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MANUFACTURE OF METHYL ETHYL KETONE

CAPACITY: 500 Metric Tonnes per day

Project Report Submitted in Partial Fulfillment of the Requirements for the Degree of B.E. (Chemical)

2019

MANUFACTURE OF METHYL ETHYL KETONE CAPACITY: 500 Metric Tonnes per day Project Report Submitted in Partial

By

NAVDEEP KUMAR

CH15156

Dr. S. S. BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING & TECHNOLOGY

PANJAB UNIVERSITY CHANDIGARH 160014, INDIA

Dr. S. S. BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING & TECHNOLOGY PANJAB UNIVERSITY CHANDIGARH 160 014, INDIA

Dr. S. S. BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING & TECHNOLOGY PANJAB UNIVERSITY CHANDIGARH – 160

CERTIFICATE

This is to certify that the project entitled “MANUFACTURE OF METHYL ETHYL KETONE (CAPACITY: 500 TPD)” carried out by Mr. NAVDEEP KUAMR, CH15156 of final year B.E Chemical Engineering during the year 2018-19 is a bonafide work submitted to the Dr. S. S. Bhatnagar University Institute of Chemical and Technology, Panjab University, Chandigarh in partial fulfillment of requirements for the award of degree of Bachelor of Engineering in Chemical Engineering.

PROF. MEENAKSHI GOYAL Dr.SSB UICET PANJAB UNIVERSITY CHANDIGARH

Acknowledgement

I take this opportunity to express my profound gratitude and deep regards to Prof. Meenakshi Goyal for her exemplary guidance, monitoring and constant encouragement throughout the course of this project. The blessing, help and guidance given by her time to time shall carry me a long way in the journey of life.

I also take this opportunity to express a deep sense of gratitude to Prof. Sanchita Chauhan (Chairperson, Dr.SSBUICET) for her cordial support, valuable information and guidance, which helped me in completing the project.

Lastly, I am also thankful to all staff members of the department without whose help my project would not have been a successful one.

NAVDEEP KUMAR

1. INTRODUCTION

1.1 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:

O

R --- C --- 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 unsymmetric or mixed aliphatic ketone. It’s IUPAC name is 2-butanone. 2-Butanone ,methyl ethyl ketone, MEK, is the 2 nd link in the homologous series of aliphatic ketones and next to acetone, the most important commercially produced ketone. It is commercially produced by dehydrogenation of the secondary butyl alcohol. It is analogus to the production of actone by dehydrogenation of isopropyl alcohol on copper or zinc or bronze catalyst at 400 500 0 C. At 80-95% sec butylalcohol conversion, MEK selectivity 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 known as 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 the preparation of paints and lacquers.

Interest in MEK as a solvent for paints and adhesives has been growing in recent years. 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 selective extractant, as a special solvent for dewaxing mineral oil fractions and as a chemical intermediate.

1.2 USES:-

More than half the MEK produced in the United States finds application in surface coatings end uses. Significant volumes are also used in the production of adhesives, magnetic tapes, printing inks, solvent extraction, cleaning fluids, dewaxing agents, and dyes. In surface coatings MEK is widely used as a component in vinyl lacquer solvent systems. Its active solvency for vinyl acetate and vinyl chloride vinyl acetate copolymers makes it possible to formulate high solids lacquers containing large amounts of economical hydrocarbon diluents. In addition, it is a strong, active solvent for nitrocellulose and is extensively used in furniture and automotive lacquers. The low specific gravity of MEK enables formulators to produce larger volumes of base lacquers or thinners per pound than is possible with heavier solvents. MEK is also a coatings solvent 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 in placing air pollution regulated solvents, such as toluene, which are frequently used in these alkyd formulations.

MEK is a dewaxing agent in the refining of lubricating oils and is a solvent for adhesives, rubber, cement, printing inks, paint removers and cleaning solutions. It is used in vegetable oil extraction process and in azeotropic separation schemes in refinery. 1.3 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% Chemical industry, pharmaceutical industry 13% Adhesives 11% Miscellaneous 16% 1.4 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 MEK causes skin moisture loss and slight irritation .Sensitive persons may develop demitasses .Liquid MEK temporarily irritates eyes and corneas .MEK is usually absorbed through the 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 scendesmus quadricanda 120 mg / lit

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

2. PHYSICAL AND CHEMICAL PROPERTIES OF MEK

2.1 PHYSICAL PROPERTIES:-

MEK is a low boiling solvent with an atmospheric boiling point of 175.3 0 F (79.6 0 C). 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 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. It is highly miscible with water and many conventional organic solvents and forms azeotrope with number of organic solvents.

Some of the physical properties are listed below.

Physical Properties of MEK (all values are at 20 0 c, except where noted)

Boiling point at 1 atm, 0 C

79.6

Azeotrope with water , bp, 0 C

73.4

Wt.% ketone in vapor

88.7

Autoignition temperature, 0 C

515.6

Coefficient of cubic expansion, per 0 C

0.00119

Critical pressure, atm

43

Critical temperature , 0 C

260

Density, g/mL at 20 0 C

0.8037

Dielectric constant

18.51

Dipole moment, debye units

2.74

Electrical conductivity, mho

5.0 x 10 -8

Explosive limits in air, vol.% Upper

10

Lower

1.8

Flash point, 0 C Tag open Cup

1.11

Tag Closed Cup

-2.22

Freezing point, 0 C

-86.3

Heat of combustion, cal/g

8084

Heat of fusion, cal/g

24.7

Heat of vaporization, cal/g

106

Molecular weight

72.104

Refractive index nD

1.3791

Solubility, wt. % Ketone in water

26.3

Water in ketone

11.8

Solubility parameter

9.3

Specific heat, cal/g 0 C

0.549

Surface tension, dyn/cm

24.6

Thermal conductivity, cal/cm 2 .s. ( 0 C/cm)

3.58 x 10 -4

Vapor pressure, mmHg

80.21

Viscosity, cP

0.43

2.2 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 readily dehydrates to an unsaturated ketone:

O

CH3

O

2CH3CCH2CH3 CH3CH2CCH2CCH2CH3 OH CH3 O
2CH3CCH2CH3
CH3CH2CCH2CCH2CH3
OH
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 of MEK with aliphatic esters. MEK condenses with glycols and organic oxides to give derivatives of dioxolane. sec-Butyl amine is formed by reacting MEK with aqueous ammonia and hydrogen:

O

NH2

CH3

CCH2CH3 + NH3 + H2

Ni
Ni

CH3 CHCH2CH3 + 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

Thermal conductivity, cal/cm .s. ( C/cm) 3.58 x 10 Vapor pressure, mmH g Viscosity, cP 0.43

CH3CCH2 +HC CH CH3CH2CC CH

OH

Miscellaneous Reactions

Oxidation of MEK with oxygen produces diacetyl, a flavouring material. Chlorination yields mixtures of several monochloro and dichloro derivatives in various percentages depending on reaction conditions. The reaction of MEK with hydrogen peroxide gives a mixture of peroxides and hydro peroxides which is used to cure polyester resins at room temperature:

O

OH

CH3CCH2CH3 + H2O2

CH 3 CCH 2 CH 3 + H 2 O 2 CH 3 CCH 2 CH

CH3CCH2CH3

 

OOH

This initial addition product is the unstable precursor of seven stable peroxides and hydro peroxides. Of these, 2,2 dihydroperoxy-2,2’-dibutyl peroxide is present in the largest amount (about 45%) in the peroxide mixture:

CH3

CH 3

HOOC OO - COOH

C2H5

C2H5

MEK peroxides are widely used as catalysts for the polymerisation of polyester resins at room temperature. The condensation product of MEK and m-phenyl diamine is an efficient curing agent for epoxy resins. MEK and cobalt acetate function together as a specific catalyst for single-stage oxidation of p-xylene to terephthalic acid. Aliphatic monoketones, such as MEK also function as catalysts in the polymerisation of polyethylene terephthalate where, it is claimed, they speed condensation times and cause less yellowing of the polymer than antimony trioxide. MEK is also used in the preparation of complex catalysts used in the syndiotacic polymerisation of α- olefins such as propylene.

