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Ministry of High Education and Scientific Research Al-Qadisiyah

University College of Engineering Chemical Engineering Department


(2020-2021)

(Production Acetaldehyde by dehydrogenation of ethanol)


A Project Submitted to the College of Engineering of Al-Qadisiyah
University in Partial Fulfillment of the Requirements for the Degree
of Bachelor of Science in Chemical Engineering. .

Performed by:
Ali hassan hammadi & Ali jabbar Nasser

Under the supervision of:


M.Ahmed abbas ubeed
‫ب ِْســـــــ ِم اللَّــــــ ِه َّالر ْ َْح ٰـ ِ‬
‫ـــن َّالر ِحيـــــ ِم‬

‫ب ِز ْدنِي ِع ْل ًما﴾‬ ‫آن ِمن قَ ْب ِل أَن يُ ْق َ‬


‫ض ٰى إِلَ ْيكَ َوحْ يُهُ ۖ َوقُل هر ِّ‬ ‫﴿ فَتَعَالَى ه‬
‫َّللاُ ا ْل َم ِلكُ ا ْلحَقُّ ۗ َو ََل ت َ ْع َج ْل بِا ْلقُ ْر ِ‬
‫هللا ال َع ِ ُِّل ال َعظمي‬
‫َصد ََق ُ‬

‫سورة طه آية ﴿ ‪﴾ 111‬‬

‫‪I‬‬
‫اَلهداء‬
‫بكم احلب‬

‫اىل يؼهى االَساٍَت االول ‪ ....‬ابى انزهراء حمًد (ص)‬

‫اىل قرة انؼني وشفٍغ املؤينني ابا انقاسى املهدي املنتظر (ع)‬

‫اىل سبب وجىدي ومشؼتا طرٌقً اىل اننجاح ‪ ....‬آيم وآيب‬

‫اىل استاذي املبدع و‪.‬امحد ػباس ػبٍد احملرتو ‪............‬‬

‫اىل كم يٍ قدو ايل انؼىٌ واملساػده طٍهت املسرية انؼهًٍت‬

‫اهدي هرا اجلهد املتىاضغ‬

‫‪II‬‬
Table of Contents

N Subject Page
‫االية‬ I
‫االهداء‬ II
Table of Content III
Table and Figure IV
1.1 Introduction 1
1.2 Physical Properties 2
1.3 Chemical Properties 3
1.4 Uses 8
1.5 Manufacturing Process and Selection 9
1.6 Process Selection 13
2 Chapter Two / material and Energy balance 15
2.1 Material Balance 16-29
3 Chapter Three / Design of Equipment 30
3.1 Process Design of Distillation column 47
3.3 Design of Heat Exchanger 55
4 Chapter Four / Cost estimate 64
4.1 Storage Tank 67
4.2 Vaporizer 68
4.3 Reactor 70
4.4 Heat Exchanger 72
4.5 Two Condenser 74
4.6 Per Heater 75
4.7 Distillation Column 76
5.1 Reference 82

III
List of Table and Figure

N Number Of Figure Page


1.2 Table Physical properties of acetaldehyde 2
2.1 Figure : flow sheet for the production of acetaldehyde 16
3.1 Table : T-x – y data 32
3.2 Table : parameter used in calculation 35
Figure : temperature correction factor :one shell
3.3 56
pass :two or more even tube pass
3.4 Table : constant for use in equation 58
3.5 Figure : shall – bundle clearance 59
Figure : shall – side heat – transfer factors segment
3.6 60
baffles
3.7 Figure : tube side fraction factors 61

IV
Chapter One

Introduction
1.1 Introduction

Acetaldehyde, CH3CHO is an important intermediate in industrial organic


synthesis. Acetic acid, acetic anhydride, n-butanol, and 2-ethylhexanol are the
major products derived from acetaldehyde. Smaller amounts of acetaldehyde are
also consumed in the manufacture of pentaerythritol, trimethylolpropane,
pyridines, peracetic acid,crotonaldehyde, chloral, 1,3-butylene glycol, and lactic
acid.

Acetaldehyde (ethanal) was first prepared by Scheele in 1774, by the action of


manganese dioxide and sulfuric acid on ethanol. Liebig established the structure of
acetaldehyde in 1835 when he prepared a pure sample by oxidizing ethyl alcohol
with chromic acid. Liebig named the compound “aldehyde” from the Latin words
translated as al (cohol) dehyd (rogenated). Kutscherow observed the formation of
acetaldehyde by the addition of water to acetylene in 1881.

Acetaldehyde is an important intermediate in the production of acetic acid, acetic


anhydride, ethyl acetate, peracetic acid, pentaerythritol, chloral, glyoxal,
alkylamines, and pyridines. Acetaldehyde was first used extensively during World
War I as an intermediate for making acetone from acetic acid.

Commercial processes for the production of acetaldehyde include: the oxidation


or dehydrogenation of ethanol, the addition of water to acetylene, partial oxidation
of hydrocarbons, and the direct oxidation of ethylene. It is estimated that in 1976,
29 companies with more than 82% of the world‟s 2.3 megaton per year plant
capacity use the Wacker – Hoechst processes for the direct oxidation of ethylene.
Acetaldehyde is a normal intermediate product in the respiration of higher plants.
It occurs in traces in all ripe fruits that have a tart taste before ripening; the
aldehyde content of the volatiles has been suggested as a chemical index of
ripening during coldstorage of apples. Acetaldehyde is an intermediate product of
alcoholic fermentation but it is reduced almost immediately to ethanol. It may form
in wine and other alcoholic beverages after exposure to air, and imparts an
unpleasant taste; the aldehyde ordinarily reacts to form diethyl acetal and ethyl
acetate. Acetaldehyde is an intermediate product in
the decomposition of sugars in the body and, hence, occurs in traces in blood.
Acetaldehyde is a product of most hydrocarbon oxidations.

1
1.2 physical properties

Acetaldehyde is a colorless, mobile liquid having a pungent suffocating odor that


is somewhat fruity and pleasant in dilute concentrations. Some physical properties
of
acetaldehyde are given in Table 1.1.

The freezing points of aqueous solutions of acetaldehyde are as follows:


4.8 wt %, -2.50C; 13.5 wt %, - 7.80 C, and 31.0 wt %, - 23.00 C.
Acetaldehyde is miscible in all proportions with water and most common organic
solvents: acetone, benzene, ethyl alcohol, ethyl ether, gasoline, paraldehyde,
toluene,
xylenes, turpentine, and acetic acid.

Table 1.2. PHYSICAL PROPERITIES OF ACETALDEHYDE

Properties Values
Formula weight 44.053 44.053
Melting point -123.5
Boiling point at 101.3 kPa (1 atm), °C 20.16
Density, d4 º 0.8045
d4 11 0.7901
d4 15 0.7846
d4 20 0.7780
Coefficient of expansion per °C (0-30 0.00169
°C)
Refractive index, nD20 1.33113
Vapor density (air = 1) 1.52
Surface tension at 20 °C,mN/ma 21.2
Absolute viscosity at 15 °CmPa.s b 0.02456
Specific heat at 0 °C,J/(g.K) 2.18
At 25 °C c 1.41
= C p / C v at 30 °Cand 101.3 kPa c 1.145
Latent heat of fusion, kJ/mol c 3.24
Latent heat of vaporization, kJ/mol 25.71
Heat of solution in water at 0 °C, kJ/mol - 8.20
At 25 °C c - 6.82
Heat of combustion of liquid at constant 11867.9
pressure, kJ/mol c
Heat of formation at 273 K, kJ/mol c -165.48

2
Free energy of formation at 273 K, -136.40
kJ/mol c
Critical temperature, °C 181.5
Critical pressure, Ma (atm) 6.40(63.2)
Dipole moment, C-m (debyes ) 9.04 x 10 – 30
(2.69)
Ionization potential, Ev 10.50
Dissociation constant at 0 °C, K a 0.7 x 10 – 14
Flash point, closed cup, °C -38
Ignition temperature in air, °C 165
Explosive limits of mixtures with air, 4.5 – 60.5
vol %
acetaldehyde

1.3 CHEMICAL PROPERTIES:

Acetaldehyde is a highly reactive compound exhibiting the general reactions of


aldehydes; under suitable conditions, the oxygen or any hydrogen can be replaced.
Acetaldehyde undergoes numerous condensation, addition, and polymerization
reactions.

1.3.1 Decomposition: Acetaldehyde decomposes at temperatures above 400°C,


forming principally methane and carbon monoxide. The activation energy of the
pyrolysis reaction is 97.7 kJ/mol (408.8 kcal/mol). There have been many
investigations of the photolytic and radical – induced decomposition of
acetaldehyde and deuterated acetaldehydes.

1.3.2 The Hydrate and Enol Form: In aqueous solutions, acetaldehyde exists in
equilibrium with the hydrate, CH3CH(OH)2. The degree of hydration can be
computed from an equation derived by Bell and Clunie. The mean heat of
hydration is – 21.34 kJ/mol (89.29kcal/mol); hydration has been attributed to hyper
conjugation. The enol form, vinyl alcohol (CH2 = CHOH) exists in equilibrium
with acetaldehyde to the extent of approximately one molecule per 30,000.
Acetaldehyde enol has been acetylated with ketene to form vinyl acetate.

3
1.3.3 Oxidation: Acetaldehyde is readily oxidized with oxygen or air to acetic
acid, acetic anhydride, and peracetic acid (see Acetic acid and derivatives). The
principal product isolated depends on reaction conditions. Acetic acid is produced
commercially by the liquid – phase oxidation of acetaldehyde at 65°C with cobalt
or manganese acetate dissolved in acetic acid as a catalyst
commercially by the liquid – phase oxidation of acetaldehyde at 65°C with cobalt
or manganese acetate dissolved in acetic acid as a catalyst. Liquid – phase
oxidation of acetaldehyde in the presence of mixed acetates of copper and cobalt
yields acetic anhydride.

Peroxy acetic acid or a perester is believed to be the precursor of acetic acid and
acetic anhydride.There are two commercial processes for the production of
peracetic acid. Low temperature oxidation of acetaldehyde in the presence of metal
salts, ultraviolet irradiation, or ozone yields acetaldehyde monoperacetate, which
can be decomposed to peracetic acid and acetaldehyde. Peracetic acid can also be
formed directly by liquid – phase oxidation at 5 - 50°C with a cobalt salt catalyst.
The nitric acid oxidation of acetaldehyde yields glyoxal. Oxidations of p – xylene
to terephthalic acid and of ethanol to acetic acid are activated by acetaldehyde.

1.3.4 Reduction: Acetaldehyde is readily reduced to ethanol. Suitable catalysts for


vapor-phase hydrogenation are supported nickel and copper oxide. Oldenberg and
Rose have studied the kinetics of the hydrogenation of acetaldehyde over a
commercial nickel catalyst.

1.3.5 Polymerization: Paraldehyde,2,4,6- trimethyl – 1,3,5 – trioxan, a cyclic


trimer of acetaldehyde is formed when a mineral acid, such as sulfuric, phosphoric,
or hydrochloric acid, is added to acetaldehyde. Paraldehyde can also be formed
continuously by feeding acetaldehyde as a liquid at 15 - 20°C over an acid ion –
exchange resin.

