Co-Production of N-Butanol and Isobutanol

COPRODUCTION OF N-BUTANOL AND ISO-BUTANOL 2012
CHAPTER
INTRODUCTION
1
ABSTRACT
This design problem refers to coproduction of N-butanol and I-butanol by

the hydroformylation of propylene with a capacity of 115 kmol/day production of crude butanol
which can be fractionated further to N-butanol and I-butanol ; the raw materials are synthesis gas
and propylene of high purity. Our objective is to calculate the Material and Energy balances for
the overall process, and design calculations for the Distillation Column. Also estimation of cost
analysis and study on safety, hazard and pollution aspects have been carried out.
INTRODUCTION
N-butanol, iso-butanol, and tert-butanol have multiple uses in industrial and

consumer products. The market for n-butanol and isobutanol is over 7 billion lbs. the companies
focused on producing biobutanol have a captive market already.
Butanol is an aliphatic saturated C4 alcohol. It is termed normal butyl alcohol, n-

Butylalcohol, butyric alcohol, n-butanol or 1-butanol. The structure is represented by CH3CH2
CH2CH2OH or C4H8OH.There are four structural isomers of this alcohol; two primary, one
secondary and one tertiary.
n-Butanol occurs in nature in compound form. It also occurs sometimes in high

concentrations, in fusel oils obtained by fermentation.It is a colourless liquid, having character-
ristic vinous odour. The vapour has an irritant effect on mucous membranes and narcotic effect
in higher concentration. It is partly miscible with water. The autoignition temperature, freezing
point and boiling point is 365° C (-) 89° C and 116°C respectively with flash point of 35° C.
It is a major product since world war II and serves as a starting material for a wide
range of substances. Butyl alcohols can cause fat accumulations in the liver, heart and kidneys of
experimental animals. The largest use for butanol and its derivations is in the coating industry for
the formulation of nitrocellulose lacquers. An emerging market for butanol is latex in the form of
butyl acrylate. The more important derivatives of butanol are butyl acetate, butyl glycol ether and
plasticizers as an extraction solvent for oils, drugs and perfumes. It is an excellent diluent for br-
ake fluid formulations and also used as an extractant in the manufacture of antibiotics, vitamins
and hormones.
Isobutanol can also be used in practically all of the applications that have been
mentioned for butanol. Butanol is moderately dangerous; toxic fumes are emitted when heated to
decompos-ition. Excessive exposure can cause headache, dizziness, nausea etc. The liquid
effluent is degradeable and can be disposed after neutralisation with lime followed by
biodegradation. Liquid and gaseous effluents can also be incinerated.
COMMON USES OF BUTANOL:
2
N-butanol finds applications as:
Production intermediate for:
 Butyl acrylate
 Butyl acetate
 Dibutyl phthalate
Extractant for:
 Antibiotics
 Hormones
 Vitamins
Perfume ingredient
Degreasers and cleaning solutions
Repellent
Iso-butanol finds application as:
 Paint solvent
 Ink ingredient
 Gasoline additive
 Derivative ester precursor
 Viscosity reducer in paint
 Automotive polish and paint cleaner additive
BUTANOL ADVANTAGES:
3
One of the most important butanol advantages is the fact that it will reduce carbon
emissions. The EPA has released data showing that hydrocarbon, carbon monoxide, and nitrogen
oxide releases can be greatly reduced by use of butanol. Another advantage is that butanol has a
higher energy content than ethanol, almost 20% more by density. Due to its similarities to
conventional gasoline, it is able to blend much better than ethanol with gasoline. It has even
shown promise when using 100% butanol in a conventional gasoline engine. Besides these,
butanol experiences a lower chance of separation and corrosion than ethanol.
Butanol also resists water absorption, allowing it to be transported in pipes and

carriers used by gasoline. A very exciting advantage of butanol is that vehicles require no
modifications to use it. This means that with effective pumping systems, it can be implemented
immediately. Currently, funds are quickly rising for butanol production and the only requirement
is a cheap and fast modification to the ethanol plants which already exist. As yield efficiencies
rise, the cost butanol will continue to drop from its already reasonable price.
Quantifying advantages of butanol:

A recent article compared the full life cycle assessment of butanol and ethanol. Recall that
ethanol adds only a small positive delta to the energy balance. In some cases, producing ethanol
via fermentation costs the same energy (from fertilization, harvesting, fermentation and
separation) as energy expended in the steps involved in producing ethanol. Butanol shifts the
equation considerably.
4
CHAPTER
LITERATURE SURVEY
LITERATURE SURVEY
5
HISTORY:
DEVELOPMENT OF TECHNOLOGY
Between 1852 and 1871 butyl alcohols were discovered and their structures
established. In 1871 Lieben and Rossi prepared n-butyl alcohol by reducing n-butyraldehyde.
The original observation of the butanol production by 'Clostridia' was made by Pasteur and
acetonefermentation by Schardinger. Interest in commercializing butanol-acetone fermentation
occured in 1909 primarily as a means of obtaining L- butadiene as a raw material for a synthetic
rubber.
In 1914 Weizmann established a fermentation process in USA using 'Clostridium

Acetobutylicum' to ferment starchy material. With the outbreak of World War I demand for
acetone increased and large scale fermentation operation were established in Canada, USA, India
and elsewhere. After world war; DuPont developed fast-drying nitrocellulose lacquers for the
automobile industry requiring butyl acetate as solvent.
By 1930's synthetic production began and fermentation process using molasses

instead of grain were developed. Fermentation industry thrived until the end of World War II.
There were quite a few producers but currently only one plant in South Africa is reportedly
working with fermentation process.
The most wide spread means of producing butanol today is the oxo process
where propylene and syngas (CO and H2) are reacted. The oxo process or the hydroformylation
reaction was discovered by O. Roelen in 1938. The products were both aldehydes and ketones.
Most of the aldehydes produced are either reduced to alcohol directly or subjected to aldol
condensation prior to hydrogenation. High pressure cobalt catalysts oxo process was
commercialised since 1950. Ruhrchemie (Germany) used this process for producing detergent
range alcohols. Many variations of the above process have been developed and commercialised.
The next improvement came with the range of catalyst to phosphine-modified

cobalt carbonyls with reduced operating pressure. Two step rhodium oxo hydrogenation process
uses rhodium carbonyls as oxo catalyst with reactivities about 102 to 103 times higher than
cobalt carbonyls. The process also required less pressure. Rhodium based catalyst has been
further modified in recent years. The aldol process uses acetaldehyde as the precursor.
Acetaldehyde is produced by direct ethylene oxidation or by dehydrogenation of ethanol.
PROCESS OF MANUFACTURE AND RAW MATERIALS
In the oxo reaction, carbon monoxide and hydrogen are added to carbon carbon
double bond of propylene, in the liquid phase in the presence of catalyst, (cobalt hydrocarbonyls)
6
producing 1 -butanol and some amount of iso butanol. Though there are several variations of this
process,the differences being in the reaction conditions (pressure, temperature). In the high
pressure process, operation pressure is 200-300 kg/cm2 and temperature 100-180° C. The
catalyst is Co and the product is 75% or more of butanol and the rest i-butanol. The new process
using Rh catalyst operates at much lower pressure (7-20 kg/cm2). The isomaric ratios achieved
are about 92:8 or 95:1-butanol to isobutanol. Catalystic hydrogenation of the aldehydes lead to
the formation of the corresponding alcohols. As only primary alcohols can be obtained via the
oxo synthesis it is not possible to produce secondary and tertiary butyl alcohol by this process.
In Reppe process developed in 1942, propylene, carbon monoxide and water are
made to react under pressure in the presence of a catalyst (tertiary ammonium salt of poly
nuclear iron carbonyl hydrides). The difference between this process and classic Co catalyst
hydroformylation is that at low temperature (100° C) and pressure alcohol is formed directly.
This process has not been commercially successful inspite of certain advantages it offered
compared to conventional oxo process. This is attributed to more expensive process technology.
Until the mid 1950s the manufacture of n-butanol based on acetaldehyde was the
preferred process. With the development of the oxo synthesis, this process has lost its importance
in developed countries. Acetaldehyde is produced either from ethanol or ethylene and is
aldolized to acetaldol at normal temperature and pressure in the presence of alkaline catalyst.
With conversion of about 60% the acetaldol yield is about 95%. Unreacted acetaldehyde can be
distilled off and recycled.
Various gas and liquid phase processes have proved their value for the
hydrogenation of crotonaldehyde to butanol. Copper catalyst are particularly useful. For tropical
countries with large supplies of cheap biomass as well as for the more developed countries of the
third world who do not have their own oil resources this process is alternative to oxo process.
The plants producing butanol from alcohol have been generally located near alcohol distillaries.
Propylene-syngas based plant is located as down stream of naphtha cracker or very close to that
naphtha cracking unit which is normally a part of a petrochemical complex.
CAPITAL EQUIPMENT
Propylene is a co-product of ethylene from a naphtha cracking unit or