Phenol, glyoxal, formaldehyde, acetaldehyde, furfuraldehyde, and other chemicals can 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 upon hydrogenation produces amines.

3. PROCESS SELECTION AND DETAILS

3.1 PROCESSES AVAILABLE:

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 of 2-butanol is an exothermic reaction (51 KJ/Kgmol). The reaction is as follows.

OH

CH3 CH C2H5

3. PROCESS SELECTION AND DETAILS 3.1 PROCESSES AVAILABLE: There are a few processes listed below for

O

CH3 C C2H5

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

log Kp = -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 at

approximately 350 0 C. Copper, Zinc or Bronze are used as catalysts in gas phase dehydrogenation. Commercially used catalysts are reactivated by oxidation, after 3 to 6 months use. They have a life expectance of several years.

Sec-butyl alcohol is dehydrogenated in a multiple tube reactor, the reaction heat being supplied by heat transfer oil. The reaction products leave the reactor as gas and are split into crude MEK and hydrogen on cooling. The hydrogen is purified by further cooling. The crude MEK is separated from uncreated reactants and by-products by distillation.

LIQUID PHASE OXIDATION OF BUTANE:

MEK is produced as a by-product in the liquid phase oxidation of n-butane to acetic acid. Autoxidation of n-butane of n-butane takes place in the liquid phase according to the radical mechanism yielding MEK as an intermediate and acetic acid as end product. MEK and acetic acid (mass ratio 0.2 : 1.0) are obtained by non-catalyzed

liquid phase oxidation at 180 0 C and 53 bars with remixing. Continuous oxidation under

plug flow conditions at 150 0 C, 65 bars and a residence time of 2- 7 minutes forms MEK and acetic acid at a mass ratio of 3:1. this process has slight economic advantage over the dehydrogenation 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 is transferred in a homogenous phase on to n-butanes using redox salt pair, PdCl2 / CuCl2. O

LIQUID PHASE OXIDATION OF BUTANE : MEK is produced as a by-product in the liquid phase

n C4 H8 + ½ O2 CH3 C 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 b- butryaldehyde and corrosion caused due to free acids.

DIRECT OXIDATION N-BUTENES, MARUZEN PROCESS:

The Maruzen process is similar to the Hoechst-Wacker process except that oxygen is transferred by an aqueous solution of palladium sulfate and ferric sulfate. This method is attractive commercial route to get MEK via direct oxidation of n-butenes, but it is patented and very less information is available about this process. This process is generally not accepted due to formation of undesirable by products.

3.2 PROCESS SELECTION:

Commercially, MEK is predominantly produced by the catalytic dehydrogenatio of SBA in vapor phase over ZnO or Brass catalyst. It can, however be produced by the selective 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-butanol

can be easily produced by the hydration of n-butenes(from petrochemically produced C4 raffinates). The remaining MEK is produced by process in which liquid butane is catalytically cracked giving both acetic acid and MEK.

The vapor 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.

MEK is produced as by product from liquid phase oxidation of n-butenes to acetic 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 more advantages and is more economical compared to other processes, so this process has been selected for design in following text.

3.3 PROCESS DETAILS:

The cold feed of 2-butanol will be pumped from the feed tank to a steam heater to a vertical thermosyphon vaporizer in which alcohol is vaporized. The thermosyphon vaporizer will be heated by reaction products discharged from the reactor. The wet alcohol vapor will be passed to a knock out drum to remove any entrained liquid. The liquid separated will be recycled and the dry alcohol will be fed to the reactor via super heaters heated by flue gas. The super heaters will be designed to raise the temperature of

alcohol vapors to 500 0 C at which temperature the vapors enter the reactor.

The dehydrogenation reaction of SBA is as shown

O H

CH2 CH C2H5

The vapor phase dehydrogenation process gives high conversion of 2-butanol and high selectivity of MEK of
 

O

H2C C

C2H5

+

H2

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

400 0 C will be passed on to the thermosyphon vaporizer in order to initiate the preheating of alcohol reactor feed. The reaction products will be cooled to near saturation in the

vaporizer so that they will enter the water condenser at 150 0 C. There about 80% MEK and alcohol will be condensed and sent to the storage while the remainder will leave this unit as saturated vapor in non-condensable hydrogen.

This vapor will be fed to the bottom of the packed bed absorption column where MEK and 2-butanol will be absorbed in water. The water will be recycled from the extraction column and its rate will be controlled to provide an aqueous effluent containing 10% MEK. The hydrogen discharged from the top of the absorber will be dried and fed to the furnace.

The aqueous effluent from the absorber will be pumped into an extraction column where it will be contacted with 1,1,2-Trichlorethane to extract MEK and alcohol. In excess of about 95% of the MEK and alcohol will be extracted and remainder will be recirculated back to the absorber.

The trichloroethane extract phase will be pumped to a distillation unit for the separation unit for the separation of solvent, which is recycled. The distillate from this column will be MEK and alcohol, which will be, mixed liquid product form the condenser and this will be treated in a MEK product still for the purification of MEK. The alcohol discharged from the bottom of this column will be replaced back to alcohol feed tank. The MEK product will be cooled and stored.

4. MATERIAL BALANCE

The alcohol balance over each unit will be based on hourly production rate. For a

production rate of 500 TPD of MEK, the hourly production rate will be

=500 x 10 3 /24 kg/hr

=20833.33 kg/hr

However allowing for 8 % spillage and other losses, the hourly production rate will be

= 1.08 x 20833.33 kg/ hr

=22500.00 kg/hr

Material balance is done over the whole process. In this diagram most of the inner processes are

shown in the BLOCK.

Alcohol = 99 % MEK = 0.92% TCE = 0.08% Alcohol Recycle XR1 BLOCK MEK X
Alcohol = 99 %
MEK = 0.92%
TCE = 0.08%
Alcohol Recycle
XR1
BLOCK
MEK
X
Reactor
Prod
still
MEK = 100%
2
1

X = Pure alcohol feed, kg/Hr

R1 = Recycle ratio

MATERIAL BALANCE ACROSS THE REACTOR:-

Total feed of alcohol to reactor = X + 0.99XR1 = X (1+099R1)

For 89.1% conversion MEK produced,

= X(1 + 0.99R1 )x 0.891

74

x 72 Kg MEK

Total MEK from reactor = X (1 + 0.99 R1) x 0.891x72 + 0.0092 XR1 kg

74

The overall conversion = 98.5886%

MEK at final stream(2) =

X x 0.985886x72 kg

74

Hydrogen produced due to dehydrogenation reaction

= X (1 + 0.99 R1) x 0.891 x 2 kg. 74

H2 produced are all coming out in the stream (1) is 68.49 wt % .