Depolymerization of paraldehyde occurs in the presence of acid catalysts. After


neutralization with sodium acetate, acetaldehyde and paraldehyde are recovered by
distillation. Paraldehyde is a colorless liquid, boiling at 125.35 °Cat 101 kPa (1
atm).

Metaldehyde, a cyclic tetramer of acetaldehyde, is formed at temperatures below


0°C in the presence of dry hydrogen chloride or pyridine – hydrogen bromide. The
metaldehyde crystallizes from solution and is separated from the paraldehyde by
filtration. Metaldehyde melts in a sealed tube at 246.2°C and sublimes at 115 °C

4
with partial depolymerization.
Travers and Letort first discovered Polyacetaldhyde, rubbery polymer with an
acetal structure, in 1936. More recently, it has been shown that white, nontacky,
and highly elastic polymer can be formed by cationic polymerization with BF3 in
liquid ethylene. At temperatures below - 75°C with anionic initiators, such as metal
alkyls in a hydrocarbon solvent, a crystalline, isotactic polymer is obtained. This
polymer also has an acetal structure [poly (oxymethylene) structure].
800,000 – 3,000,000 have been reported.

Polyacetaldehyde is unstable and depolymerizes in a few days to acetaldehyde.


The methods used for stabilizing
polyformaldehyde have not been successful with polyacetaldehyde and the
polymer has no practical significance (see Acetal resins).

1.3.6 Reactions with aldehydes and ketones: The base catalyzed condensation of
acetaldehyde leads to the dimmer, acetaldol, which can be hydrogenated to form
1,3 butandiol or dehydrated to form crotonaldehyde. Crotonaldehyde can also be
made directly by the vapor-phase condensation of acetaldehyde over a catalyst.

Crotonaldehyde was formerly an important intermediate in the production of


butyraldehyde, butanol, and 2-ethylhexanol. However it has been replaced
completely with butyraldehyde from the oxo process. A small amount of
crotonaldehyde is still required for the production of crotonic acid.

Acetaldehyde forms aldols with other carbonyl compounds containing active


hydrogen atoms. Kinetic studies of the aldol condensation of acetaldehyde and
deuterated acetaldehydes have shown that only the hydrogen atoms bound to the
carbon adjacent to the –CHO group takes part in the condensation reactions and
hydrogen exchange. A hexyl alcohol, 2-ethyl-1 butanol, is produced, industrially
by the condensation of acetaldehyde and butaraldehyde in dilute caustic solution
followed by hydrogenation of the acrolein intermediate. (see alcohols, higher
aliphatic) condensation of acetaldehyde in the presence of dimethylamine
hydrochloride yields polyenals which can be hydrogenated to a mixture of alcohols
containing from 4 to 22 carbon atoms.

The base catalyzed reaction of acetaldehyde with excess formaldehyde is the


commercial route to pentaerythritol. The aldol condensation of three moles of form
aldehyde with one mole of acetaldehyde is followed by a crossed cannizzaro

5
reaction between pentaerythrose, the intermediate product, and formaldehyde to
give pentaerythritol. The process proceeds to completion without isolation of the
intermediate.

Pantaerythrose has been made by condensing acetaldehyde and formaldehyde at


450 C using magnesium oxide as a catalyst. The vapor-phase reaction of
acetaldehyde and formaldehyde at 450C over a catalyst composed of lanthanum
oxide on silica gel gives acrolein.

Ethyl acetate is produced commercially by the Tischenko condensation of


acetaldehyde with an aluminum ethoxide catalyst. The Tischenko reaction of
acetaldehyde with isobutyraldehyde yields a mixture of ethyl acetate, isobutyl
acetate, and isobutyl isobutyrate.

1.3.7 Reactions with Ammonia and Amines: Acetaldehyde readily adds


ammonia to form acetaldehyde ammonia. Diethyl amine is obtained when
acetaldehyde is added to a and the mixture is heated to 50-750C in the presence of
a nickel catalyst and hydrogen at 1.2 MPa (12atm). Pyridine and pyridine derivates
are made from paraldehyde and aqueous ammonia in the presence of a
catalyst at elevated temperatures; acetaldehyde may also be used by the yields of
pyridine are generally lower than when paraldehyde is the staring material. Levy
and Othmer have studied the vapor- phase reaction of formaldehyde, acetaldehyde,
and ammonia at 3600 C over oxide catalysts; a 49% yield of pyridine and picolines
was obtained using an activated silica-alumina catalyst. Brown polymers result
when acetaldehyde reacts with ammonia or amines at a PH of 6-7 and temperature
of 3-250C. With acetaldehyde, a primary amines can be condensed to Schiff bases:
CH3CH=NR, the schiff base rivets to the starting materials in the presence of
acids.

1.3.8 Reactions with Alcohols and Phenols: Alcohols add readily to acetaldehyde
in the presence of a trace of mineral acid to form acetals; eg, ethanol and
acetaldehyde form diethyl acetal. Similarly, cyclic acetals are formed by the
reactions with glycols and other polyhydroxy compounds; eg, the reaction of
ethylene glycol and acetaldehyde gives 2 – methyl – 1,3 – dioxolane.
Mercaptals, CH3CH(SR)2, are formed in a like manner by the addition of
mercaptans. The formation of acetals by a noncatalytic vapor – phase reactions of
acetaldehyde and various alcohols at 3500C has been reported. Butadiene can be

6
made by the reaction of acetaldehyde and ethyl alcohol at temperature s above
3000C over a tantala – silica catalyst. Aldol and crotonaldehyde are believed to be
intermediates.

Butyl acetate has been prepared by the catalytic reaction of acetaldehyde with
butanol at 3000C.

Reaction of one mole of acetaldehyde with excess phenol in the presence of a


mineral acid catalyst gives 1,1 – bis (p-hydroxyphenyl) ethane. With acid catalysts
acetaldehyde and three moles or less of phenol yield soluble resins. Hardenable
resins are difficult to produce by the alkaline condensation of acetaldehyde and
phenol as acetaldehyde tends to undergo aldol condensation and self-resinification.

1.3.9 Reactions with Halogens and Halogen compounds: Halogens readily


replace the hydrogen atoms of the methyl group: eg, chlorine reacts with
acetaldehyde or paraldehyde at room temperature to give chloroacetaldehyde;
increasing the temperature to 700-800C gives dichloroacetaldehyde; and at a
temperature of 80-900C chloral is formed.

The catalytic chlorination with an antimony powder or aluminum chloride ferric


chloride has been described. Bromal is formed by an analogous series of reactions.
It has been postulated that acetyl bromide is an intermediate in the bromination of
acetaldehyde in aqueous ethanol. The gas – phase reaction of acetaldehyde and
chlorine, has prepared acetyl chloride.

The oxygen atom in acetaldehyde can be replaced by reaction of the aldehyde


with phosphorus pentachloride to produce 1,1 – dichloroethane. Hypochlorite and
hypoiodite react with acetaldehyde yielding chloroform and iodoform,
respectively.

Phosgene is produced by the reaction of carbon tetrachloride with acetaldehyde in


the presence of anhydrous aluminum chloride. Chloroform reacts with
acetaldehyde in the presence of potassium hydroxide and sodium amide to form
1,1,1 – trichloro – 2- propanol.

1.3.10 Miscellaneous Reactions: Sodium bisulfite adds to acetaldehyde to form a


white crystalline addition compound, insoluble in ethyl alcohol and ether. The
bisulfite addition compound frequently is used to isolate acetaldehyde from
solution and for purification; the aldehyde is regenerated with dilute acid.

7
Hydrocyanic acid adds to acetaldehyde in the presence of an alkali catalyst to form
the cyanohydrin; the cyanohydrin may also be prepared by reaction of sodium
cyanide with the bisulfite addition compound. Acrylonitrile can be made by
reaction of acetaldehyde with hydrocyanic acid and heating the cyanohydrin to 600
– 7000C. Alanine can be prepared by reaction of ammonium salt and alkali metalo
cyanide with acetaldehyde; this is the Strecker amino acid synthesis, a general
method for the preparation of -amino acids.

Grignard reagents add readily to acetaldehyde, the final product being a secondary
alcohol. Thioacetaldehyde is formed by reaction of acetaldehyde with hydrogen
sulfide; thioacetaldehyde polymerizes readily to the trimer.

Acetic anhydride adds to acetaldehyde forming ethylidne diacetate in the presence


of dilute acid; boron fluoride is also a catalyst for the reaction. Ethylidene diacetate
is decomposed to the anhydride and aldehyde at temperatures of 220-2680C and
initial pressures of 1.5 – 6.1 kPa (110- 160 mm Hg), or by heating to 1500C with a
zinc chloride catalyst. Acetone has been prepared in 90% yield by heating an
aqueous solution of acetaldehyde to 4100C in the presence of a catalyst.

Acetaldehyde can be condensed with active methylene groups. The reaction of


isobutylene with aqueous solutions of acetaldehyde in the presence of 1-2%
sulfuric acid yields alkyl-m-dioxanes, the principal product being 2,4,4,6-
tetramethyl – m dioxane in yields up to 90%.

1.4 Uses:

The manufacturers use about 95% of the acetaldehyde produced internally as an


intermediate for the production of other organic chemicals. Figure 1 illustrates the
significant variety of organic products ( and their end uses) derived from
acetaldehyde.

Acetic acid and acetic anhydride are the derivatives of acetaldehyde followed by
n-butanol and 2-ethylhexanol. Twenty percent of the acetaldehyde is consumed in
variety of other products, the most important being pentaerythritol, trimethylol
propane, pyridines, peraceticacid, crotonaldehyde, chloral, lactic acid.

8
1.5 MANUFACTURING PROCESSES AND SELECTION

The economics of the various processes for the manufacture of acetaldehyde are
strongly dependent on the price of the feedstock used. Since 1960, the Æ liquid-
phaseoxidation of ethylene has been the process of choice. However, there is still
commercial production by the partial oxidation of ethyl alcohol, dehydrogenation
of ethyl alcohol and the hydration of acetylene. Acetaldehyde is also formed as a
co product with ethyl alcohol and acetic acid.

1.5.1 Oxidation of Ethylene: Wacker – Chemie and Farbwerke Hoechst,


developed the direct liquid phase oxidation of ethylene in 1957 – 1959. The
catalyst is an aqueous solution of PdCl2 and CuCl2. In 1894, F.C. Phillips
observed the reaction of ethylene with an aqueous palladium chloride solution to
form acetaldehyde.
C2H4+PdCl2 + H2O→CH3CHO +Pd +2HCl

The metallic palladium is reoxidized to PdCl2 with CuCl2 and the cuprous chloride
formed is reoxidized with oxygen or air.

Pd + 2CuCl2 →PdCl2 +2CuCl


2CuCl+1/2 O2 + 2HCl → 2CuCl2 + H2O

The net result is a process in which ethylene is oxidized continuously through a


series of oxidation – reduction reactions.