alternatively from natural gas cracking unit. Syngas is produced by reforming naphtha or natural
gas. Naphtha/natural gas cracking unit and reformer are two main capital equipment of a
petrochemical complex. The capital cost for these units is substantial.
The other capital equipment required for oxo process are syngas compressors,
alcohol reactors, blowers, waste heat boilers besides various safety and control equipment.
NOCIL imported most of the capital equipment for their butanol plant except waste boilers. For
the alcohol route some of the plant and equipment were imported by Somaiya and Oswal units,
but today they are all available indigenously.
7
In the late 1960s, Indian capability in terms of capital equipment fabrication was
restricted compared to what is today. Neverthless there are certain propritory or patented design
equipment like reformer furnace, syngas compressors, reactor and blowers are supplied by
technology supplier. Fabrication facility for reformer furnace is available in India.
STRUCTURE AND STATUS OF INDIAN INDUSTRY

At present, five units, all in private sector, are engaged in the manufacture of
butanol. The present installed capacity is about 25,700 TPA against licensed capacity of 33,200
TPA. Only one unit has been issued with license for expansion. There are three units in
Maharashtra, and one each in U.P. and A.P. Only two units are using petrochemical feed stock.
There are large number of organisations in the organised sector who have been issued with
letters of intent or industrial licenses for the manufacture of butanol and the approved capacity is
close to 92,000 TPA. Out of these, only Andhra Petro and Reliance Industries plant will be based
on petrochemical feed stock. Butanol production in 1982 was 10,740 MT and in 1992 about
20,000 MT.
The main producing units are Oswal Petro Chemicals, National Organic Chemical
Industries Limited, Somaiya Organic (I) Limited, Kolhapur Sugar Mills Limited and recently
commissioned Andhra Petro having installed capacities of 4200, 6000, 7500, 3000 and 5,000
TPA respectively. The product quality of NOCIL, Oswal and Somaiya is satisfactory and very
close to international specifications. NOCIL, one of the oldest petrochemical complex in India
commissioned their butanol plant in 1969 with capital investment of Rs. 452 lakhs, the present
replacement value of which is Rs. 5,437 lakhs. For Somaiya's plant original project cost was Rs.
411 lakhs and the present cost of expansion is Rs. 194 lakhs. The performance of these units,
over the years was satisfactory. None of the units are exclusively making butanol but
manufacturing other chemicals also. The ex works price of butanol of NOCIL is Rs 30,000 per
MT while that of Oswal and Somaiya it is Rs 38,000 and Rs. 30,500 respectively.
The major problem with the industry is feed stock, besides other constraints like
power, infrastructure etc. Both naphtha and alcohol are allocated feed stock. While one is
controlled by Central Government the other is controlled by States. Industrial alcohol prices are
altered and allocations changed by the States at times causing problem for industry. This requires
a uniform policy on alcohol by the States.
DEMAND / EXPORT / IMPORT
The demand of normal butanol by the end users was more than what industry could
produce. This necessitated import. The major sectors of consumption are paints and resins,
Pharmaceuticals, esters, plasticizers and others. The demand in 1984-85 was 13,465 MT while
the production was 11,965 MT and import was 1500 MT. The corresponding figures for the year
8
1991-92 are 22,000, 20,000 and 5,000 MT respectively, Estimated demand for the year 1999-
2000 AD is 46,700 MT. Unless the price is internationally competitive, export possibility is
remote.
TECHNOLOGY
The technologies for butanol manufacture are the followings
 Oxo-synthesis or propylene hydroformylation

 Crotonaldehyde hydrogenation starting from acetaldehyde or ethanol.
 fermentaion.
 Reppe synthesis,
The most important and widely commercialised technology is the oxo-synthesis.

It is in use in the developed countries having substantial petrochemical feed stock. The oxo-
synthesis technology in use in NOCIL plant is from Shell, Netherlands for the alcohol section
and Holdor - Topsoe for reformer section. Davy Mckee, U.K. is the technology supplier for
Andhra Petro's oxo alcohol plant.
The technologies for Somaiya Organics plant is from Melle-Beznos, France.