Total quantity of hydrogen at stream (1) = X ( 1 + 0.99 R1 ) x 0.891x2 kg/hr 74 x 0.6849

MEK in stream (1)

=

X( 1 + 0.99R1 ) x 0.891 x2 74 x 0.6849

x 0.0822 kg

MEK Balance: -

(MEK from reactor) = (MEK at recycle)

+ (MEK at stream (1))

+(MEK at stream (2))

X(1 + 0.99R1) x 0.891 x 72 +0.0092 XR1= 0.0092 XR1 + X x 0.985886 x 72

74

74

+

(1 + 0.99R1 ) x 0.891 x 2

x 0.0822

74 x 0.6849

(1 + 0.99 R1) (0.8669 2.8902 x 10 -3 ) = 0.9592 (1 + 0.99 R1) = 1.1102 R1 = 0.1102 = 0.1113

0.99

MATERIAL BALANCE ACROSS THE CONDENSER:-

Amount of feed to condenser = X (1 + R1 ) kg/hr

MEK = X(1 + 0.99 R1) 0.891 x 72 + 0.0092XR1 kg

74

Alcohol = X( 1 + 0.99 R1) x 0.109 kg

H2

= X( 1 + 0.99 R1) x 0.891 x 2 kg

74

Alcohol =12.04 % L MEK = 87.96% F V Condenser Alcohol=10.9% MEK= 86.70% Alcohol = 5.38%
Alcohol =12.04 %
L
MEK = 87.96%
F
V
Condenser
Alcohol=10.9%
MEK= 86.70%
Alcohol = 5.38%
MEK = 80.72%
H2 =13.90%
H2=2.41%

F= Feed L= Condensate from condenser V= Vapor from the condenser

Overall material balance

F = L + V

Component balance

(Alcohol)Feed = L(0.1204) + V( 0.0538)

(Alcohol)Feed = F(0.1204) + V(0.0538 0.1204) X(1 + 0.994R1) x 0.109 = X ( 1 + R1 ) (0.1204) + V(0.0538 0.1204) 0.1210X = 0.1338X 0.0666V.

V = 0.19204X L

= X( 1 + R1) V

L = 1.1113X 0.19204

= > L = 0.9193X

F = 1.1113X L = 0.9193X V = 0.19204X

MATERIAL BALANCE ACROSS THE ABSORPTION COLUMN:-

VR2 Absorption Column V Alcohol = 5.38% MEK = 80.72% H2 = 13.9% K M Alcohol
VR2
Absorption
Column
V
Alcohol = 5.38%
MEK = 80.72%
H2 = 13.9%
K
M
Alcohol = 0.92%
MEK= 8.22%
H2 = 88.49%
Water = 22.37%

Alcohol = 0% MEK = 0.5% Water = 99.5%

Alcohol = 0.65% MEK = 10.32% water = 89.05%

V

= Vapor from condenser.

VR2 = Absorber feed.

M

= Vapor from absorber.

K = Absorber effluent.

Overall material balance

V

+ VR2 = K+M

Alcohol balance

V

x (0.0538) + 0 = K (0.0065) + M (0.0092) (2)

H2 balance

 

(V x 0.139) + 0 = 0 + M (0.6849)

M

=

0.139

 

0.6849 V

M

= 0.20294 V

M

= (0.20294) (0.19204X)

M

= 0.039X

Alcohol balance

K (0.0065) = (0.19204X) (0.0538) (0.039X) (0.0092)

K= 1.5343X

From (1)

VR2 = K + M - V = 1.5343X+0.039X-

0.19204X VR2 = 1.38126X

R2 =

1.38126X

 

0.19204X

 

R2 = 7.19256

 

V

= 0.19204X kg/hr.

VR2 = 0.19204 x 7.19256 = 1.38126X kg/hr

K

= 1.5343X kg/hr

M

= 0.039X kg/hr

MATERIAL BALANCE ACROSS THE EXTRACTION COLUMN:-

VR2 Alcohol = 0.0% MEK=0.5% Water=99.5% N Extraction Alcohol = 1.24% column K MEK = 19.00%
VR2
Alcohol = 0.0%
MEK=0.5%
Water=99.5%
N
Extraction
Alcohol = 1.24%
column
K
MEK
= 19.00%
Alcohol =0.65%
TCE = 79.62%
Water = 0.14%
MEK=10.32%
Water=99.5%
C
Alcohol= 0%
MEK=0.14%
TCE=0.99.69%

Water =0.17%

N = Extract

C

= Solvent

K + C = N + VR2

Alcohol balance

 

=>

C

= N + VR2 K

=> C = 0.65123X

N = 0.80427 X kg.

C

= 0.65123 X kg.

L

Alcohol = 12.04% MEK = 87.96%

Overall material balance,

K x 0.0065 + 0 = N x 0.0124 + 0

0.0124

= > N = (1.5343X)

0.0065

N = 0.80427X

From overall mass balance,

=> C = 0.80427X + 1.38126X 1.5343X

MATERIAL BALANCE ACROSS THE SOLVENT RECOVERY UNIT:-

D Solvent Recovery Still
D
Solvent
Recovery
Still

N Alcohol = 1.24% MEK = 19.00% TCE = 79.62% Water = 0.14%

Alcohol = 11.17% MEK = 88.82% TCE = 0.01%

MEK = 0.14% TCE = 99.69%

C

Water = 0.17%

= Condensate from condensate.

L

D

N + L = D + C

D

= N + L C

D

D

= 1.07234X

D Alcohol = 11.17% MEK = 88.82% TCE = 0.01%

P = MEK product

D

= P + XR1

= MEK still feed.

Overall material balance

= 0.80427X + 0.9193X 0.65123X

MATERIAL BALANCE ACROSS THE MEK PRODUCT STILL:-

XR1 MEK Prod still P
XR1
MEK
Prod
still
P

Alcohol =12.04 % MEK = 87.96%

Alcohol = 1.00% MEK = 99.00%

XR1 = Alcohol recycle

Overall material balance

=> 1.07234X = P + 0.1113X

=> P + 1.07234X 0.1113X

=> P = 0.96104X

P = 22500 kg/Hr

(0.96104X) = P = 22500.00 X = 22500

0.96104

X = 23412.13685 kg/Hr

Fresh feed of alcohol required = 23412.13685 kg/hr.

Putting the values of X we get all the flow conditions of all the streams. The material balance is shown in the flowsheet in the next page.

5.FLOWSHEET

Feed Liq. from condenser Absorber feed Absorber Effluent MEK Still Feed Alcohol Recycle Wt. % Wt.
Feed
Liq. from condenser
Absorber feed
Absorber Effluent
MEK Still Feed
Alcohol Recycle
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Alcohol
23412.136 100.00
2591.342
12.04
--
-- 233.488
0.65 2804.315
11.17
99.00
MEK
--
--
18931.435
87.96
161.691
0.5 3707.072
10.32
22298.946
88.82
23.9731
0.92
Hydrogen
--
--
--
--
-- --
--
--
--
-- --
--
TCE
--
--
--
-- --
--
-- --
2.5098 0.01
2.0846 0.08
Water
--
-- --
-- 32176.557
99.5
31980.681
89.05
--
-- --
--
Total
23412.136 100.00
21522.777
100.00 32338.248
100.00
35921.241
100.00 25105.770
100.00
2605.77
100.00
B
C
D
E
F
ReRrr
A
Vapour From
Reaction Products
Vapour From
Solvent
Extract
MEK Product
Absorber
Condenser
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Wt.
%
Alcohol
8.391 0.92
2834.24
10.89
241.838
5.38
--
-- 233.488
1.24
225.00 1.00
MEK
74.977 8.22
22556.739
86.70
3626.371 80.72
21.345
0.14 3577.639
19.00
22275.00
99.00
Hydrogen
624.722
68.49
626.921
2.41 626.921
13.90
--
-- --
-- --
--
TCE
-- --
--
--
--
--
15199.421
99.69 14992.191
79.62
--
--
Water
204.045
22.37
--
-- --
-- 25.919
0.17 26.361
0.14
--
--
Total
912.136
100.00 26017.907
100.00 4495.130
100.00
15246.685
100.00 18829.679
100.00
22500.00
100.00

A = REACTOR B = CONDENSER C = ABSORPTION COLUMN

D = EXTRACTION COLUMN E = SOLVENT RECOVERYCOLUMN F = MEK PRODUCT STILL

21

6. ENERGY BALANCE

Basis:- 1 Hr. Operation

ENERGY BALANCES ACROSS THE FEED PREHEATING EQUIPMENT:-

The heating of cold 2-butanol feed is to be completed in three stages in order to avoid large heat losses. The cold feed is first preheated to its boiling point using steam as heating medium and then vaporized in a thermosyphon reboiler utilizing the heat contained in the reaction products. The vapor, which has entrained liquid is removed from the knock out drum, and then heated to reaction temperature using flue gas.