C2H4 + ½ O2 → CH3CHO ΔH = -244 kJ(102.1 kcal)

Studies of the reaction mechanism of the catalytic oxidation have suggested that a
cis – hydroxyethylene – palladium  complex is formed initially, followed by an
intramolecular exchange of hydrogen and palladium to give a gem – hydroxyethyl
palladium species which leads to acetaldehyde and metallic palladium.
There are two variations for the production of acetaldehyde by the oxidation of
ethylene; the two – stage process developed by Wacker – Chemie and the one –
stage process developed by Farbwerke Hoechst. In the two – stage process
ethylene and oxygen (air) react in the liquid phase in two stages. In the first stage
ethylene is almost completely converted to acetaldehyde in one pass in a tubular
plug-flow reactor made of titanium. The reaction is conducted at 125-1300C and
1.13 Mpa (150 psig) palladium and cupric chloride catalysts. Acetaldehyde
produced in the first reactor is removed from the reaction loop by adiabatic
flashing in a tower. The flash step also removes the heat of reaction. The catalyst

9
solution is recycled from the flash – tower base to the second stage (or oxidation)
reactor where the cuprous salt is oxidized to the cupric state with air. The high
pressure off – gas from the oxidation reactor, mostly nitrogen, is separated from
the liquid – catalyst solution and scrubbed to remove acetaldehyde before venting.
A small portion of the catalyst stream is heated in the catalyst regenerator to
destroy undesirable copper oxalate. The flasher overhead is fed to a distillation
system where water is removed for recycle to the reactor system and organic
impurities, including chlorinated aldehydes, are separated from the purified
acetaldehyde product.

In the one-stage process ethylene, oxygen, and recycle gas are directed to a
vertical reactor for contact with the catalyst solution under slight pressure. The
water evaporated during the reaction absorbs the heat evolved, and make – up
water is fed as necessary to maintain the catalytic solution concentration. The gases
are water – scrubbed and the resulting acetaldehyde solution is fed to a distillation
column. The tail – gas from the scrubber is recycled to the reactor. Inerts are
eliminated from the recycle gas in a bled – stream which flows to an auxiliary
reactor for additional ethylene conversion. This oxidation process for olefins has
been exploited commercially principally for the production of acetaldehyde, but
the reaction can also be applied to the production of acetone from propylene and
methyl ethyl ketone from butanes. Careful control of the potential of the catalyst
with the oxygen stream induced commercially by a variation of this reaction.

1.5.2 From Ethyl Alcohol:


3.2.1 Acetaldehyde is produced commercially by the catalytic oxidation of ethyl
alcohol. Passing alcohol vapors and preheated air over a silver catalyst at 4800C
carries out the oxidation.

CH3CH2OH + ½ O2 → CH3CHO + H2O, ΔH = 242 kj/mol (57.84 kcal / mol)


With a multitubular reactor, conversions of 74-82% per pass can be obtained
while generating steam to be used elsewhere in the process.

1.5.2.1 Acetaldehyde also, produced commercially by the dehydrogenation of ethyl


alcohol.
Reaction:
C2H5OH →CH3CHO + H2

Catalyst: Cu -Co-Cr2o3
Temperature: 280 – 3500 C.

10
Process description: The raw material i.e., ethanol is vaporized and the vapors, so
generated, are heated in a heat exchanger to the reaction temperature by hot
product stream. The product stream is cooled to –100 C and in doing it, all
unreacted ethanol and acetaldehyde are condensed. The out going gaseous stream,
containing hydrogen mainly, is scrubbed with dilute alcohol (alcohol + water) to
remove uncondensed products and the undissolved gas. The remaining pure
hydrogen (98%) is burnt in stack.

Figure 2-1, shows the flow sheet of the process in which ethanol is vaporized in
vaporizer and heated to the reactor temperature in heat exchanger. The heated
vapors are passed through the converter. The product stream is first cooled in heat
exchanger and then in condensers using water and liquid ammonia. This condenses
most of the unreacted ethanol and the acetaldehyde formed in reactor. The
escaping gas, which is almost pure hydrogen, is scrubbed by ethanol to remove all
the traces of the product. The liquid stream consisting of mainly ethanol and
acetaldehyde, is distilled in distillation column to get acetaldehyde.

1.5.3 From Acetylene: Acetaldehyde has been produced commercially by the


hydration of acetylene since 1916. However, the development of the process for
the direct oxidation of ethylene in the 1960s has almost completely replaced the
acetylene – based processes and in 1976 there was only small volume production
in a few European countries. In the older processes, acetylene of high purity is
passed under a pressure of 103.4 kPa (15 psi) into a vertical reactor containing a
mercury catalyst dissolved in 18-25% sulfuric acid at 70-900C.

HC = CH + H2O → CH3CHO

Fresh catalyst is fed to the reactor periodically; the catalyst may be added in the
mercurous form but it has been shown that the catalytic species is a mercuric ion
complex (100). The excess acetylene sweeps out the dissolved acetaldehyde which
is condensed by water and refrigerated brine and scrubbed with water; the crude
acetaldehyde is purified by distillation and the unreacted acetylene is recycled.

The catalytic mercuric ion is reduced to catalytically inactive mercurous sulfate


and metallic mercury; this sludge, consisting of reduced catalyst and tars, is
drained from the reactor at intervals and resulfated. Adding ferric or other salts to
the reaction solution can reduce the rate of catalyst depletion. The ferric ion
reoxidizes mercurous to the mercuric ion while it is reduced to the ferrous state;
consequently, the quantity of sludge, which must be recovered, is reduced

11
(81,101). In one variation, acetylene is completely hydrated with water in a single
operation at 68-730C using the mercuric iron salt catalyst. The acetaldehyde is
partially removed by vacuum distillation and the mother liquor recycled to the
reactor. The aldehyde vapors are cooled to about 350C, compressed to 253 kPa
(2.5 atm), and condensed. It is claimed that this combination of vacuum and
pressure operations substantially reduces heating and refrigeration costs.

Acetaldehyde may also be made from methyl vinyl ether and ethylidene diacetate,
both of which can be made from acetylene. Methyl vinyl ether is made by the
addition of methanol to acetylene at 1.62 Mpa (16 atm) in a vertical reactor
containing a 20% methanolic solution of potassium hydroxide. Hydrolysis of the
ether with dilute sulfuric acid yields acetaldehyde and methanol which are
separated by distillation; the methanol is recycled to the reactor. Acetylene and
acetic acid form ethylidene diacetate in the presence of mercuric oxide and sulfuric
acid at 60-800C and atmospheric pressure. After separation, the ethylidene
diacetate is decomposed to acetaldehyde and acetic anhydride by heating to 1500C
in the presence of a zinc chloride catalyst (81). Acetaldehyde has been made from
methyl vinyl ether and ethylidene diacetate in the past, but neither process is used
today.

1.5.4 From Saturated Hydrocarbons: Acetaldehyde is formed as a co product in


the vapor – phase oxidation of saturated hydrocarbons, such as butane or mixtures
containing butane, with air or, in higher yield, oxygen. Oxidation of butane yields
acetaldehyde, formaldehyde, methanol, acetone, and mixed solvents as major
products; other aldehydes, alcohols, ketones, glycols, acetals, epoxides, and
organic acids are formed in smaller concentrations. This is of historic interest.
Unlike the acetylene route, it has almost no chance to be used as a major process.
From synthesis Gas: A rhodium-catalyzed process capable of converting synthesis
gas directly into acetaldehyde in a single step was reported in 1974 (84-85).

CO + H2→ CH3CHO + other products

The process comprises passing synthesis gas over 5% rhodium on SiO2 at 3000C
and 2.0 Mpa (20 atm). The principal co products are acetaldehyde, 24% acetic
acid, 20%; and ethanol, 16%. In the years 1980 an beyond, if there will be a
substantial degree of coal gasification, the interest in the use of synthesis gas as a
raw material for acetaldehyde production will increase.

12
1.55 Specifications, Analytical, and Test Methods:

Commercial acetaldehyde has the following typical specifications: assay, 99%


min; color, water-white; acidity, 0.5% max (acetic acid); specific gravity, 0.790 at
200C; bp, 20.8 at 101.3 kPa (1 atm). Acetaldehyde is shipped in steel drums and
tank cars bearing the ICC red label. IN the liquid state, it is noncorrosive to most
metals; however, it oxidizes readily, particularly in the vapor state, to acetic acid.
Precautions to be observed in the handling of acetaldehyde have been published by
the manufacturing chemists association.
Analytical methods based on many of the reactions common to aldehydes have
been developed for the determination of acetaldehyde. In the absence of other
aldehydes, it can be detected by the formation of a mirror from an alkaline silver
nitrate solution (Tollens‟ reagent) and by the reduction of Fehling‟s solution. It can
be determined quantitatively by fuchsin-sulfiur dioxide solution (Schiff‟s reagent)
or by the reaction with sodium bisulfite, the excess bisulfite being estimated
iodometrically. Acetaldehyde present in mixtures with other carbonyl compounds,
organic acids, etc. can be determined by paper chromatography of 2,4 –
dinitrophenylhydrazones polarographic analysis either of the untreated mixture or
of the semicarbazones, the color reaction with thymol blue on silica gel (detector
tube method) mercurimetric oxidation, argentometric titration, microscopic and
spectrophotometric methods, and gas – liquid chromatographic analysis. With the
advent of gas – liquid chromatographic techniques, this method has superseded
most chemical tests for routine analysis.
Acetaldehyde can be isolated and identified by the crystalline compounds of
characteristic melting points formed with hydrazine‟s, semicasrbazides, etc.; these
derivatives of aldehydes can be separated by paper and column chromatography.
Acetaldehyde has been separated quantitatively from other carbonyl compounds on
an ion exchange resin in the bisulfite form; the aldehyde is eluted from the column
with a solution of sodium chloride. In larger quantities, it may be isolated by
passing the vapor into ether and saturating the ether with dry ammonia; the
product, acetaldehyde – ammonia, crystallizes from the ether solution. The
reactions of acetaldehyde with bisulfite, hydrazine‟s, oximes, semicarbazones, and
5,5–dimethyl – 1,3 cyclohexanedione (dimedone) have been used to isolate
acetaldehyde from solutions.

1.6 PROCESS SELECTION:


Here, ethyl alcohol dehydrogenation is selected for the production of
acetaldehyde. Because, in this process, hydrogen is taken out as a by-product
which can be used else where or which can be used to generate heat. In

13
dehydrogenation process more conversion-taking place compared to other processes.
The dehydrogenation catalyst has a life of several years but requires periodic reactivation.
In dehydrogenation process, number of products are less, soseparation of acetaldehyde „
from other product is not a difficult problem.

14
Chapter Two
Material and Energy Balance

15
2.1 flow sheet

Figure 2.1 Flow sheet for the production of acetaldhyde.

2.1 MATERIAL BALANCE

We produce acetaldehyde by dehydrogenation of ethanol. Flow chart is


as shown in the figure.
Reaction:

C2H5OH → CH3CHO + H2
16
Catalyst: Cu -Co-Cr2o3
Temperature: 280 – 3500 C.