Oswal plant technology is form UCC, USA. Somaiya, Oswal and Kohlapur Sugar plants are
alcohol based. The plants of NOCIL, Somaiya and Oswal are in operation for a considerable
period of time and technologies are fully absorbed. The state of the art technology is based on
rhodium catalyst. None of the oxo-synthesis technologies are available indigenously. Catalysts
are very critical for the technologies referred above. Both indigenous and imported catalysts are
in use by the units.
TECHNOLOGY SUPPLIERS AND ENGINEERING CONSULTANTS
Internationally there are several technology suppliers. Some of the technology

suppliers are Shell, Netherlands, Union Carbide, Celanese Chemical, Dow Chemical all from
USA, BASF, Huls, Hoechst, Germany and Koeichemical, Tokuyama Petrochemical and few
others from Japan. The other technology suppliers are Davy Mckee, U.K. &Barsou &Consultors
Assocites, Brazil. The engineering consultants are Shell/Haldor-Topsoe, Davy Mckee and few
others. Davy Powergas (India), Lurgi. India Company Pvt. Ltd. and NOCIL Technical Service
are the Engineering consultants. Molasses to ethanol technology is available indigenously as was
seen in the case of EO/EG manufacture. None of the national laboratories is in a position to
provide the technology for butanol be it oxo process or ethanol based route.
INTERNATIONAL SCENARIO
USA is the largest producer of butanol as well as isobutanol followed by

Germany and Japan and other Contries in Europe. Most of the butanol manufacturers do not
9
exclusively manufacture butanol but other chemicals as well. Oxo process is the predominant
process in operation all over the world. Countries having biomass and ethanol are following the
ethanol route and a limited few are following the fermentation process. These countries are
Brazil, South Africa and probably Argentina. Although the capacity utilization varied between
60-70% but the growth of the industry was fairly rapid. In 1976 butanol production in USA was
248,100 MT while the world production was 540,000 MT and the corresponding figures for 1984
was 700,000 MT and 1,200,000 MT respectively. Compared to this, butanol industry growth rate
in India is insignificant. In the international arena the R&D efforts, in most of the cases have
been directed towards improvement of catalyst, leading to improvement in operating conditions
with respect to lowering of pressure and conversion of raw material to finished product and
conservation of energy.
R&D EFFORTS, TECHNOLOGY ABSORPTION AND GAPS
In the area of oxo synthesis (hydroformylation), NCL, Pune has considerable

expertise. PDIL and NCL have expertise in the field of catalyst. A good number of industrial
catalysts have been developed by them and are in commercial use. There are other catalyst
manufacturers also who manufacture practically whole range of catalyst for butanol industry.
With active involvement of Indian industry, NCL is in a position to undertake development of
indigenous oxo technology. Some of the national laboratories and industrial houses have
considerable R&D work to their credit in the field of fermentation, more so for the production of
ethanol, both potable and industrial.
THRUST AREA
No major improvements have taken place in the ethanol based technology for
butanol in the world as well as in India. This can be attributed to the fact that oxo process is the
predominant process in the world. In India though* alcohol is available yet because of various
constraints with respect to allocation, pricing and other factors, industry efforts in utilizing
alcohol for value added products did not materialize extensively.
Industry using alcohol as a feed stock for various chemicals, continued to sustain
Their activities without much investment in terms of modernization and up gradation of
technology. Therefore, alcohol route needs a thrust to make it economically competitive with
oxo process that what it is today. Fermentation process for the manufacture of butanol along with
other valuable co-products like acetone, ethanol, carbon dioxide, hydrogen, riboflavin and
livestock feed is another very promising area where adequate thrust would bring about
substantial benefit to a tropical country like India.
10
CHAPTER
SELECTION OF
PROCESS
SELECTION OF PROCESS
11
The processes of manufacture of butanol are propylene hydro-formulation (oxo

synthesis), crotonaldehyde hydrogenation starting with acetaldehyde or ethanol,Reppe synthesis
and fermentation. The raw materials for oxo process are propylene and syngas. In Reppe process,
the raw materials are propylene, carbon monoxide and water. For the production of acetaldehyde
ethanol or ethylene can be used. Acetaldehyde is aldolized followed by hydrogenation.
Fermentation process uses molasses or starch grains to produce simultaneously butanol, acetone,
ethanol carbon dioxide, livestock feed, hydrogen and riboflavin.
1.Oxo-synthesis (propylene hydroformylation):
 Propylene and syngas (CO and H2) are reacted. The products were both
aldehydes and ketones.
 Most of the aldehydes produced are either reduced to alcohol directly

Or subjected to aldol condensation prior to hydrogenation.
2. Hydrogenation starting from acetaldehyde or ethanol:
 The aldol process uses acetaldehyde as the precursor. Acetaldehyde is

produced by direct ethylene oxidation or by dehydrogenation of ethanol.
 Acetaldehyde is aldolized followed by hydrogenation in the presence of

alkaline catalyst at normal conditions.
3. Fermentaion:
 Fermentation process uses molasses or starch grains to produce

simultaneously butanol, acetone, ethanol , carbondioxide,hydrogen .
 The butanol production by 'Clostridia' was made by Pasteur and acetone

fermentation by Schardinger.
4.Reppe synthesis:
 In Reppe process, propylene, carbon monoxide and water are made to

react under pressure in the presence of a catalyst (tertiary
ammonium salt of polynuclear iron carbonyl hydrides).
 The difference between this process and classic hydroformylation is

that at low temperature (100° C) and pressure alcohol is formed
directly
.
CHOICE OF PROCESS:
12
 Oxo process is the process commercialized successful due to high yields.