COLD FEED PREHEATER:-

Total feed = 23412.14+2605.77 kg

= 26017.91 kg 26017.91 kg per hour of 2-butanol is to be preheated from 25 0 C it boiling point 107.5 0 C.

Heat load on preheater,

Q = 26017.91 x 1.497(380.5 288)

= 3.603 x 10 6 KJ The heating medium is used is dry saturated steam at 420K

Steam requirement = 3.603 x 10 6

2123.4

= 1696.8 kg/hr

2-BUTANOL VAPORIZER:-

2-butanol feed is vaporized at 107.5 0 C using reaction products.

Heat load on vaporizer is , Q = M x  = 26017.91 x 557.43 kj

= 14.5032 x 10 6 kj/hr Average Cp of reaction products = 2.3 KJ / Kg 0 k

14.5032 x 10 6 = 26017.91 x 2.304 (642 T)

T = 400 K

FIRST SUPER HEATER:-

2-butanol vapors is to be heat4ed from 380.5 k to 573k . using flue gas which enters at 673 k & cools to 423k.

Cp = 2.038 kj/kg k.

Heat load on super heater, Q = M x Cp x (T2 T1) = 26017.91 x 2.038 (573 380.5)

Q = 10.207 x 10 6 kj/hr

Mass flow rate of flue gas =

10.2072 x 10 6

1.2 x ( 673-423) = 3.4024 x 10 4 kg/hr

SECOND SUPER HEATER:-

It raises the temperature of vapor from 573 to 773 k . using flue gas which enters at 873k abd cools to 623k

Cp = 2.674 kj/kg k

Heat load on super heater Q = M x Cp x (T2 T1) = 26017.91 x 2.674 (773 573)

Flue gas requirement,

= 13.9144 x 10 6 kj/hr

=

13.9144 x 10 6

1.195 x (873- 623) = 4.6575 x 10 3 kg/hr

ENERGY BALANCE ACROSS THE REACTOR:-

The feed enters the reactor at 773k and leaves at 663k. The conversion obtained in the reactor is 89.1%. The heat balance includes two terms i.e , sensible heat change due to cooling of reaction mixture and heat consume due to reaction.

Q = M x Cp x(T2 T1) + M x H

Mean Cp = 2.68 kj/kg k

H = 73900 kj/kgmol

Total 2-butanol feed = 23412.14 + 2579.71 kg = 25991.85 kg/hr = 351.24 kmol/hr

Q = 26017.91 x 2.68 x (663- 773) + 351.24 x .891 x 73900 = 15.457 x 10 6

It is assume that a flue gas is available at 800k & leaving 750k.

Cp = 1.195 kj/kg k

Flue gas requirement,

15.457 x 10 6

= 1.195 x (800-750) = 25.869 x 10 4 kg/hr

ENERGY BALANCE ACROSS THE CONDENSER :-

The vapor enters condenser at 127 0 C (400k) at 1 bar pressure. Liquid and the vapor leaving the condenser is in equilibrium. At the more mole fraction x = 0.88 of the condensate we get both liquid and vapor temperature from the T- x- y diagram and temperature are

299.6 k. = liquid temperature., 335.7 k = vapor temperature

We take cooling water enters at 24 0 C and leaving at 42 0 C

CpH2 = 14650 J/ kg k Cpalcohol = 1760 J/ kg k CpMEK = 1664 J/ kg k

Cpmix = 0.867 x 1664 + 0.1089 x 1760 + 0.0241 x 14650 = 1987.42 J/kg. Heat loss to reduction in vapor temperature from 400k to 335.7k Q1= 26017.91 x 1.98742 (400- 335.7)

= 3.325 x 10 6 kj/ hr

Heat loss due to condensation Q2 = 2591.34 x 689.19 + 18931.44 x 486.11

= 10.989 x 10 6 kj/hr

Heat loss due to further cooling of a part of vapor is Q3 = 21522.78 x 1.987 x (335.7 299.6)

= 1.544 x 10 6 kj/hr

Total heat lost = Q = Q1 + Q2 + Q3 = (3.325 + 10.989 + 1.544) x 10 6 kj/hr

= 15.858 x 10 6 kj/hr

Mass flow of cooling water

=

15.858 x 10 6

4.187 x (42- 24)

=

2.104 x 10 5 kg / hr

ENERGY BALANCE ACROSS THE ABSORBER :-

Heat of condensation of MEK

= 3707.072 x 443.14

= 1.643 x 10 6

kj/hr

Heat of condensation of alcohol is = 233.488 x 560 = 0.1308 x 10 6 kj/hr

Heat of solution

= (3707.072 + 233.488) x 0.35 = 0.001379 x 10 6 kj/hr

Heat loss in cooling gasses from 62.7 to 27 0 C = (74.98 x 1.47 + 8.392 x 1.53 + 624.723 x 14.65) (62.7

27)

= 0.3311 x 10 6 kj/hr

Total heat released = 2.1063 x 10 6 kj/hr

Heat removed by water vapor = (204.045 x 2437.9) = 0.49744 x 10 6 kj/hr Heat gained by irrigating liquor

  • a) Water: 31980.6816 x 4.186 (T 300)

  • b) MEK: 3707.072 x 2.299 x ( T-300 )

  • c) Alcohol: 233.488 x 2.429 x (T- 300 )

Total heat gained = 0.49744 x 10 6 + 0.142961 x 10 6 (T-

300)kj/hr

Heat released = heat gained

= >

2.1063 x 10 6 = 0.49744x 10 6 + 0.14296 x 10 6 (T 300)

= >

T = 311.25 k

ENERGY BALANCE ACROSS THE EXTRACTION COLUMN:-

It is assume that the extraction process is isothermal. All that streams come at 27 0 C and leaves at 27 0 C.

ENERGY BALANCE ACROSS THE SOLVENT RECOVERY & UNIT:-

Feed is not saturated liquid it is sub-cool liquid. Saturation temperature is 93 0 C From x-y diagram we get Rm = 0.38.