Process description: The raw material i.e., ethanol is vaporized and the
vapors, so generated, are heated in a heat exchanger to the reaction
temperature by hot product stream. The product stream is cooled to –
100 C and in doing it, all unreacted ethanol and acetaldehyde are
condensed. The out going gaseous stream, containing hydrogen mainly,
is scrubbed with dilute alcohol (alcohol + water) to remove
uncondensed products and the undissolved gas. The remaining pure
hydrogen (98%) is burnt in stack. The material and energy balance in a
plant design is necessary because this fixes the relative flow rates of
different flow streams and temperatures in the flow sheet.

Notations used:
Msteam = Mass flow rate of steam.
ΔHsteam = enthalpy of steam.
meth = Mass flow rate of ethanol.
maectel = Mass flow rate of acetaldehyde.
mhydrogen = Mass flow rate of hydrogen.
Cp = specific heat capacity.
ʎ=Latent heat of vaporization
xF = mole fraction of Acetaldehyde in liquid/Feed.
yD = mole fraction of Acetaldehyde in Distillate.
xW = mole fraction of Acetaldehyde in Residue.

Amount of acetaldehyde to be produced = 150 TPD

17
Molecular weight of ethanol = 46 kg/kmol.

Molecular weight of acetaldehyde. = 44 kg/kmol.

Molecular weight of hydrogen = 2 kg/kmol. Let conversion be 97%.

the acetaldehyde produced to be some extra.

from the stoichiometry of reaction :


C2H5OH → CH3CHO + H2
1 mole of acetaldehyde is produced.

By using 1 mole of ethanol

Therefore to produce 47.3 kmol/hr of acetaldehyde amount of ethanol reacted

47.3 kmol/hr provided kc yields 100 % thus for yield of 97 %

Amount of ethanol reacted = 47.3 *0.97

= 45.89 kmol/hr

Basis :one our operation.

18
Material balance of Vaporizer:

100 C, super heated stream of ethanol

In put = Out put


45.89 kmol/hr.

Stream Mole of Mole of Mole of Total mole


acetaldehyde ethanol hydrogen
1 0 45.89 0 45.89

2 0 45.89 0 45.89

19
Material of Reactor:

Amount of acetaldehyde produced =0 .97 * 45.89 = 44.51 kmol/hr

Amount of hydrogen produced = 0.97 * 45.89 = 44.51 kmol/hr.

Amount of ethanol unreacted = 44.89-44.51= 1.38 kmol/hr.

20
Stream Mole of Mole of Mole of Total mole
acetaldehyde ethanol hydrogen
3 0 45.89 0 45.89
4 44.51 1.38 44.51 45.89

Distillation column:

Assume xd =0.99 D=44.951


xw=0.01 9
xf=0.97

meth = 1.38 kmol/hr


macetal = 44.51 kmol/hr
Total feed = F = 45.89 kmol/hr.
xf = 0.97

10, w=0.939

Amount of acetaldehyde =44.51 kmol/hr


Amount of ethanol =1.38 kmol/hr
F=44.51+1.38=45.89 kmol/hr

Total material balance F=D+W


45.89=D+W  D=45.89-W………(1 )

Material balance of acetaldehyde F*xf=D*xd+W*xw ………(2)

Sub (1) in (2)

21
W=0.939 kmol/hr
D=44.951 kmol/hr

Amount of Acetaldehyde in D
=44..951*0.99=44.501 kmol/hr

Amount of Ethanol in D
=44.951-44.501=0.45 kmol/hr

Amount of Acetaldehyde in W
=0.939*0.01=0.0093 kmol/hr

Amount of Ethanol in W
=0.939-0.0093=0.9297 kmol/hr

Stream Mole of Mole of Total mole


Acetaldehyde Ethanol
8 44.51 1.38 45.89

9 44.501 0.45 45.89

10 0.0093 0.9297 45.89

Energy balance of of Vaporizer

Energy balance of of Vaporizer:


As shown in the figure,
Ethanol liquid inlet temperature= Ti= 30 C.
Ethanol leaves as superheated steam a 100 C= To
Heating fluid is assumed to be saturated steam here and to provide sufficient temperature

22
gradient; it is taken to be about 3 atmospheric pressure
From steam table enthalpy of steam at this temperature = ʎsteam = 514.9 kcal/kg.
Boiling point of ethanol = Tb=78.4 C.
Specific heat of ethanol, at 30 C= Cpi=0 .054 kj/kmol C.
at 100 C= Cpo=0 .0399 kj/ kmol C.
ʎeth=200.6 kcal/kg
meth,in =45.89 *46 =2110.94 kg/hr
From heat balance we have
In put =out put
Msteam *ʎsteam=meth*Cpl(Tb-T)+meth*ʎeth+meth*Cpg (T-Tb)

( ) ( )
Msteam =

Msteam=979.78kg/hr.

Energy balance of Reactor:

Heat of reaction = ΔHr = 332.64 kcal / kg.


Ti=200 c To=310 c

Specific heat capacity of ethanol= 0.539 kcal kg C.

meth,in=2110.94 kg/hr.

Hin=meth*Cp*ΔT

=2110.94*0.539*(310-200)

=125157 kcal.

Cp of ethanol =0.549 kcal/kg .C

Cp of aectaldehyde =0.528 kcal/kg .C

23
Cp of aectaldehyde =0.528 kcal/kg .C

meth,out =1.38 *46 =63.48 kg/hr.

maectel,out=1958kg/hr

mhydrogen,out=89.02kg/hr

Hout= meth,out* Cp *ΔT+ maectel,out * Cp * ΔT + mhydrogen,out * Cp *ΔT

=63.48*0.549*(310-200)+1958*0.528*(310-200)+89.02*2.448*(310-

200)=141525.502 kcal/hr

Q= Hout - Hin + ΔHr

=141525.502-125157+332.64=16701.142 kacl/hr

Cpw=1 kcal/kg. C

ΔT=600-25=575 c

Q=mw*Cpw*ΔT

mw=Q/Cpw* ΔT=16701.142/1*575=29.045kg/hr.

Energy balance of Heat exchanger:

meth=2110.94 kg/hr

Cp=0.4382 kcal/kg.C

ΔT=200-100=100c

24
Q23= meth * Cp*ΔT

Q23=2110.94*0.4382*100

=92501.390 kcal

meth=63.48 kg/hr

Cp of ethanol =0.549 kcal/kg .C

maectel, =1958.44kg/hr

Cp f aectaldehyde =0.528 kcal/kg .C

mhydrogen=89.02 kg/hr

Cp of hydrogen =2.448 kcal/kg .C

Q45= meth*Cp*ΔT+ maectel,out * Cp* ΔT + mhydrogen, * Cp *ΔT

=63.48*0.549*(310-T)+1958.44*0.528*(310-T)+89.02*2.448*(310-T)

Q45=398916.6176-1286.826T

Q23= Q45

92501.390=398916.6176-1286.826T

T=238.11 C

Energy balance of Condenser C1:

ʎeth =200.6 kcal/kg

ʎaectel =139.5 kcal/kg

25
meth=63.48kg/hr

maectel, =1958.44kg/hr

Q ∑ m.ʎ= meth*ʎeth+ maectel * ʎaectel

Q=63.48*200.6+139.5*1958.44

=285936.46 kcal

Cpw=1 kcal/kg. C

ΔT=50-25=25

Q=mw*Cpw*ΔT

Mw=Q/CPw* ΔT

=285936.46/1*25

=11437.458kg/hr

Energy balance of Condenser 2:

Q ∑ m.ʎ= meth*ʎeth+ maectel * ʎaectel

Q =285936.46 kcal

ʎamonia=590 kal/kg

Q= mamonia*ʎamonia

26
= =484.637
Mamonia

Energy balance of Preheater


At 40 C,
Cp, acetaldehyde=0.347kcal /kg C.

Cp, ethanol=0.616kcal/kg C.

Q= meth*Cp*ΔT+ maectel,out * Cp* ΔT

Q=63.48*0.616*(40-25)+1958.44*0.347*(40-25)

=10780.235kcal.

Cpw=1 kcal/kg. C

ΔT=50-30=20 c

Q=mw*Cpw*ΔT

Mw= = =539.011kg/hr.

Energy balance of Distillation column:

ΔH= Q - Ws

Q= ΔHW + ΔHD - ΔHF

=W*Cpw*(TW-T) + D*CpD*(TD-T) – F*CpF*(TF-T)

Cpi, acetaldehyde=0.347kcal/kgC.

27
Cpi, ethanol=0.616kcal/kgC.

Cpo, acetaldehyde=0.482kcal/kgC.

Cpo, ethanol=0.5803kcal/kgC.

meth,D=0.45 *46 =20.7kg/hr

maectel,D=44.501 =1958.04kg/hr

D =20.7+1958.04=1978.74kg/hr

meth,W=0.9297 *46 =42.766kg/hr

maectel,W=0.0093 *44 =0.409kg/hr

W =42.766+0.409=43.175kg/hr

meth,F=63.48kg/hr

maectel,F=1958.44kg/hr

F =63.48+1958.44=2021.92kg/hr

Cpmix,w=∑Xi*Cpi= *0.5803* *0.482


=0.0026kcal/kg.c

Cpmix,D=∑Yi *Cpi *0.5803* *0.482

=0.0028 kcal/kg.c
Cpmix,f=∑Zi *Cpi= *0.616* *0.482

=0.00902 kcal/kg.c

28
P= 1atm=760 mmHg

For acetaldhyde

ln P*=A- ln (760)= 16.2418 -


( )

T=293.07 K =20.07 C

For ethanol

ln P*=A- ln (760)= 18.9119 -


( )
T=351.89 k =78.89 c

T= ∑ Xi *Ti

Tw= *78.89* *20.07

=15 c
TD= *78.89* *20.07

=16.39 c
Tf= *78.89* *20.07

=48 c

Q= W*Cpw*(TW-T) + D*CpD*(TD-T) – F*CpF*(TF-T)

Q=43.175*0.0026*(15-60) + 1978.74*0.0028*(16.39-60)

– 2021.92*0.00902 * (48-60) Q= -27.728kcal.

29
Chapter three
Design of Equipement

30
3.1 PROCESS DESIGN OF DISTILLATION COLUMN:

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 Acetaldehyde in
liquid/Feed.yD = mole fraction of
Acetaldehyde in Distillate. xW = mole
fraction of Acetaldehyde in Residue.
MF = Average Molecular weight of Feed, kg/kmol
MD = Average Molecular weight of Distillate,
kg/kmolMW = Average Molecular weight of
Residue, kg/kmol Rm= Minimum reflux ratio
R = 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.
q = Thermal condition of Feed.
ρL = Density of Liquid, kg/m3.
ρV = Density of Vapor, kg/m3.
qL = Volumetric flow rate of
Liquid, m3/sqV = Volumetric flow
rate of Vapor, m3/s
L = Viscosity of Liquid, cP.
TL = Temperature of
Liquid, ◦ K.TV =
Temperature of Vapor, ◦
K

T – x- y date:

31
T ◦C 98.5 89.9 80 71 60.5 50 39
X 0.000 0.06 0.1 0.3 0.7 0.9 1.000
Y 0.000 0.304 0.418 0.665 0.87 0.958 1.000
Table 3.1 T-x-y data.