 Reppe process is more expensive process technology design than oxo process.
 Acetaldehyde hydrogenation results in low conversions and high amounts of secondary
alcohols.
 Fermentation yields very less quantities of butanol .
Petrochemical production of solvents became much easier and cheaper

and also when farmer interests in molasses caused molasses prices to increase
dramatically. The combination of these events made fermentative production of acetone
and butanol inefficient and not economical.
13
CHAPTER
PHYSICAL AND
CHEMICAL
PROPERTIES
N-BUTANOL
14
Physical state and appearance: Liquid. (Z)

Odor: Vinous. (Slight.)
Taste: Not available.
Molecular Weight: 74.12g/mole
Color: Colorless.
pH (1% soln/water): Not available.
Boiling Point: 117.7°C (243.9°F)
Melting Point: -89.5°C (-129.1°F)
Critical Temperature: Not available.
Specific Gravity: 0.81(Water = 1)
Vapor Pressure: 0.6 kPa (@ 20°C)
Vapor Density: 2.55 (Air = 1)
Volatility: Not available.
Odor Threshold: 1.2 ppm
Water/Oil Dist. Coeff.: Not available.
Ionicity (in Water): Not available.
Dispersion Properties: See solubility in water, methanol, diethyl ether, n-octanol.
Solubility:
Easily soluble in methanol, diethyl ether. Partially soluble in cold water, hot water, n-octanol.
Stability and Reactivity Data :
Stability: The product is stable.

Instability Temperature: Not available.
Conditions of Instability: Not available.
Incompatibility with various substances:
Highly reactive with oxidizing agents, reducing agents. Slightly reactive to reactive with organic
materials, acids, alkalis.
Corrosivity: Non-corrosive in presence of glass.
Special Remarks on Reactivity: Not available.
Special Remarks on Corrosivity: Not available.
Polymerization: Will not occur.
ISO-BUTANOL
15
Form: liquid
Colour: colourless
Odour: sweet musty
Melting point/range: -108 °C
Boiling point/range :108 °C
Flash point 28 °C; closed cup
Autoignition temperature ;428.7 °C
Vapour pressure 14 hPa; 20 °C
Density 0.801 g/cm3; 20 °C
Water solubility : partly soluble, partly miscible
Solubility in other
solvents
partly soluble
Viscosity, dynamic 4,703 mPa.s
Relative vapour density 2.55
Stability and reactivity :
Materials to avoid Oxidizing agents, Reducing agents, Acids and bases

Hazardous
decomposition products
No decomposition if stored normally.
16
CHAPTER
OXO PROCESS OR
PROPYLENE
HYDROFORMYLATION
OXO PROCESS OR PROPYLENE HYDROFORMYLATION
17
Raw materials
1. Propylene (93%min)
2. Synthesis gas:
CO:46.6%
H2:49.2%
CO2: 0.5%
H2O : 0.3%
CH4: 3.4 %
Catalyst: triphenylphosphine rhodium hydro carbonyl
Intermediates:
N-butyraldihyde
Iso-butyraldehyde
Products:
N-butanol
Iso-butanol
Reaction proceeds as:
TWO STEPS
1.HYDROFORMYLATION:
C3H6 + CO + H2 C4H8 O
Propylene Syn gas Butyraldehyde(N ,iso)
2.HYDROGENATION:
C4H8 O + H2 CH3CH2CH2CHO
Butyraldehyde(N,iso) Butanol(N,Iso)
Catalysts comparison:
COBALT BASED RHODIUM BASED
18
TEMPARATURE(˚C) 145-180 60-100