R= 2Rm = 0.76

Feed:

Alcohol = 233.48 = 3.155 kmol /hr

 

74

MEK =

3577.639 = 49.689 kmol/hr

72

TCE =

14992.191 = 112.3kmol/hr

133.5

Water =

26.3613 = 1.465 kmol /hr

18

Total = 166.609 kmol /hr

Mole fraction of MEK

XMEK =

49.689 = 0.2982

166.609

Feed temperature = 27 0 C

F . HF =3.155 x170.058 (27- 0) + 49.689x165.726 x 27+112.3 x148.56x27 + 1.465x75.36

x27

F . HF = 0.69025 x 10 6 kj/hr

Distillate:-

Alcohol = 233.488 = 3.1552 kmol /hr

74

MEK = (3577.639 21.3454 ) = 49.39 kmol/hr

72

Water = (26.3613 25.9195) = 0.0246 kmol /hr

18

TCE = 2.5098 = 0.0188 kmol/hr

133.5

Total = 52.5886 kmol/hr

D = 52.5886 kmol/hr

Mole fraction of MEK, XMEK = 49.39 = 0.94

52.5886

from T-x-y diagram distillate temperature = 80.4 0 C

Cp MEK = 170 kj/kmol k

Cp alcohol = 228 kj/kmol k

Cp water = 75.37 kj/mol k

Cp TCE = 148.56 kj/mol k

D. HD = 3.1552 x 228 + 49.39 x 170 + 0.4421 x 75.37 + 0.0188x 148.56(80.4)

= 0.7358 x 10 6 kj/hr

Residue:

MEK = 21.2454 kg = 0.2965 kmol/hr

TCE = 15199.421 kmol = 113.85 kmol /hr

133.5

Water = 25.9195 = 1.4399 kmol /hr

18

Total = 115.5864 kmol/hr

XMEK = 0.2965 = 0.0026

115.5864

From T-x-y diagram the temoerature obtained . T = 112 0 C = 385k (residue)

Cp MEK = 175 kj/mol k Cp alcohol = 260 kj/kmol k Cp water = 75.37 kj/kmol k

Cp TCE = 148.56 kj/kmol k

W. Hw = 0.2965 x 175 + 113.85 x 148.56 + 1.4399 x 75.37x (112) = 1.9123 x 10 6 kj/hr

Condenser :-

VHv =D.HD + L. HL + Qc.

VHv = (D + L ) . HL +Qc

Qc = V x (Hv - HL)

Qc = V x 

  • V = (1 + R ) x D

  • D = 52.5886 kmole/hr

  • V = ( 1 + 0.76 )x 52.5886 = 92.556 kmole/hr.

Vx= 92.556 x 3.18445 x10 4

= 2.9474 x10 6 kj/hr Qc = 2.9474 x 10 6 kj/hr

Cooling water requirement =

2.9474 x 10 6

4.187 x (42 24) = 3.911x 10 4 kg/hr

Reboiler:-

Overall heat balance

F. HF + QB = Qc + D . HD + WHw QB = Qc + D . HD + WHw - F. HF

QB = DHD = WHw + Qc - FHF

QB = 0.7358 x 10 6 +1.9123 x 10 6 + 2.9474 x 10 6 0.69025 x 10 6

QB = 4.90525 x 10 6 kj/hr

Steam is available at 3.302 bar steam temperature = 410 k

Steam requirement is = 4.90525 x 10 6

2153.4

= 2277.91 kg/hr

One cooler is attached to cool the residue.

Residue enters the cooler at 112 0 C and leaves at 27 0 C

So, cooling water requirement = 1.451299 x10 6 4.187 (42- 24)

= 1.92567 x 10 4 kg/hr

One more heat exchanger is used to raise the temperature of the mixed liquor of condensate and the distillate from the solvent recovery column to 82 0 C

2591.3424 x 170.058 + 18931.435 x 165.726 (26.6)

74

72

+ 212.9726 x 260 + 3367.511 x 175 + 2.5098 x 148.56

74

72

72

133.5

+ QB = 2804.315 x 260 + 22298.946 x 165.726 + 2.5098 x 148.56 (82)

74

133.5

QB = 2.981 x 10 6 KJ/hr

Steam is available at 3.302 bar, steam temperature = 410 K. Steam requirement = 2.981 x 10 6

2153.4

= 1384.32 Kg/hr

ENERGY BALANCE ACROSS THE DISTILLATION COLUMN:-

Condenser:

Qc = V x 

Qc= V x = 541.261 x 3.1 x 10 7 + 5.4673 x 4.5 x

  • 10 7 = 17.025 x 10 6

So, mass flow rate of cooling water = 17.025 x 10 6

Reboiler:

4.187 x (42-24) = 2.25899 x 10 6 kg/hr

QB = DHD + WHw + Qc - FHF

FHF = 2804.315 x 260 + 22298.946 x 165.726 + 2.5098 x 148.56 (82)

74

72

= 5.01696 x10 6 kj/hr DHD= 225.0 x 228 + 22275.0 x 170

74

Reboiler : 4.187 x (42-24) = 2.25899 x 10 kg/hr Q B = DH D +

72

(80.5)

133.5

=4.2896 x 10 6 kj/hr WHw = 2579.7131 x 260 + 23.9731 x 175 +

74

72

= 0.97632 x10 6

2.0846 x 148.65

133.5

x (107)

kj/hr QB = 17.274 kj/hr

Reboiler : 4.187 x (42-24) = 2.25899 x 10 kg/hr Q B = DH D +

Steam available at = 3.302 bar. Steam temperature = 410 k

Steam requirement = 17.274 x 10 6

2153.4

= 8021.733 kg/hr.

Distillate & the residue both has to be cooled

Heat load to cool the distillate from 80.5 to 30 0 C = 225 x 228 + 22275 x 170 (80.5

30)

So, cooling water requirement,

Recycle 2-butanol is 107 to 27 0 C

74

72

= 2.69099 x 10 6 kj/hr.

= 2.69099 x 10 6

4.187 x (42- 24) =3.57056 x 10 4 kg/hr

Heat load = 2579.7131 x 260 + 239731 x 175 + 2.0846 x 148.65

74

72

133.5

= 0.72996 x 10 6 kj/hr

(107- 27)

Cooling water requirement = 0.72996 x 10 6 4.187 x (42 24) = 9685.52 kg/hr.

7. MAJOR EQUIPMENT

DISTILLATION COLUMN: 79.5 0 C D = 312.416 k-moles xD = 0.99 Enriching section F= 347.604
DISTILLATION COLUMN:
79.5
0 C
D = 312.416 k-moles
xD = 0.99
Enriching
section
F= 347.604 k. moles
xF = 0.891
TF =82 0 C
Stripping
section
107
0 C

Glossary of notations used

F = molar flow rate of feed, kmol/hr D = molar flow rate of distillate, kmol/hr W = molar flow rate of residue, kmol/hr. xF = mole fraction of MEK in liquid xD = mole fraction of MEKin distillate xW = mole fraction of MEKin residue

Total Reboiler

W= 35.188

Xw= 0.012

Rm = minimum reflux ratio R = actual reflux ratio

L

= molar flow rate of liquid in the enriching section, kmol/hr G

= molar flow rate of vapor in the enriching section, kmol/hr L = molar flow rate of liquid in stripping section, kmol/hr G = molar flow rate of vapor in stripping section, kmol/hr

M

= average molecular weight of feed, kg/kmol

q = Thermal condition of feed

 

Feed = Saturated liquid at boiling point .