Preliminary calculations:

F = 45.89 kmol/hr , xF = 0.97, MF = 44.123


kg/kmol.
D = 44.951kmol/hr , xD = 0.99, MD = 44.04
kg/kmol.W = 0.939 kmol/hr , xW = 0.01, MW =
45.64 kg/kmol.

Distillation column temperature = 40 ◦ C

Assume Minimum reflux ratio = 1


Distillation column pressure = 1 atm. = 760
mm Hg.Basis: One-hour operation.
From the graph,

= =0.49

32
Thus Rm=1
Let
R=1.5*Rm

Therefore R=1.5*1=1.5

Thus,
xD/(R+1)=0.99/(1.5+1)=0.39

Number of real trays in =7

Number of Theoretical Stages = 7 – 1 = 6 stages

Number of Actual Stages = 7 – 1/0.6 = 10 stages

Assume tray Spacing = 0.5 m

Height of column = Number of Actual Stages * tray Spacing

= 10 * 0.5 = 5 m

Now, we know that,

R = Lo/ D

=> Lo = R*D
i.e., Lo= 0.0714*144.7
i.e., Lo =10.33 kmol/hr.
Therefore, Lo = 10.33 kmol/hr.

L= Liquid flow rate on the Top tray = 10.33 kmol/hr.


Since feed is Liquid, entering at bubble point,
q= (HV-HF) / (HV-HL) = 1
Now,
Slope of q-line = q/ (q-1)
= 1/ (1-1) = 1/0 = ∞

33
Now we know that,
(L¯ -L)/ F = q = 1
(L¯ - L) = F
L¯ = F + L
i.e., L¯ = 10.33 + 152.798
i.e., L¯ = 163.128 kmol/hr.

Therefore, liquid flow rate in the Stripping Section = 163.128 kmol/hr.


Also, we know that,
G¯ = [(q-1) ×F] + G
i.e., G¯ = [(1-1) ×F] + G
i.e., G¯ = [0×F] +G
i.e., G¯ = 0 +G
G¯ = G

Now, we know that,


G=L+D
i.e., G = Lo +D
i.e., G= 10.33 + 144.7
i.e., G= 155.03 kmol/hr.

Thus, the flow rate of Vapor in the Enriching Section = 155.03 kmol/hr.

Since G¯ =G
G¯ =G = 155.03 kmol/hr
Therefore, the flow rate of Vapor in the Stripping Section = 155.03 kmol/hr

34
List of parameters used in calculation:

PROPERTY TOP BOTTOM TOP BOTTOM


X 0.99 0.95 0.95 0.177
Y 0.99 0.97 0.97 0.177
Liquid, L 10.33 10.33 163.128 163.128
kmol/hr.
Vapor, G 155.03 155.03 155.03 155.03
kmol/hr.
T liquid, ◦ C 39.77 39.77 39.77 80.05
T vapor, ◦C 53.00 54.01 54.01 94.13
Mavg. liquid 44.02 44.1 44.1 45.646
kg/kmol
Mavg. Vapor 44.02 44.06 44.06 45.646
kmol/hr
Liquid, L 454.726 455.55 7193.9 7446.14
kg/hr.
Vapor, G 6824.42 6830.02 6830.6 7076.5
kg/hr
‘density’ ρl 784.69 784.50 784.50 747.87
kg/m3
‘density’ ρg 3.4376 3.425 3.425 3.361
kg/m3
(L/G)( ρl/ρg)0.5 0.0039 0.004 0.06958 0.0705
Table 3.2 Parameters used in calculations.

Design Specification:
a) Design of Enriching Section:

Tray Hydraulics,
The design of a sieve plate tower is described below. The equations and
correlations are borrowed from the 6th and 7th editions of Perry‟s Chemical
Engineers‟ Handbook.

35
1. Tray Spacing, (ts) :

Let ts = 18” = 457 mm. (range 0.15 – 1.0 m).

2. Hole Diameter, (dh):

Let dh = 5 mm. (range 2.5 – 12 mm).

3. Hole Pitch (lp):

Let lp = 3* dh (range 2.5 to 4.0 times dh).


i.e., lp = 3*5 = 15 mm.

4. Tray thickness (tT):

Let tT = 0.6* dh (range 0.4 to 0.7 times dh).


i.e., tT = 0.6*5 = 3 mm.

5. Ratio of hole area to perforated area (Ah/Ap):

Refer fig 3
Now, for a triangular pitch, we know that,

Ratio of hole area to perforated area(Ah/Ap)=1/2(π/4*(dh2)/(3/4)* lp)2


i.e., (Ah/Ap) = 0.90* (dh/lp)2

i.e., (Ah/Ap) = 0.90* (5/15)2


i.e., (Ah/Ap) = 0.1

Thus,
(Ah/Ap) = 0.1

36
6. Plate Diameter (Dc):

The plate diameter is calculated based on entrainment flooding considerations


L/G {ρg/ρl} 0.5 = 0.004--------------------- (maximum value)
Now for,
L/G {ρg/ρl} 0.5 = 0.004 and for a tray spacing of 500 mm.
We have,

From the flooding curve,------------------ (fig.18.10, page 18.7, 6th edition Perry.)

Flooding parameter, Csb, flood = 0.29 ft/s .


Now,
Unf = Csb, flood * ( / 20) 0.2 [(ρl - ρg) / g]0.5

---- {eqn. 18.2, page 18.6, 6th edition Perry.}

Where,
Unf = gas velocity through the net area at flood, m/s (ft/s)
Csb, flood = capacity parameter, m/s (ft/s, as in fig.18.10)
= liquid surface tension, mN/m (dyne/cm.)
ρl = liquid density, kg/m3 (lb/ft3)
ρg = gas density, kg/m3 (lb/ft3)

Now, we have,
 = 19.325 mN/m = 19.325 dyne/cm.
ρl = 784.5 kg/m3.
ρg = 3.425 kg/m3.

Therefore,
Unf = 0.29*(19.325/20)0.2*[(784.50-3.4250)/ 3.4250]0.5

i.e.,Unf = 4.349 ft/s =1.325

.Let,

37
Actual velocity, Un= 0.8*Unf

i.e., Un = 0.8
i.e., Un = 1.06 m/s

It is desired to design with volumetric flow rate maximum (therefore, actual is less
than the maximum).

Volumetric flow rate of Vapor at the bottom of the Enriching Section

= qo = 6830.62 / (3600*3.4250) = 0.554 m3/s.

Now,

Net area available for gas flow (An)

38
Net area = (Column cross sectional area) - (Down comer area.)
An = Ac - Ad

Thus,
Net Active area, An = to/ Un = 0.554/ 1.06 = 0.522 m2.

Let Lw / Dc = 0.77 (range 0.6 to 0.85 times Dc ).

Where, Lw = weir length, m

Dc = Column diameter, m

Now,
ϴc = 2*sin-1 (Lw / Dc) = 2*sin-1 (0.77) = 100.7

Ac = (/4)* Dc2 = 0.785* Dc2 , m


Ad = [(/4) * Dc2 *(ϴ /360)] - [(Lw /2) * (Dc /2) *cos (ϴc /2)]

i.e,Ad== [0.785* Dc2* (100.7 /360 ◦ )]- [(/4) * (Lw /Dc )* Dc2*cos(100.7)]

i.e., Ad = 0.0968*D 2, m2

Since An = Ac -Ad
0.522=(0.785* D 2 )-(0.0968* Dc2)

i.e., 0.6882* D 2 = 0.522

 D 2 = 0.522/ 0.6882 = 0.7585


 D =  0.7585
Dc = 0.87 m
Since Lw / Dc = 0.77,

39
 Lw = 0.77* Dc = 0.77*0.87 = 0.67 m.

Therefore, Lw = 0.67 m.

Now,
Ac = 0.785*0.872 = 0.5944 m2
Ad = 0.0968*D 2 = 0.0968*0.872 = 0.0724 m2
Aa = Ac –2* Ad
i.e., Aa = 0.5944- 2*0.0724  Aa= 0.4496 m2

7- Perforated plate area (Ap):

Now,
Lw / Dc = 0.67/ 0.87 = 0.7701

ϴc = 100.73 ◦

=180 º - ϴc
=180 º - 100.73 º
=79.27 º

Now,

Acz = 2* Lw* (thickness of distribution)

Where, Acz = area of calming zone, m2 (5 to 20% of Ac )

Acz = 2*0.67* (30×10-3) = 0.0402 m2--------- (which is 6.76% of Ac)

Also,
Awz =2*{(/4)*D 2 *ϴc /360 ◦ ) – (/4)* (Dc –30*10-3)2 *ϴc /360 ◦ )}

40
Where, Awz = area of waste periphery, m2 (range 2 to 5% of Ac)

i.e., Awz =2*{(/4)*0.872 (100.73 º /360 ◦ ) – (/4)* (0.87–30*10-3)2 *100.73


/360 ◦ )}

i.e., Awz = 0.0225 m2 --------- (which is 3.8% of Ac)

Now,
Ap = Ac - (2*Ad) - Acz - Awz
i.e., Ap = 0.5944- (2*0.0724) - 0.0402 - 0.0225
Thus, Ap = 0.387 m2.

8.Total Hole Area (Ah):

Since,
Ah / Ap = 0.1
Ah = 0.1* Ap
i.e., Ah = 0.1*0.387
Ah = 0.0387 m2
Thus, Total Hole Area = 0.0387 m2

Ah = nh *(/4)* d 2
Where, nh = number of holes.
nh = (4*Ah)/(*d 2)
i.e., nh =(4*0.0378)/(*0.0052)
 nh ≈1971
Therefore, Number of holes = 1971.

41
9.Weir Height (hw):

Let hw = 50 mm.

10.Weeping Check

The static pressure below the tray should be capable enough to hold the liquid
above the tray so that no liquid sweeps through the holes.
All the pressure drops calculated in this section are represented as mm head of
liquid on the plate. This serves as a common basis for evaluating the pressure
drops.

42
b). Design of Stripping Section:

Tray Hydraulics

The design of a sieve plate tower is described below. The equations and
correlations are borrowed from the 6th and 7th editions of Perry‟s Chemical
Engineers‟ Handbook.

1 Tray Spacing, (ts) :

Let ts = 18” = 457 mm.

2 Hole Diameter, (dh):

Let dh = 5 mm.

3 Hole Pitch (lp):

Let lp = 3*dh
i.e., lp = 3*5 = 15 mm.

4 Tray thickness (tT):


Let tT = 0.6* dh
i.e., tT = 0.6*5 = 3 mm.