PRESSURE(bars) 45-100 6-25
N/isoDISTRIBUTION 3-4:1 8-16:1
YIELD 67% 75%
Kinetics of the heterogeneous hydroformylation of propylene:
Using hydrocarbonyltri(triphenylphosphine)rhodium(I), dissolved in

triphenylphosphine and capillary condensed into the pores of a support, as a catalyst.
The results can be described by the power rate equation:
a b c
r ' =k 0[Rh] pC p H p CO exp(-Ea/RT)
3 2 ❑
where Ea, the apparent activation energy, is equal to 79.1 kJ/mol, and the reaction
orders a, b and c are 1.03, 0.09 and 0.23, respectively. The reaction order in carbon monoxide c
is pressure dependent, and at carbon monoxide pressures above 0.15 MPa equal to 0.08. The
selectivity towards n-butyr-aldehyde is not influenced by the hydrogen and propylene pressures,
but varies strongly with the partial pressure of carbon monoxide. When this partial pressure is
lowered from 0.52 to 0.05 MPa, the selectivity increases from 10 to 30. Similarly, an increase in
temperature from 70 to 106.8 °C raises the selectivity from 6.7 to 11.5. With Kieselguhr and
polystyrene—20% divinylbenzene (XAD-2) as catalyst supports, the rate of reaction is first order
in rhodium complex concentration in the solvent ligand PPh3. The kinetics differ significantly
from those found in homogeneous hydroformylation in, for instance, toluene.
P0A −P A
W
X
=∫
d XA
A P
=¿ ∫
d
P0AA [
=
−1 ]0
P A −P A
1−a
[
1−a
=0.981 x 10−3 g . R h . s /¿ ¿
c.c C3
]
F AO 0 −r A P
a
k [ R h ] PA
0
0
k [ R h] PA 1−a
A❑
Where
− Ea −79.1
RT
=¿ (4.721 x 10−12 ¿ e 8.314 x 10
−3
T
k =k o e
And
19
[ R h ] =10.1 mol/m3.
Ea = 79100 j/mol
K= 19.77
R= 8.314 J/mol k
OXO UNIT :
P= 5.23 bar
P0A −P A
W
X
=∫
d XA
A P
=¿ ∫
A
P0A
d
=
[ −1 ]
P 0A −P1−a
A
[
1−a
=0.981 x 10
−3
]g . R h . s /¿ ¿
c.c C3
F AO 0 −r A P
a
k [ R h ] PA
0
0
k [ R h] PA 1−a
A❑
PA = 8.75 * 10(-5) bar
XA = 1 – (pA /pA0) = 0.998 Conversion = 99.8%
PROCESS DESCRIPTION
20
OXO UNIT:
Hydroformylation of oxo reaction:
N – Bal: I – Bal: C3 H8 = 10.2: 1 :0.2
Hydroformylation of propylene to Aldehyde
C3 H6 + H2 +CO  C4 H8O (N – Bal and I – Bal)
Undesired side Reaction

Hydroformylation of propylene to propane.
C3 H6 + CO +H2  C3 H8
Catalyst : Rhodium
Pressure : 15.7 bar
Temperature : 900C.
The Oxo reactor serves to produce Crude Butyraldehyde using propylene and
synthesis gas in presence of Rhodium catalyst by Hydroformylation.
The mixture of purified Synthesis gas containing stripped propylene and purified
propylene feedstock are mixed with recycle gas including recycled including vent gas from the
Oxo compressor. The process reactants cycle gas mixture is then fed to the Oxo reactor. Which
contains rhodium based catalyst solution.
The reaction is exothermic taking place in the liquid phase at a temperature of 90-
0
110 C and a pressure of 15.7 bar. Circulating gases and evaporating the product remove a large
proportion of the reaction heat. The balance of heat is removed by circulating tempered water
through a cooling coil within the reactor. The tempered water system is a closed loop. The water
is circulated with the tempered water circulation pump. The tempered water heat is utilized in
the propylene vaporizer, while the remainder is removed by tempered water cooler. Tempered
water cooler is titanium plate heat exchange using seawater for cooling.
The tempered water is supplied from the carbon steel surge drum. Water makeup
is given from the MP condensate system. The tempered water system is maintained under a
Nitrogen blanket in the surge drum to minimize corrosion and to maintain water quality.
The Oxo Reactor temperature is maintained 90-110 0C. Below that larger catalyst
volume is required to produce the product and a higher gas circulation rate need to remove it.
Above that range causes deactivation of the catalyst takes place, which is very expensive.
FLOWSHEET FOR BUTANOL PRODUCTION:
21
REC2
REC1
22
COMP-REC
PROPYLEN 17
BUTANOL CAMPAIGN
15
B9
FEEDCOMP B10 OXO-UNIT
B4
B-AL-COL
FLASH1 B-OL-COL
SYNGAS 10 21
18
16
9 19 N-BUTANO
HYDNATOR
FLASH2
I-BUTANO
23
2 25
BUTANAL
B3
SYNG
COPRODUCTION OF N-BUTANOL AND ISO-BUTANOL
2012
In Butanol campaign the N-Bal/I-Bal is directly fed in to the VPH converter, and
is hydrogenated to from N-Butanol or I-Butanol.
Butanol campaign overview.
i) Vapor phase hydrogenation.