M

= 72.218

xD

Rm+1

= 0.66

Rm+1 =

xD

0.99

=

=

1.5

0.66

0.66

Rm = 1.5 1.00 = 0.5

R= 1.5 Rm = 0.75

xD

0.99

=

= 0.566

R+1

0.75 +1

Number of trays from graph =14

 

L

= RD = 0.75x312.416 = 234.312 K-moles

G =L+D = 234.312 + 312.416

= 546.728K-moles

q=1 (Feed is saturated liquid)

L = L+qf = 234.312 + 1(347.604) = 581.916 K-moles

G = G+(q 1) F = 546.728 +0 = 546.728 K-moles

(A) ENRICHING SECTION:

PLATE HYDRAULICS :

(1) Tray spacing ( ts) = 500 mm

(2) Hole diameter (dh) =5mm

(3) Pitch (lp) =3dh = 3x 5

(A) ENRICHING SECTION: PLATE HYDRAULICS : (1) Tray spacing ( t s ) = 500 mm

=15mm lar pitch

(4) Tray thickness (tT ) =0.6 dh = 3mm

(5)

Ah

=

Area of hole= 0.10

Ap

Area of pitch

(6) Plate diameter (Dc) :

(L/G)(g/L) 0.5 = 0.0246 (maximum at top)

Flooding check at top

(Ref :1, p: 18-7, fig :18-10)

Csb,flood = 0.3 ft/s Csb,flood = capacity parameter (ft/s) Unf = Gas velocity through net area at flood (ft/s or m/s)

Properties

 

Enriching section

Stripping section

 

Top

Bottom

Top

Bottom

Liquid (k-

234.312

234.312

581.916

581.916

moles/hr)

Liquid (kg/hr)

16875.15

16917.33

42046.34

43047.82

Vapor (k-

546.728

546.728

546.728

546.728

moles/hr)

Vapor (kg/hr)

39375.35

39419.09

39446.43

40444.75

x

0.99

0.9

0.8725

0.012

y

0.99

0.95

0.925

0.012

T liquid ( o C)

79.5

81.5

82.0

107.0

T vapor( o C)

80.5

82.5

83.5

107.5

vapor(kg/m 3 )

2.482

2.471

2.466

2.500

liquid (kg/m 3 )

750.02

750.00

750.00

739.88

(L/G)(g/L) 0.5

0.0246

0.0246

0.061

0.0619

liq (dyn/cm)

18.00

18.00

17.28

17.28

vapor

00048

0.0048

0.0048

0.0048

liq

0.27

0.27001

0.449

0.449001

0.0599

0.0.0059

0.148

0.149

Dvapor (m 2 /s)

Dliquid (m 2 /s)

1.688x10 -9

1.688x10 -9

1.952x10 -9

1.952x10 -9

Average conditions and Properties

   

Enriching section

Stripping section

Liquid (k-moles/hr)

234.312

581.916

(kg/hr)

16896.24

42547.08

Vapor ( k-moles/hr)

546.728

546.728

(kg/hr)

39397.22

39945.59

 

80.5

94.5

 

Tliq ( O c )

 
     
 

Tvapor ( O c )

 

81.5

95.5

 

750.01

744.94

 

liq (kg/m 3 )

 
 

2.4765

2.483

 

vapor (kg/m 3 )

 

Csb, flood = Unf

2 0

0.2

 g
 g

L-g

0.5

 



( Ref; 1, pg: 18-7)

= liquid surface tension g = gas density L = liquid density

 
 

0.2

0.5

Unf = 0.3

 

18

750.01 2.4765

= 5.105 ft/s = 1.556m/s

 

20

2.4765

Consider , 80% flooding

Un = 0.8 Unf = 1.2448 m/s Un = Gas velocity

Volumetric flow rate of vapor =

39397.22

= 4.419 m 3 /s

3600 x 2.4765

Net Area (An) = Volumetric flow rate of vapor

=

4.419= 3.549m 2

Let

L w = 0.75

Dc

Lw = Weir Length

Dc = Column Diameter Area of column (Ac ) = D 2 = 0.785 D 2

4

c

c

Sin(C/2) = (LW/2)/(DC/2) = 0.75

c= 97.2 0 Area of down comer (A ) =

d

D 2 c - Lw Dc Cos ( c)

4

c

360

2

2

2

= 0.0879 D

c

2

An = Ac Ad.

0.785Dc 2 0.0879 Dc 2 = 3.549

  • Dc = 2.26m.

  • Dc 2.3m

Lw = 0.75 Dc = 1.725m. Lw 1.7m

Ad = 0.0879(2.3) 2 = 0.465 m 2

Ac = (2.3) 2 = 4.155m 2

4

An = Ac- Ad =4.155-0.465 =3.69 m 2

Active area (Aa) = Ac 2Ad = 4.155 2(0.465) = 3.225 m 2

Lw = 1.7 = 0.74

Dc

2.3

 

c = 95.5  .

Lw = 0.74(2.3) 1.7m

(7) Perforated Area (Ap):

Acz = 260mmx Lw = 2 x 65 x10 -3 x1.7 = 0.221 m 2

A cz =

0.221

= 0.0532

Ac

4.155

Acz = 5.32% Ac

= - c = 180 95.5 = 84.5 

Awz is the waste zones area.

A

wz

= 2

4
4

D 2

c

360

- (D

4

c

0.05) 2 

360
360

2

= 0.084 m A wz = 0.084 = 0.0202

Ac 4.155

Awz = 2.02Ac

Ap = Area of perforation. Ap = Ac 2Ad Acz Awz

= 4.155 0.221 2 (0.465) 0.084

2

= 2.92 m (8) Hole Area (Ah):

Ah = Area of holes.

Ah = 0.1 Ap = 0.292 m 2 nh = number of holes.= nh = 4x 0.292=

(9) hw = 50mm

hw = weir height

(5 x 10 -3 ) 2

14872

(10) Weeping check: (Sieve Tray)

(a) (Ref:1, p:18-9, eq:18-6)

hd = K1 + K 2(g /L )Uh 2

K1 = 0 (for sieve tray)

Uh = Linear gas velocity through holes.

hd = pressure drop across dry hole (mm liquid)

K2 = 50.8

Cv

2

For Ah = 0.0905 Aa

tT = 0.6 dh

Cv

= 0.75.

(Ref :1, pg :18-9).

Cv = Discharge co-efficient. (Ref :1, fig: 18-14, pg :18-9)

K2 = 50.8 = 90.31

  • 0.75 2

(Uh)top = 39375.35

2.482 x 0.292 x 3600

= 15.126 m/s

(minimum)

(hd) top

= 90.31

2.4765

750.01

(15.126) 2 =68.23 mm of clear liquid .

h=

409

Ldh

( Ref: 1, pg:18-7, eq:18-2 (a)

h= head loss due to the bubble formation

h

= 409

18

750.01x5

=1.963 mm of clear liquid

how =

Lw

Fw 664

q

(Ref: 1, pg: 18-10, eq:18-12 (a)).

how = height of crest over weir

Fw = weir constriction correction factor.

q = Lt L

 

q = liquid flow per serration (m 3 /s )

 

q=

16896.24

= 6.258 x10 -3 m 3 /s

750.01 x 3600

q 1

= 99.197

= 1.35

(Ref:1, pg:18-11, fig:18-16)

(Lw) 2.5 (5.577) 2.5

Lw = 0.74

Dc

Fw = 1.01

1.7
1.7

how = 1.01 (664) 6.258 x10 -3

= 15.99 mm of clear liquid

hd + h= 68.23+1.963 = 70.193mm

hw + how = 50+15.99

For Ah = 0.09 Aa hw + how = 65.99 mm

= 65.99mm

(Ref :1, pg:18-7, fig:18-11)

hd + h= 18mm < 70.193 mm

There is no weeping

(11) Flooding check:

Since the maximum flow rate is at the bottom, flooding checked at the bottom.

hds = hw + how + hhg

2

(For sieve trays)

hhg = liquid gradient across plate (mm liquid)

(how )bottom = 16 mm

hds = Calculated height of clear liquid over the dispersers.

hds = 50+16+0.25 = 66.125 mm

2

(11) Flooding check: Since the maximum flow rate is at the bottom, flooding checked at the

Ua = linear gas velocity through active area.