5 Ratio of hole area to perforated area (Ah/Ap):

Refer fig 3
Now, for a triangular pitch, we know that,

Ratio of hole area to perforated area(Ah/Ap)=1/2(π/4*(dh2)/(3/4)* lp)2

i.e., (Ah/Ap) = 0.90* (dh/lp)2


i.e., (Ah/Ap) = 0.90* (5/15)2
i.e., (Ah/Ap) = 0.1

40
Thus,
(Ah/Ap) = 0.1

6-Plate Diameter (Dc):

The plate diameter is calculated based on the flooding considerations


L/G {ρg/ρl}0.5 = 0.0705 ---------------- (maximum value)
Now for,
L/G {ρg/ρl}0.5 = 0.0705 and for a tray spacing of 457 mm.
We have,
From the flooding curve, ---------- (fig.18.10, page 18.7, 6th edition
Perry.)

Flooding parameter, Csb, flood = 0.27 ft/s.


Now,
Unf = Csb, flood * (/ 20) 0.2 [(ρl - ρg) / ρg]0.5
---- {eqn. 18.2, page 18.6, 6th edition Perry.}

where,
Unf = gas velocity through the net area at flood, m/s (ft/s)
Csb, flood = capacity parameter, m/s (ft/s, as in fig.18.10)
 = liquid surface tension, mN/m (dyne/cm.)
ρl = liquid density, kg/m3 (lb/ft3)
ρg = gas density, kg/m3 (lb/ft3)
Now, we have,

 = 18.330 mN/m = 18.330 dyne/cm.


ρl = 747.87 kg/m3.
ρg = 3.361 kg/m3.

Therefore,
0.5
Unf = 0.27* (18.33/20) 0.2× [(747.87-3.361)/ 3.361]
i.e., Unf = 3.949 ft/s
Let,

41
Actual velocity, Un= 0.8*Unf
i.e., Un = 0.83.949
i.e., Un = 3.159 ft/s
Un = 0.9628 m/s

Now,

Volumetric flow rate of Vapor at the bottom of the Stripping Section


= qo =1.9657/ (3.361) = 0.5848 m3/s.
Now,
Net area available for gas flow (An)
Net area = (Column cross sectional area) - (Down comer area.)
An = Ac – Ad
Thus,
Net Active area, An = qo/ Un = 0.5848/ 0.9628 = 0.6074 m2.
Let Lw / Dc = 0.77

Where, Lw = weir length, m


Dc = Column diameter, m

Now,
ϴc = 2*sin-1(Lw / Dc) = 2*sin-1 (0.77) = 100.7

Now,
Ac =(/4)*D 2= 0.785*D 2, m2

Ad = [(/4) * D 2 * (ϴ /360 ◦ )] - [(L /2) * (D /2) *cos (ϴ /2)]

i.e,Ad== [0.785* D 2 * (100.7 /360 ◦ )]- [(/4) * D 2 * (Lw /Dc )*Dc*cos(100.7/2)]


i.e., Ad = 0.0968*D 2, m2

Since An = Ac -Ad
0.6882=(0.785* D 2 )-(0.0968* D 2)

i.e., 0.6882* D 2 = 0.6074

 D 2 = 0.6074/ 0.6882 = 0.8826

42
 Dc =  0.8826

Dc = 0.94 m
Therefore, Dc = 0.94 m
Since Lw / Dc = 0.77
 Lw = 0.77* Dc = 0.77*0.94 = 0.724 m.
T herefore, Lw = 0.724 m.

43
Now,
Ac = 0.785*0.942 = 0.694 m2
Ad = 0.09688*D 2 = 0.0968*0.942 = 0.0866 m2
An = Ac - Ad
i.e., An = 0.694 - 0.0866
 An = 0.6074 m2

7-Perforated plate area (Ap):

Aa = Ac - (2*Ad)
i.e., Aa = 0.694- (2*0.0866)
 Aa = 0.5208 m2

Now,

Lw / Dc = 0.724/ 0.94 = 0.7702


ϴc = 100.746 0
=180 ◦ -ϴc
i.e..=180 º -100.746 º

44
=79.254

Now,
Acz = 2* Lw* (thickness of distribution)

Where, Acz = area of calming zone, m2

Acz = 2*0.724* (30*10-3) = 0.04344 m2 -------- (which is 6.26% of Ac)

Also,
Awz =2*{(/4) *D 2 *(ϴ /360 º ) – (/4)*(D -0.03)2 *(ϴ /360 º )

Where, Awz = area of waste periphery, m2

i.e., Awz =2*{(/4)*0.942 * (100.746 ◦ /360 ◦ ) - (/4)*(0.94-


0.03) 2*(100.746 ◦ /360 ◦ )}

i.e., Awz = 0.0244 m2 ---- (which is 3.515% of Ac)

Now,
Ap = Ac - (2*Ad) - Acz - Awz
i.e., Ap = 0.694- (2*0.0866) - 0.04344 - 0.0244

Thus, Ap = 0.453 m2

8-Total Hole Area (Ah):

Since,
Ah / Ap = 0.1
 Ah = 0.1* Ap
i.e., Ah = 0.1*0.453
 Ah = 0.0453 m2

Thus, Total Hole Area = 0.04147 m2


Now we know that,
Ah = nh*(/4)*d 2
Where nh = number of holes.
 nh = (4*Ah)/ (*d 2 )

45
i.e., nh =(4*0.0453)/(*0.0052)
 nh = 2307.21 ≈2308
Therefore, Number of holes = 2308.

6 .Weir Height (hw):

Let, hw = 50 mm.

7.Weeping Check

All the pressure drops calculated in this section are represented as mm head of
liquid on the plate. This serves as a common basis for evaluating the pressure
drops.

46
3.2 MECHANICAL DESIGN OF DISTILLATION COLUMN:

Diameter of the tower =Di = 940 mm =0.940 m


Working/Operating Pressure = 2.087 atmosphere = 2.1558 kg/cm2
Design pressure = 1.1*Operating Pressure = 1.1*2.1558 = 2.37138 kg/cm2

Working temperature = 95 ◦ C = 368 ◦ K


Design temperature = 104.5 ◦ C = 377.5 ◦ K
Shell material - IS: 2002-1962 Carbon steel (specific gravity 7.7)

Permissible tensile stress (ft) = 95 MN/m2 = 970 kg/cm2


Insulation material - asbestos
Insulation thickness = 2”= 50.8 mm

Density of insulation = 2700 kg/m3


Top disengaging space = 0.3 m
Bottom separator space = 0.4 m
Weir height = 50 mm
Down comer clearance = 1” = 25.4 mm

b) Head - torispherical dished head:

Material - IS: 2002-1962 Carbon steel


Allowable tensile stress = 95 MN/m2 = 970 kg/cm2

c) Support skirt:

Height of support = 1000 mm = 1.0 m


Material - Carbon Steel

d) Trays-sieve type:

Number of trays = 7
Hole Diameter = 5 mm
Number of holes:
Enriching section = 1971
Stripping section = 2308
Tray spacing:

47
Enriching section: 18” = 457 mm
Stripping section: 18” = 500 mm
Thickness = 3 mm

e) Support for tray:

Purlins - Channels and Angles


Material - Carbon Steel
Permissible Stress = 127.5 MN/m2 =1299.7 k gf/cm2

1. Shell minimum thickness:

Considering the vessel as an internal pressure vessel.


ts = ((P*Di)/ ((2*ft*J)- P)) + C
where ts = thickness of shell, mm
P = design pressure, kg/cm2
Di = diameter of shell, mm
ft = permissible/allowable tensile stress, kg/cm2
C = Corrosion allowance, mm
J = Joint factor
Considering double welded butt joint with backing strip
J= 85% = 0.85
Thus, ts = ((2.37138*940)/ ((2*970*0.85)- 2.1558)) + 3 = 4.35 mm
Taking the thickness of the shell = 6 mm (standard)

2. Head Design- Shallow dished and Torispherical head:

Thickness of head = th = (P*Rc*W)/ (2*f*J)


P =internal design pressure, kg/cm2
Rc = crown radius = diameter of shell, mm
W= stress intensification factor or stress concentration factor for torispherical
head,
W= ¼ * (3 + (Rc/Rk)0.5)
Rk = knuckle radius, which is at least 6% of crown radius, mm
Now, Rc = 940 mm

48
Rk = 6% of Rc = 0.06*940 = 56.4 mm
W= ¼ * (3 + (Rc/Rk)0.5) = ¼ * (3 + (940/56.4)0.5) = 1.7706 mm
th = (2.37138*940*1.7706)/ (2*970*0.85) = 2.39 mm
Including corrosion allowance take the thickness of head = 6 mm

Weight of Head:

Diameter = O.D + (O.D/24) + (2*sf) + (2*icr/3) --- (eqn. 5.12 Brownell and Young)
Where O.D. = Outer diameter of the dish, inch
icr = inside cover radius, inch
sf = straight flange length, inch

From table 5.7 and 5.8 of Brownell and Young


sf =1.5”
icr = 2.31”

Also, O.D.= 940 mm = 37”


Diameter = 37+ (37/24) + (2*1.5)+(2/3*2.31)
d = 43.08” = 1094.23 mm.
weight head =((*d2*t)/4) * (ρ/1728)
=((*43.082*0.2362)/4) * (7700/1728)=1534.15 lb
= 695.87 kg

3. Shell thickness at different heights

At a distance „X‟m from the top of the shell the stresses are:

3.1 Axial Tensile Stress due to Pressure:


Fap= =
( ) ( )

This is the same through out the column height.

49
3.2 Circumferential stress

2 * fap = 2*185.758 = 371.516 k gf/cm2

3.3 Compressive stress due Dead Loads:

3.3.1 Compressive stress due to Weight of shell up to a distance ‘X’ meter


from top.

fds = weight of shell/cross-section of shell

=(/4) * (Dо–Di2 ) *ρs * X/(/4) * (Do –Di2 )

=weight of shell per unit height X/ ( *Dm *(ts – c)

Where Do and Di are external and internal diameter of shell.


ρs = density of shell material, kg/m3
Dm = mean diameter of shell,
ts = thickness of shell,
c = corrosion allowance

Now, ρs = 7700 kg/m3 =0.0077 kg/cm3


fds ρs* X = (7700*X) kg/m2 = (0.77*X) kg/cm2
The vessel contains manholes, nozzles etc., additional weight may be estimated
20% of the weight of the shell.
fT,ds = 1.2 * 7700*X = 0.924* (X) kg/cm2

3.3.2 Compressive stress due to weight of insulation at a height X meter:


‫؟‬ ( )
Fԁ(ins)= =
( )‫؟‬ ( )

where Dins, tins, ρins are diameter, thickness and density of insulation respectively.

Dm = (Dc+ (Dc+2ts))/2

Assuming asbestos is to be used as insulation material.

50
ρins = 2700 kg/m3
tins = 2” = 5.08 cm.
Dins =Dc+2ts+2tins = 94+ (2*0.6) + (2*5.08) = 105.36 cm.
Dm = (94+ (94+ (2*0.6)))/2 = 94.60 cm

Fԁ(ins)=
( )
= 5.092028*X kg/cm3

-
3.3.3 Stress due to the weight of the liquid and tray in the column up to a
height X
meter.