ii) Refining section.
N-Butanol specification: (wt%):

Purity 99.5 (min)
Water 0.1 (max)
Aldehydes. (As Butyraldehydes) 0.05 (max)
Acidity (As acetic acid) 0.01 (max)
I – Butanol specification: (wt%):

Purity 99.5 (min)
Water 0.20 (max)
Acidity (As acetic acid) 0.01 (max)
Vapor phase hydrogenation:
Butyraldehyde from the isomer column and from storage tank is fed directly to
the vaporizer. The vaporizer design enables to vaporize the liquid feeds. To avoid liquid
carryover to converter which can damage catalyst and to concentrate heavies in the VPH system
which have been produced by VPH side reactions.
The catalytic reaction takes place at hot spot temperature of 160-170 0C and a pressure of
4.5 kg/cm2. The hydrogenation reaction is exothermic, the heat produced is being used to
generate dump steam at 1.5kg/cm2 an 1150C from condensate to the reactor.
23
Hydrogenation:
N/I –Bal + H2  N/I Butanol
Pressure : 4.5 kg/cm2
Temperature : 160-1700C.
Catalyst : copper based Zinc
Butanols refining:
All the main constituents in crude butanol are relatively low boiling compounds.
The distillation was done just above atmospheric pressure. So that vacuum set is not used.
Column pressure is controlled by using Nitrogen supply and atmospheric venting.
24
CHAPTER
6
MATERIAL AND
ENERGY BALANCES
MATERIAL AND ENERGY BALANCES
Basis: 100 kmol per day of crude butanol production
25
1.Hydroginator:
From literature conversion is 94%
C4H8 O + H2 CH3CH2CH2CH2OH
Butanal(N,iso) Butanol(N,Iso)
For 100 kmol of crude butanol
(a) Butanal required = 100/0.94 =106.4 k mol/day ( since 94% conversion)
Total crude fed to reactor = 106.4/0.99 =107.46 kmol /day (since 99% convesion)
Butane to reactor = 1.26 kmol/day
Butaraldehyde unreacted = 106.4 – 100 = 64 kmol / day
(b) Hydrogen reqired = 100/0.94 =106.4 kmol /day
Total syn gas required = 106.4/0.492 = 216.2kmol /day (since 49.2% of H2 in syn gas)
Since no side reactions at reactor conditions .the outlet of the reactor contains
Butanol = 100 kmol / day
Butane = 1.26 kmol / day
CO2 = 216.2*0.466 = 100.7 kmol / day
CO = 216.2*0.005 = 1.081 kmol /day
H2O = 216.2*0.003 = 0.649 kmol /day
CH4 = 216.2*0.034 = 7.35 kmol /day
Butaraldehyde unreacted = 106.4 – 100 = 64 kmol / day
98% of crude butanal exit from 1 st reactor is recovered and it is send to the 2nd reactor
the content of butanal from the outlet of first reactor = 106.4/0.98 = 108.6 kmol/day
2.Oxo unit :
26
C3H6 + CO + H2 C4H8 O
Propelene Syn gas Butanal(N ,iso)
For 108.6 kmol /day of butanol (99.8% conversion)
(A) Propylene required = 108.6/0.998 = 108.8 kmol / day (100% pure)

=117 kmol/day (93% pure)
Propane entering = 8.2 kmol/day
(B) CO required =108.8 kmol/day
Syn gas required = 233.5 kmol/day

H2 entering = 233.5*0.492 = 114.9 kmol/day
(C) Side reactions :
(a) C3H6 + H2 C3H8
Propylene propane
(b) CH4 + CO + H2 C2H5 OH

