the material down the
sewer.Material from a leaky container should be carefully transferred to another suitable
container. During such transfer, all sources of ignition must be kept away from the area.In the
event of a leak in a tank car which cannot be readily repaired by simple adjustments or tightening
of the fittings, the supplier should be telephoned or wired immediately for instructions. The area
around the tanker should be evacuated and only properly protected personnel should be allowed
to enter the area.Clothings wet with methyl ethyl ketone should be removed immediately and
body washed with soap and water. The clothing should not be used again until thoroughly
cleaned and dry.

86
Waste Disposal

All relevant regulations of local and State Authorities for prevention and control of pollution
should be observed.Water contaminated with methyl ethyl ketone should be sent for effluent
treatment before discharging to the river or creek.Best way to dispose of the methyl ethyl ketone
waste is by incineration in a furnace.

FIRE PREVENTION AND FIRE FIGHTING

Preventing Fire Hazard—Fire can be prevented if the material is kept away from heat or flame.
The fire hazard can also be avoided bypreventing mixing of oxidizing materials with methyl
ethyl ketone and using non-sparking tools near this solvent.

Fire:
Fire can be prevented to a large extent by employees through basic knowledge and
understanding about characteristic and behavior of Fires. With this awareness, effective actions
can be taken to prevent the combination of events which result in the fire. Hence ,it is essential to
explain basic chemistry of fire, Types of fire and fundamental fire/explosion prevention, fire con
troll/extinguishments etc.

What is fire ?
Fire is a chemical reaction, in which substance (fuel) combines with oxygen. The reaction is
exothermic and usually associated with emission of light and smoke.
Oxygen + heat + fuel = FIRE
Remove any one = NO FIRE.

Types of Extinguishers to be Used—Foam dry chemical powder and carbon dioxide can be
used to extinguish the flame. Water spray is ineffective for extinguishing, but may be used to
keep fire exposed containers cool.

87
TRAINING AND HEALTH MONITORING

Training and Education—Persons handling or working on plant involving methyl ethyl ketone
shall have training such that they can be expected to carry out their jobs effectively and safely.
They should be familiar with accepted method of handling and should be appraised of the use of
protective equipment for safe handling. During instructions, stress should be given that persons
know the hazards due to eye contacts, skin contacts, inhalations and ingestion. All persons
should be familiar with the location of alarm boxes, first-aid boxes, fire extinguishers and
personal protective equipment including the use of breathing apparatus.Safety In handling
methyl ethyl ketone depends, to a great extent, upon the effectiveness of employees education,
proper safety instructions, intelligent supervision and the use of safe equipment.

Health Monitoring

Pre-employment Medical Examination—This is required for employees who would be


exposed to methyl ethyl ketone. Preclude from exposure those individuals with diseases of the
skin, blood and central nervous system.‘In addition to the pre-placement medical examination
annual regular medical examination should be carried out.’

FIRST AID

1) Inhalation—Remove victim to fresh air. If required, use artificial respiration to restore


breathing. Get immediate medical attention.
2) Skin Contact—Wash area of contact with soap and water. Clothing wetted with methyl
ethyl ketone should be immediately removed. If irritation persists, get medical attention.
3) Eye Contact—Immediately wash with plenty of water including under the eyelids. If
irritation persists, get medical attention.
4) Ingestion—If victim is conscious, give 3 glasses of water or milk and induce vomitting.
Get medical attention as soon as possible.

Caution: Nothing should be given by mouth to an unconscious patient.

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CONCLUSION

Thus the project based on manufacturing of MEK 5000 tons per year includes.
1) Material balance

2) Energy balance

3) Factor for selecting the process

4) Design of equipment such as

a) Condenser

b) Absorption

5) Cost estimation

In carrying out this project we applied


a. Chemical process calculation

b. Process equipment and design concepts

c. Application of heat and mass balance principle

d. Economic

Thus the project covers all aspects required for the manufacturing of MEK and Could be
implemented in reality.

PLANT LAYOUT

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