Fd,li = Σ weight of attachments per unit height X


* *(𝑡𝑠−𝑐)

The top chamber height is 0.3 m and it does not contain any liquid or tray. Tray
spacing is 457 mm.
Average liquid density = 775.45 kg/m3
Liquid and tray weight for X meter

Fliq-tray = [(X-0.3)/0.5+1]*(*Di2/4) ×ρl


= [(X-0.3)/0.5+1]*(*0.942/4) ×775.4
= [2X + 0.4] * 538.11 kg

fd (liq) = Fliq-tray *10/ (*Dm* (ts - c))


= [2X + 0.4] * 538.11 *10/ (*946* (6 - 3))
= [2X + 0.4] * 0.6035
= 1.207*X + 0.2414 kg/cm2

51
3.3.4 Compressive stress due to attachments such as internals, top head,
platforms and ladder up to height X meter.

Fd (attch)=Σ weight of attachments per unit height X


* *(𝑡𝑠−𝑐)

52
Now total weight up to height X meter = weight of top head + pipes +ladder, etc.,
Taking the weight of pipes, ladder and platforms as 25 kg/m = 0.25 kg/cm
Total weight up to height X meter = (695.87+25X)

fd (attch.) = (695.87+25X) * 10/ *946* (6 - 3) = 0.7805 + 0.028X kg/cm2


Total compressive dead weight stress:
fdx = fds + fins +fd (liq) + fd
(attch)
= 0.924X + 5.092X + [1.207X+0.2414] + [0.7805 +0.028X]
fdx = 7.251X + 1.0219 kg/cm2

4. Tensile stress due to wind load in self supporting vessels:

fwx = Mw /Z

Where, Mw = bending moment due to wind load = (wind load* distance)/2


= 0.7*Pw*D*X2/2

Z = modulus for the section for the area of shell ≈*Dm2 * (ts-c)/4
Thus, fwx =1.4*Pw*X2/(* Dm* (ts-c))
Now Pw = 25 lb/ft2 --- (from table 9.1 Brownell and Young)
= 37.204 kg/m2

|Bending moment due to wind load


Mwx = 0.7*37.204*0.94*X2/2 = 12.24(X2) kg-m
fwx= 1.4*37.204*X2(*0.94*(6-3)*10-3) = 0.58792(X2) kg/cm2

5. Stresses due to Seismic load:


fsx = Msx/(*Dᴍ 2* (ts-c) / 4)
Where, bending moment Msx at a distance X meter is given by
Msx = [C*W*X2/3] * [(3H-X)/H2]

Where, C = seismic coefficient,


W= total weight of column, kg

50
H = height of column

Total weight of column = W= Cv**ρm*Dm*g* (Hv+ (0.8*Dm))*ts*10-3

----- (eqn. 13.75, page 743, Coulson and Richardson 6th volume)

51
Where W = total weight of column, excluding the internal fittings like plates, N
Cv = a factor to account for the weight of nozzles, man ways, internal
supports, etc.
= 1.5 for distillation column with several man ways, and with plate

support rings or equivalent fittings


Hv = height or length between tangent lines (length of cylindrical section)
g = gravitational acceleration = 9.81 m/s2
t = wall thickness
ρm = density of vessel material, kg/m3
Dm = mean diameter of vessel = Di + (t *10-3) = 0.94+ (6 *10-3) = 0.946 m

W=1.5**7700*0.946*9.81*(3.0+(0.8*0.946))*6*10-3 =7590.341 N=773.73 kg.


Weight of plates -------- (Coulson and Richardson 6th volume)
Plate area =*0.942/4 = 0.694 m2

Weight of each plate = 1.2*0.694 = 0.8328 kN


Weight of 7 plates = 7*0.8328 = 5.8296 kN = 594.25 kg.
Total weight of column = 773.73 + 594.25 = 1367.98 kg.
Let, C = seismic coefficient = 0.08
Msx = [0.08*1367.98*X2/3] * [((3*3.4)-X)/3.42]
= 36.48X2 * [0.8823-0.086X] kg-m
fsx = Msx*103*Dm2* (ts-c)/4

=36.48X2 * [0.8823-0.086X * 103/(*94.62* (6-3)/4)


= [1.526X2- 0.14878X3], kg/cm2

52
On the up wind side:

ft,max = (fwx or fsx) + fap –fdx

Since the chances of, stresses due to wind load and seismic load, to occur together

is rare hence it is assumed that the stresses due to wind load and earthquake load

will not occur simultaneously and hence the maximum value of either is therefore

accepted and considered for evaluation of combined stresses.

Thus,

ft,max = 0.58792X2 + 168.871- [7.215X + 1.0129]

i.e., 0.58792X2- 7.251X + 168.871 - 1.0129- 824.5 = 0

0.58792X2- 7.251X - 656.64 =0

=> X = 40.15 m

53
On the down side:
fc,max = (fwx or fsx) - fap +fdx
3.075X2 - 86.1618+ [7.3580X + 0.6701] = fc,max

The column height is 3.4 m, for which the maximum value is


fc,max = 0.58792(3.4)2 - 168.871+ [7.251(3.4) + 1.0129]
= -136.408 kg/cm2

this shows that the stress on the down wind side is tensile.
ft,max = 85% of allowable tensile stress.
ft,max = 970 * 0.85 = 824.5 kg/cm2.
ft,max = 0.58792(X)2 – 168.871 + [7.251(X) + 1.0129] = 824.5
Therefore, X = 35.38 m.

Hence we see that the design value of the column height is more than 3.4 m, which
is the actual column height. So we conclude that the design is safe and thus the
design calculations are acceptable.

Hence a thickness of 6 mm is taken throughout the length of shell.


Height of the head = Dc/4 = 0.94/4 = 0.235 m
Skirt support Height = 1.0 m
Total actual height = 3.4 + 1 + 0.235 = 4.635 m

54
3.3 Design Of Heat Exchanger

Heat load=288830 kcal

=335.7 kw
( −𝑡2)−( −𝑡1)
∆Tim= = 121 𝑐
( −𝑡1)

R= − 2 = 0.77
𝑡 −𝑡1

S=𝑡 −𝑡1 = 0.47


−𝑡1

55
Figure 3.3 Temperature correction factor : one shell pass : two or more
even tube passes

∆Tm=∆Tlm * F =112

From table (12-1)

U=200 w/m,c.

56
Q=U A ∆T

A= = =15 m2

Choose O.d=18 mm

I. d=15 mm

L=4 m

Area of one tube =L*di*π

Area of one tube =4*18*10-3 *π=0.226 m2


Number of tube=
\ = =66

As the shell-side fluid relatively clean use

1.25 triangular pitch.

From table (12-4)

K1=0.249 , n1=2.207

57
Table 3.4 constants for use in equation

Db=do( )1/n1
Db =bundle diameter

N=number of tube

Db=18( )1/2.207

Db=226 mm

Use a split-ring floating head type.

58
Bundle diameter clearance=51 mm

Shell diameter , Ds=226+51=277 mm

Tube cross-sectional area=𝜋 𝑑i2


4

Tube cross-sectional area=176.6 mm2


Figure 3.5 shall – bundle clearance
Tubes per pass=66 = 33

59
Bundle diameter clearance=51 mm

Shell diameter , Ds=226+51=277 mm

Tube cross-sectional area=𝜋/4𝑑i2


Tube cross-sectional area=176.6 mm2

Tubes per pass=66/2=33

60
Total flow area=33*176.6*10-6=0.0058 m2

Mixture flow=1.83
Mixture mass velocity=

Density of mixture=∑yi pi

y ethanol= =0.023
y acetaldehyde= =0.928
y hydrogen= = 0.042

∑yi=1

p ethanol=293

p acetaldehyde=241

p hydrogen=0.09

Density of mixture=230.4

Mixture linear velocity= =1.37

Mixture of viscosity=∑yi µi

ethanol=0.068 m pa.sµ

acetaldehyde=0.16 m pa.sµ

hydrogen=0.002037 m pa.sµ
Mixture of viscosity=0.15 m pa.s

re=𝑝*u*di=230.4*1.37*15*10 = Re=31565
µ 0.15*10

57
Cp mixture=∑yi cpi

Cp ethanol=0.549kcal/kg
Cp acetaldehyde=0.528 kcal/kg
Cp hydrogen=2.485 kcal/kg

Cp mixture=0.607 kcal/kg

=2.54 kj/kg
Kf=thermal conductivity

Kf mixture=∑yi kfi

kf ethanol=0.049
w/m.c

kf acetaldehyde=0.186 w/m.c

kf hydrogen=0.31 w/m.c
Kf mixture=0.18 w/m.c
Pr=cp* /Kf=2.1
.

The coefficient can be calculated

0.33
= j 𝑅𝑒 𝑃 ( )0.14

Neglected( )

= =266

58
Shell-side coefficient

Choose baffle spacing= = mm

Tube pitch=1.25 * 18=22.5 mm

Calculate the area for cross flow As


( )
As=

pt=tube pitch

Ds=shell inside diameter m

Lb=baffle spacing m

( )
As= *10=0.003

Gs= * =600

Equivalent diameter

de=1.1(pt2-0.917 do2)
de=12.8 mm

µ ethanol=0.32 m pa.s

Cp ethanol=1.83
.
kf=0.049

Re= =24000

Pr= =12

59
Choose 25 percent baffle cutFrom figure (3.6)
-3
jh= *jh*Re*3.8*10

hs= *Re*Pr0.33

hs=793

Figure 3.6 shall – side heat – transfer factors , segmental baffles

Overall Coefficient
Thermal conductivity of stainless steelkw=32
Take the fouling coefficient from table (12-2)

Kw=

Ethanol=5000 Mixture=5000
.

60
𝑈

Figure 3.7 tube – side fraction factors

61
∆pt=Np(8)jf( )( )-m+2.5

Neglected the viscosity correction term

∆pt=4303 =4.3kap

Shell side

Linear velocity= = =0.85

From figure (3.8) at re=24000

jf=4.3*10-3

Figure 3.8 shall – side fraction factors , segmental baffles

62
∆ps =8 jf ( )( ) ( µ )-0.14
Neglected viscosity correction

∆ps =8*4.3*10-3*277*4000*7020.852

∆p =13730 = 13 kpa

63
Chapter four

cost estimation

64
Fixed capital cost :
The fixed capital cost is estimated according to the following correlation

Fixed capital =ppc{1+f10+f11+f12}

Total physical plant cost(ppc)=PEC{1+f1+f2+f3+f4+f5+f6+f7+f8+f9}

PEC=total purchase cost of major equipment.