Ua = 39397.22

3600 x 2.4765 x 3.225

= 1.37 m/s

g = 2.4765 kg/m 3

Fga = Ua (g ) ½ =1.768(FPS)

( Ref:1, pg:18-10, fig:18-15)

Aeration factor (ß) =0.59

Relative froth density ( t) =0.22

hl l = pressure drop through aerated liquid

hf = actual height of froth.

hl l = hds = 0.59 (66.125) = 39.1mm

hf = hl l = 39.1 = 185.5mm

t

0.22

hda = 165.2

q b

Ada

2

( Ref:1, Pg: 18-10, eq:18-14)

hda = head loss under the down comer

Ada = minimum area of flow under the down comes apron.

hap = hds - c = 66.125-25.4 = 40.725mm

Ada = Lw x hap = 1.7 x 40.725x10 -3 = 0.069 m 2

2 -3 hda = 165.2 6.266 x10 = 1.36mm 0.069
2
-3
hda = 165.2
6.266 x10
= 1.36mm
0.069

ht = total head loss across the plate

hd= it’s calculated at the bottom(maximum) = 68.68 mm

ht = hd + hl l = 68.68+39.1 =107.78 mm

hdc = ht + hw + how + hhg + hda

= 107.78 + 50 + 16 + 0.25 + 1.36 = 175.39 mm

(Ref :1, eg:18-3, pg:18-7)

Taking (dc) average = 0.50 ; dc = relative froth density h l = actual back-up

dc

h 1 dc = 175.39 = 350.78mm <500 mm

0.5

Flooding check is satisfied

i.e. There is no flooding.

(12) Column efficiency ( AIChE METHOD ):

(A) Point Efficiency: EOG

Ng = 0.776+0.00457hw 0.238 Ua g 0.5 +105 w

(Nsc,g) 0.5

Ng = gas phase transfer unit

Nsc,g = g=

g Dg

0.0048 x10 -3

= 0.324

2.4765 x 0.0059 x10 -4

(Ref :1, pg:18-15, eq:18-36)

Nsc,g = gas phase Schmidt number

  • 39397.22 = 1.37 m/s

Ua =

3600 x 2.4765 x 3.225

Df = Lw + Dc

=

1.7+2.3 = 2.0m

2

2

Df = width of flow path on plate

W = liquid flow rate (m 3 /sm)

W= q

 

Df

q =

16896.24

= 6.26 x10 -3 m 3 /s

750.01 x 3600

W= 6.26 x10 -3

= 3.13 x10 -3 m 3 /m-s

2.0

Ng = 0.776+0.00457(50) 0.238 (1.37) (2.4765) 0.5 +105 (3.13 x10 -3 ) (0.324) 0.5

Ng = 1.44

NL = KL a L

(Ref:1, pg: 18-15, eq:18-36 (a) )

NL = liquid phase transfer units KL a = liquid phase transfer coefficient (m/s) QL =Residence time of liquid in froth or spray zone.

(DL)average = 1.688 x10 -9

KL a =( DL ) ½ (0.40 Ua g ½ +0.17)

(Ref:1, pg:18-16, eg:18-40(a) )

KL a = (3.875 x10 8 x 1.688 x 10 -9 ) ½ ( 0.40x1.37 (2.4765) ½ +0.17)

KL a = 0.833 m/s

 

L =

hL A a

(Ref:1, pg:18-16, eq:18-39)

1000qb

hl = liquid hold-up on plate

L =

39.1 x 3.225

=

20.14 s

1000(6.26 x10 -3 )

NL = 0.833 x 20.14

=16.78

mtop=0.3375

G m = 2.3333

Lm

mbottom = 0.413

t = mtop

Gm

= 0.7875

Lm

b = mbottom Gm

= 0.9637

Lm

avg = 0.876

= stripping factor

 

Nog

=

1

(Ref: 1, pg:18-15, eq:18-34)

 
 

1

+

Ng

 

NL

 

=

1

= 1.34

 

1

+

0.876

2.51

1.44

 

16.78

 

EOG= 1- e (N

og

)

EOG= 1- e (1.34) = 0.738

(Ref:1, pg: 18-15, eq:18-33)

(B) Murphee plate efficiency : Emv

L = Residence time of liquid = 20.14 s

which is large.

Npl=Zl 2

DE l

Zl 'F FRV F

= 1.55 m

DE=6.675x10 -3 Ua 1.44 +0.922x10 -4 hl 0.00562

=0.0084 m 2 /s

Npe=

1.55 2

(0.0084x 20.14)

=14.20

  x Eog =0.876 x 0.738 = 0.646  Emv = 1.26 (from graph) EOG
 x Eog =0.876 x 0.738
= 0.646
 Emv
= 1.26
(from graph)
EOG
 Emv = 0.93
(C ) Overall column efficiency : Eoc
Eoc = log 1+Ea( - 1)
log()
(Ref:1, pg:18-17, eq:18-46)
Ea = Murphee vapor efficiency
Ea
=
1
(Ref:1, pg:18-13, eq:18-37)
Emv
1+ Emv

1-

= fractional entrainment

0.5

For L

g

= 0.0246 G

L

For 80% flood

 

From (Ref:1, fig:18-22, pg:18-44)

= 0.15

Ea= 0.93 x

1

= 0.79

 

1+0.93 x 0.15

1-0.15

Eoc

= log

1+0.79(0.876-1)

= 0.78

log(0.876)

NA = Actual tryas;

NT= theoretical trays.

NA =

NT

=

4

= 5.14 ~ 6

Eoc

0.78

Height of enriching section = 6 x 0.500 = 3.00 m

(B) STRIPPING SECTION :

PLATE HYDRAULICS :

(1) Tray spacing (ts) = 500 mm

(2) Hole diameter (dn) = 5mm

(3) Pitch (lp) =15mm

Ea= 0.93 x 1 = 0.79 1+0.93 x 0.15 1-0.15 Eoc = log 1+0.79(0.876-1) = 0.78

lar pitch

(4) Tray thickness (tr) =3mm

(5) Ah = 0.10 Ap

(6) Plate Diameter (Dc) :

(L/G)(g/L) 0.5 = 0.0619 (maximum of top)

Csb flood =0.28 ft/s

Unf = 1.434 m/s

Consider , 80% flooding .

Un =1.1472 m/s

Volumetric flow rate of vapor =4.4939 m 3 /s

Net area (An ) =3.917 m 2

Column diameter (Dc) =2.4 m Lw =1.778 m Value of Lw taken as 1.75 m. Lw = 0.73

Dc

Lw = 1.75 m

c = 93.8 0 = 86.2 0

Ac = 4.524 m 2 Ad = 0.462 m 2

An = 4.062 m

2

Aa = 3.6 m2

Acz = 0.192 m2 Awz = 0.026 m2 Ap = 3.126 m2 Ah = 0.3126 m2 nh = 16685

(9) hw =50mm

(5.17% of Ac)

(2.00% of Ac )

(10) Weeping check (Top) :

(a) (hd)top = 57.54 mm of clear liquid

(hd)bottom = 93.83 mm of clear liquid

(b) h= 1.89 mm of clear liquid

(c ) how =30.194 mm of clear liquid

hw + how = 80.194 mm hd + h= 59.43 mm

From graph, hd + h= 18mm < 59.43 mm

There is no weeping.

(11) Flooding check (Bottom)

how = 30.445 mm

hds =80.57 mm ; =0.60 ; t = 0.2 hl l =48.342 mm hf = 241.71mm hap = 55.17 mm Ada = 0.097 m 2 hda = 4.6 mm

ht

= 107.192 mm

hdcl = 192.687 mm

h

= 385.374 mm < 500 mm

dc

There is no flooding

(12) Column Efficiency (AIChE METHOD):

(A)

Point Efficiency :EOG

(a)

Ng =2.384

(b)

L = 10.88 s.