F1=equipment correction(0.45)

F2=piping(0.45)

F3=instrumentation(0.15)

F4=electrical(0.1)

F5=buildings process(0.1)

F6=utilities(0.45)

F7=storages(0.2)

F8=site development(0.05)

F9=ancillary buildings(0.2)

F10=design of engineering(0.25)

F11=contractors fee (0.05)

F12=contingency (0.1)

65
Cost Escalation (inflation) :

The cost of equipment and materials is estimated based on mid- 1998.The cost up
to sept. 2021 is calculated using the following correlation:-

Cost in 2021=cost in 1998 * cost index in year 2021/cost index in year 1998

Equipment cost in 1998

The equipment cost in mid-1998 is calculated by using figure in {chemical


engineering vol.6}

The total cost of Electro chemical unit consist from the following equipment:

1- Storage tank

2-Vaporizer

3-Reactor

4- Heat exchanger

5- Two Condenser

6- Heater

7- Distillation column

66
4-1 Storage tank

Density of feed = 789kg/m3

Total mass = 6591.34kg/hr.


Total density = 789 kg / m3
Assume required time = half hour
VT=total mass /total density

VT=(6591.34*0.5hr)/ 789= 4.1 m3 Take as 4 m3

take L/D=3

V = π/4 * D2 * L = 3 * (π/4) * D3

D = 1.1 m

L=3.6 ml

From figure (7.1 b) Vol.6

67
Cost of vertical vessel =5000$

Purchased cost = (bare cost from figure)*material factor*pressure factor .


material stainless steel (S.S)

pressure = 1 bar.

Purchase cost =5000*2*1 =10000 $

Cost in 2021=Cost in mid 1998* cost index in year 2021/cost in year 2998

=10000*( 675.3/161.9) =4171.093 $

4-2 Vaporizer (Heat exchanger and vessel)

10.1-Heat exchanger
A = 15m2
type factor =floating head

from figure (6-3b heat exchanger)

68
Cost of Heat exchanger = 25000 $

purchased cost= (bare cost from figure )*material factor* pressure factor

(material stain less steel(S.S factor

Pressure = 1 bar

purchased cost=25000*2*1 = 50000 $

Cost in 2021 = Cost in 2004* Cost index in 2021 / Cost index in 2004

= 50000 * (675.3 / 161,9) = 208554.66 $

10.2 vessel

69
purchased cost= (bare cost from figure )*material factor* pressure factor

(material stain less steel(S.S factor

Pressure = 1 bar

purchased cost=6000*2*1 = 12000 $

Cost in 2021 = Cost in 2017 * Cost index in 2021 / Cost index in 2017

= 12000 * (675.3 / 659.715) = 12283.486 $

Total cost of evaporator =51181.191 + 12283.486 = 63464.67$

4-3 Reactor
Density of feed = 789kg/m3

Total mass = 6591.34kg/hr.


Total density = 789 kg / m3
Assume required time = half hour
VT=total mass /total density
V = π/4 * D2 * L = 3 * (π/4) * D3

D = 1.1 m

take L/D=6
VT=(6591.34*0.5hr)/ 789= 4.1

Q=U * A

Assume U = 1 m/s

A =Q / U =4.1/1 =4.1 m2

A=𝜋 * D2 * L  D = 0.92 L=5.52

From figure (6.5 b) Vol.6

70
71
Cost of vertical vessel =7000$

Purchased cost = (bare cost from figure)*material factor*pressure factor .

material stainless steel (S.S)

pressure = 1 bar.

Purchase cost =7000*2*1 =14000 $

Cost in 2021=Cost in mid 1998* cost index in year 2021/cost in year 2998

=14000*(675.3 / 463) =204119.43$

4-4 Heat exchanger

A = 15m2
type factor =floating head

from fig(6-3b heat exchanger)

72
Cost of Heat exchanger = 25000 $

purchased cost= (bare cost from figure )*material factor* pressure factor

(material stain less steel(S.S factor

Pressure = 1 bar

purchased cost=25000*2*1 = 50000 $

Cost in 2021 = Cost in 1998 * Cost index in 2021 / Cost index in 1998

= 50000 * (675.3 / 463) = 72926.56$

73
4-5 Two Condenser

Density of feed = 789kg/m3

Total mass = 6591.34kg/hr.


Total density = 748.5 kg / m3
Assume required time = half hour
VT=total mass /total density

VT=(6591.34*0.5hr)/ 789=4.4

take L/D=3

V = π/4 * D2 * L = 3 * (π/4) * D3

D = 1.23 m

L=3.69 ml

Q=U * A

Assume U = 1 m/s  A =Q / U =4.4/1 =4.4 m2

From figure (6-4 b) Vol.6

74
Cost of Condenser =2200 $

Cost in 2021= Cost in 2004 * Cost index in 2021 / Cost index in 2004

= 2200 * (675.3 / 463) = 2251.97 $

Two Condenser =4503.94 $

4-6 per Heater

Ce=CSⁿ [8]
Where
Ce = purchased equipment cost $,
S = characteristic size parameter, in the units given in Table 6.2,
C = cost constant from Table 6.2,
n = index for that type of equipment
C=560 n=0.77
Q=145847.87 kcal (from energy balance)
Ce=560*145847.870.77
=5301406.3 $

Cost in 2021 = Cost in 2004* Cost index in 2021 / Cost index in 2004

= 5301406.3 * (675.3 / 463) = 7732267.11$

75
4-7 Distillation column

Carbon steel
Vessel
Heigh =5 m
Dimeter =0.87m
Pressuer = 2bar

76
Cost of Distillation column =10000
purchased cost= (bare cost from figure )*material factor* pressure factor

(material stain less steel(S.S factor

Pressure = 1 bar

purchased cost=10000*2*1 = 20000 $

Plates
Diameter = 0.5 m
Type = sieve
No =7
Cost1998 = 200
Total cost of plate =7*200=1400$
Total cost of Distillation column =1400+20000 =34000
Cost in 2021= Cost in 2004 * Cost index in 2021 / Cost index in 2004

= 34000 * (675.3 / 468) =49060.25$

Total cost of all equipment = 8059334$

Total Physical Plant Cost(PPC)= PEC[1+F1+F2+F3+F4+f5+F6]

=8059334 [1+0.45+0.45+0.15+0.1+0.1+0.45+0.2+0.05+0.2]

= 25386902 $

77
Fixed capital = PPC[1+F7+F8+F9]

=25386902 [ 1+ 0.25 + 0.05 + 0.1] = 35541662.8 $

Cost of acetaldehyde plant of capacity 15000TPYin 2002 is 21.3182*108 $

Chemical Engineering Plant Cost Index:

Cost index in 2002 = 402

Cost index in 2021 = 620

Present cost of Plant = (original cost) * (present cost index)/(past cost index)

=29.167*108 $

i.e., Fixed Capital Cost (FCI) =29.167*108 $

Estimation of Capital Investment Cost:


I. Direct Costs: material and labor involved in actual installation of complete

facility (70-85% of fixed-capital investment)

a) Equipment + installation + instrumentation + piping + electrical + insulation +

Painting (50-60% of Fixed-capital investment)

1. Purchased equipment cost (PEC): (15-40% of Fixed-capital investment)

Consider purchased equipment cost = 25% of Fixed-capital investment

i.e., PEC = 25% of 29.167*108 $

=0.25*29.167*108 =7.29175*108 $

78
2. Installation, including insulation and painting: (25-55% of purchased
equipment cost.)

Consider the Installation cost = 40% of Purchased equipment cost

= 40% of 7.29175*108 =2.9167*108 $

3. Instrumentation and controls, installed: (6-30% of

Purchased equipment cost.)

Consider the installation cost = 15% of Purchased equipment cost

= 15% of 7.29175*108 =1.0937625*108 $

4. Piping installed: (10-80% of Purchased equipment cost)

Consider the piping cost = 40% Purchased equipment cost

= 40% of 7.29175*108 =2.9167*108 $

5. Electrical, installed: (10-40% of Purchased equipment cost)

Consider Electrical cost = 25% of Purchased equipment cost

= 25% of 7.29175*108 =1.8229375*108 $

Hence total cost of (1+2+3+4+5) =16.04185*108

=)55% of FCI)

B. Buildings, process and Auxiliary: (10-70% of Purchased equipment cost)

Consider Buildings, process and auxiliary cost = 40% of PEC

= 40% of 7.29175*108 =2.9167*108 $

79
C. Service facilities and yard improvement: (40-100% of Purchased equipment
cost)

Consider the cost of service facilities and yard improvement = 62% of PEC

= 62% of 7.29175*108 =4.520885*108 $

D. Land: (1-2% of fixed capital investment or 4-8% of Purchased equipment cost)

Consider the cost of land = 5% of PEC

= 5% of 7.29175*108 =0.3645875*108 $

Direct cost =23.8440225*108 $

=(81.75% of FCI)

II. Indirect costs: expenses which are not directly involved with material and
labour

of actual installation of complete facility (15-30% of Fixed-capital investment)

A. Engineering and Supervision: (5-30% of direct costs)

Consider the cost of engineering and supervision = 15% of Direct costs

i.e., cost of engineering and supervision

= 15% of 23.8440225*108 =3.5766034*108

80
B. Contingency: (5-15% of Direct costs )

Consider the contingency cost = 10% of Direct costs

i.e., Contingency cost = 10% of 23.8440225*108

=2.38440225*108 $

Indirect Costs =5.9610057*108 $

III. Fixed Capital Investment:

Fixed capital investment = Direct costs + Indirect costs

=29*108 $

IV. Working Capital: (10-20% of Fixed-capital investment)

Consider the Working Capital = 15% of Fixed-capital investment

i.e., Working capital = 15% of 29.167*108

=4.37505*108 $

V. Total Capital Investment (TCI):

Total capital investment = Fixed capital investment + Working capital

=33.54205*108 $

81
5.1 References

1. Anil Kumar “ Chemical Process Synthesis and Engineering Design” , Tata


Mc-GrawHill: page 421- 441.
2. B.C Bhattacharya, “Chemical Equipment Design”, Chemical Engineering
Education Development center.
3. L.E. Brownell And E.H. Young, “Process Equipment Design”, John Wiley
&Sons Inc. New York,
4. Gopala Rao And Marshall Sittig, “Dryden‟s Outlines Of Chemical
Technology”,2nd Ed., East-West Press, Page No:,28-638.
5. Indian Standard “Specification For Shell And Tube Heat Exchangers”, Is
4503-1967, Page No: 5-66
6. Joshi M. V., “Process Equipment Design”, 2nd Ed., Mc-Millan India Ltd,
7. Max. S Peters And Klaus Timmerhaus, “Process Plant Design And
EconomicsFor
Chemical Engineers”, 3rd Ed., Mc-Graw Hill Book Company, Page No: 207-
208,484-485.
8. Mc Ketta “ Encyclopedia of Chemical Processing and Design” , vol.1
page 97-107
9. R. H. Perry And Don W. Green, “Perry‟s Chemical Engineers‟ Hand
Book”, 6th Ed.
Mc-Graw Hill International Edition.
9. R. K. Sinnott, “Coulson And Richardson‟s Chemical Engineering Series,
Volume-6,
Chemical Equipment Design” 3rd Ed., Butter Worth-Heinemann, Page No:
828-855.
11. Treybal: “Mass Transfer Operations” Mc Graw Hill.page,
12. Ulman , “Chemical Engineering Encyclopedia” page 114

82

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