(c)

Kla = 0.83 m/s

NL = 9.03

=

1.215

Nog=1.805

 

EoG=0.83

(B)

Murphee plate efficiency :Emv

Zl = 1.64 m DE = 7.94x10 -3 m 2 /s L = 10.88 s Npe = 31.31 x Eog = 1.0

Emv = 1.7 Eog

Emv = 1.411

(C) Overall column efficiency :

= fractional entrainment

0.5

For L

g

= 0.0619 G

L

= 0.05

Ea = 1.312

 

Eoc = 1.276

NA = 9

0.83

 

=11

Height of stripping section = 11 x 0.500 = 5.5 m

Total height of the column = Enriching section + stripping section

= 3.00 + 5.5

= 8.5 m

Summary of the Distillation Column Enriching section

Tray spacing = 500

mm

Column diameter = 2.3m Weir length = 1.7m Weir height = 50 mm Hole diameter = 5 mm Hole pitch = 15 mm, triangular Tray thickness = 3mm Number of holes = 14872 Flooding % = 80

Stripping section

Tray spacing = 500 mm Column diameter = 2.4m Weir length = 1.75 m Weir height = 50 mm Hole diameter = 5 mm Hole pitch = 15 mm, triangular Tray thickness = 3mm Number of holes = 16685 Flooding % = 80

DISTILLATION COLUMN

6.2 MECHANICAL DESIGN

Specifications:-

Inside Dia :- 2.4m = 2400mm

Ht of top engaging section = 40cm.

Working pressure = 1atm = 1.032 kg/cm 2

Design pressure = 1.032 x 1.1 = 1.135 kg/cm 2

Shell material = Carbon steel ( Sp. gr. = 7.7)

Permissible tensile abs tress = 950 kg/cm 2

Insulation material = asbestos

Density of insulation = 2700 kg/m 3

Tray spacing = 500 mm

Insulation thickness = 50 mm

Down comer & plate material = S.S

Sp.gr of SS = 7.8

SKIRT = 2m

 

Shell thickness:-

ts =

P.Dt

+C

SKIRT = 2m Shell thickness :- t s = P.D t +C 2fj -p t s

2fj -p

ts = shell thickness

P= design p r

 

DI = ID of shell

f = allowable stress

J = joint factor (0.85)

C= corrosion allowance (2 mm)

ts =

1.135 x 2400

+ 2

2 x 0.85 x 950 1.135

= 3.68 mm.

Taking min shell thickness of 6mm

Shell out side Do = 2400+2x6 = 2412mm

The column is provided with torispherical head on both ends.

For torrispherical head, or radius

=> Ro = Do = 2412 mm

ro = 6% Ro = 0.06 x 2412 = 144.72 mm = 145 mm

Calculation of head thickness

t = 0.885 Prc

+ C

f x E 0.1P

rc = crown radium

E = joint

efficienc

f = allowable stress

C = corrosion allowance

ts = 0.855 x 1.135 x 2412 + 2 950 x 0.85 0.1 x 1.135 = 5.00 mm

Take head thickness to be 8mm approximate blank diameter can be found out as;

Diameter = OD + OD + 2 Sf + 2 icr

24

Sf = 800 mm

3

Diameter = 2412 + 2412 + 2 x 800 + 2 x 145

24

= 4209.2

= 4210mm

Wt of head = d 2 t [ !

4

3

= x (4.210) 2 x 0.006 x 7700 4 = 643.13kg.

Calculation of thickness with Hight ;-

Carbon steel material IS 2002 1962 Grade I

Tensile strength R20 = 37 kgf/cm 2

Yield stress = 0.55 R20 = 20.35 kgf/cm 2

fap = p.di

4(ts-c)

= 1.135 x 2400 4 x (6 2)

= 170.25 kg/cm 2

fap = tensile stress due to internal pr ( kg/cm 2 )

Stresses due to dead load (compressive) :-

w = (wt . of the shell + attachment)+ (wt . of plate). (wt of liquid hold up) + (wt . of the head)

w1 = wt of shell = dit fs . X

w2 = wt of insulation = ( do 2 in- do 2 )Sins . X

9

wh = wt of head = 643.13 kg.

Wp = wt of each plate = (An - Ah ) x t2 . !r + hw +( ts hap) x t2[ !p + Wa

WL = wt of liquid = ( Aa * HL+ Ad * hdl)fL

w = w1 + w2 + wh + (wp + wL) x X ts

w1 = wt of shell = (2.4) x 6 x 10 -3 x 7700 (X)

= 348.34 X

w2 = wt of insulation = (2.512 2 2.412 2 ) x 2700

4

= 1044.17 X kg.

wh = wt of head = 643.13 kg.

wp = wt of each plate.

= (4.062- 0.3276) x 0.003 x 7800 + 0.05 + (0.500 0.0552)x 0.003 x 7800 + wa

wp = 150 kg.

WL

=

wt . of liq

= 3.6 x 48.342 x 10 -3 + 0.462 x 0.192687x 744.94

= 205.2 kg

w = 348.34 x + 1044.17x+(150 + 205.2) X + 643.13

= 2102.51 X + 643.13

0.500

Stress due to dead level (compressive) at dist X:

fdw = w

.

 

di (ts 6)

 

= 2102.51 X + 643.13 x 2400 x ( 6 2) x 10 -1

 
 

= 6.971 X + 2.132 kg/cm 2

 

Stress due to wind load at a dist X:-

 

fwx = 1.4 Pw X 2 do (ts c)

 

This design is being due for a wind pressure of 150

kg/m 2 Pw = 150 kg/m 2

 

fwx = 1.4 x 150X 2

 

.

 

x 241.2 x ( 6 2) x 10 -1

 

= 0.693 x 2 kg/cm 2

Resultant longitudinal stress in the up wind

Ftmax = fax + fap fdw

950 x 0.5 = 0.693 X 2 - (6.971X + 2.132) + 170.25

=> 0.693X 2 6.971 X 302.618 = 0

X = 6.971 ¥ > 2 + 4 (0.693) (302.618)] 2 x 0.693

= 26.52 m

Resultant longitudinal stresses:- at down wind sides:-

- Fcax = - fwx + fap fdw

Fcmax = 1 (yield stress) = 1 x 20.35

3

3

= 6.783 kg/cm 2

- 6.783 = - 0.693x 2 + 170.25 (6.971X +

2.132) => 0.693x 2 + 6.971x 174.898 = 0

X = - 6.971 ¥ 2 + 4 x (0.693 ) (174.898)

  • 2 x 0.693

= - 6.971 23.096 2 x 0.693

= 11.64 m.

Which suggests that the design is safe. Since the design is being made on the basis of higher diameter, so the design is assumed to before for the entire length of the tower.

Design of skirt support:-

Specifications:-

Top disengaging space = 1.25 m

Bottom separator space = 2.25 m

Skirt Hgt = 2m.

Total Height of column including skirt height-

H = 8.50 + 2.00 +1.25 + 2.25 m

H = 14 m

Wt. of shell w1 = di x t x fs x H = 4876.76 kg.

Wt of insulation w2 = ( 2.152 2 2.412 2 ) x 2760 x 14 4 = 14618.38kg

Wh = Wf. Of Head = 643.13 kg.

Wp = Wt. Of plate = 150kg.

W = W1 + W2 + (WP + WL) H + Wn ts

= 4876.76 + 14618.38 + (150 + 205 .2 ) x 14 + 643.13 0.5 = 30083.87 kg

Wind Load:

fwb = (K P1 H DO). (H/2) DO 2 . t

4

= 2K P1 H 2 DO DO 2 t.

K = 0.7, P1 = 128.5 kg/m 2

fbw = 2 x (0.7) (128.5 x 14 2 x 2.412) kg/cm 2 x (2.412) 2 x t x 10 4

fbw = 4653.289 = 0.46533 t

t

<

fds = w

,

Dmt.