Methane ethanol
1 kmol propane == 1 kmol propylene
Propane formed = propylene reacted
= propylene in feed – propylene for butanol
Propane produced = 108.8 – 108.6
= 0.2 kmol/day
Ethanol produced == CO reacted in side reaction
==0.2 kmol/day
Since the outlet of 1st reactor contains
Butaraldehyde = 108.6 kmol/day
Hydrogen = 114.9 – 108.8 – 0.2 – 0.2 = 5.7 kmol/day
Methane = (233.5*0.034) – 0.2 =7.739 kmol/day
27
Propane = 0.2 kmol/day
Ethanol = 0.2 kmol/day
CO2 = 233.5*0.005 = 1.1675 kmol/day
H2O = 233.5*0.003 = 0.7 kmol/day
Total feed inlet to flash column = 125.567 kmol/day
Since flash column less volatiles are collected as bottom and high volatiles are collected as top
(1) Since flash bottoms : (no losses in the column)
Butane = 1.26 kmol/day
Propane =0.2 kmol/day
Ethanol =0.2 kmol/day
Water = 0.2 kmol/day
Methane = 7.739 kmol/day
(2) Flash over head contains
CO2 =1.1675 kmol/day
H2 = 5.7 kmol/day
(3)butaraldehyde column :
F = total flash bottoms as feed to distillation= 118.70 kmol/day
XF = butanol in feed / total feed
=108.6/118.70 =0.915
XD = 0.1, XW = 0.99
W = Inlet to 2nd reactor = 107.46 kmol/day
Xw =butanal in reactor feed / total reactor feed(w)
= 106.4/107.46 = 0.99
28
FXF = D XD + WXW
118.7* 0.915 = D*0.1+ 107.46*0.99
D = 11.24 kmol/day
Distillate contents :
Butanol = 2.2 kmol/day
Ethanol = 0.2 k mol/day
Propane = 0.2 k mol/day
Bottoms of columns are fed to the 2nd reactor .the second reactor outlet are fed to flash
column .where the crude butanol (combination of n and iso butanols) separated as bottom
and the rest are flashed off.
CO = 100.7 kmol/day
CO2 = 1.081 kmol/day
CH4 = 7.35 kmol/day
Flash bottoms which are send to butanol column as feed contains
Butanol = 100 kmol/day
Selectivity 10.2:1 = n : iso butanol
n- butanol = 10.2*100/11.2 = 91 kmol/day
iso butanol = 9 kmol/day
butaraldehyde = 6.4 kmol/day
water = 0.649 kmol/day
F = 116.049 kmol/day
Therefore XF = 91/116.049
Desired residues composition
29
n- butanol xw = 0.995
Butaraldehyde = 0.003
Iso butanol = 0.001
Water = 0.001
Desired distillate composition
Iso butanol = 0.995
Butaraldehyde = 0.003
n- butanol xD =0.001
water = 0.001
FXF = D XD + W XW
116.049*0.784 = W*0.995 + (116.049-W)*0.001
W = 91.4325 kmol/day
D = F – W =24.6165
Conclusion :
N – butanol production = 91.4325 kmol/day (99.5% pure)
Iso butanol production = 24.6165 kmol/day
COMPRESSOR :
Component WEIGHT CPin heat cpout Heat
entering leaving
KG/day KJ/KG. K KJ/Day KJ/KG.K KJ/day
30
C3H6 4830 1.542 2220579.5 1.687 2753550.8
C3H8 378.4 1.7 191697 1.877 240072.6
CO 3220 1.04 997942 1.05 1143166.7
H2 242 14.41 1039191 14.4 1178271.2
CO2 133.82 0.86 34295 0.9 40995.9
CH4 54.12 2.18 35160 2.35 43000
H2O 13.29 1.87 7406 1.878 8437.5
TOTAL 4525135.5 5407493.6
Compressor heat load = 882358.2 kj/day = 10.212 kwatts
OXO UNIT :
selectivity =10.2:1 (N: ISO ) at T=900C & P=15.7 bar , Conversion 99.8%
C3H6 + CO + H2 C4H8 O
Propelene Syn gas Butanal(N ,iso)
31
INPUT
Out put :
Input : B1
Syn gas = 233.5 kmol/day
CO = 108.8 kmol/day
OUT PUT
H2 = 114.9 kmol/day
CH4 = 7.94 kmol/day
H2O = 0.7 kmol/day
H2 = 5.7 kmol/day
Propylene = 117 kmol/day
• ΔHR - ΔHr0 + ΔHP = ΔHT
• ΔHR = Enthalpy of reactants = 5,40,749.36 kJ/day
• ΔHr0 = standard enthalpy change of reaction = -1,16,840.85 kJ/day (99.8% conversion)
• ΔHP = enthalpy of products = 22,89,380.5 kJ/day
• ΔHT = total enthalpy change in the reactor = 27,13,289 kJ/day
FLASH COLUMN I :
In flashing P = 1 atm and T = 25 ͦ c
Vapor fraction = 0.207

Over head :
32 H2 = 5.7 kmol/day
VENT
B3
INPUT
Input :
Butaraldehyde = 108.6 kmol/day Bottom :

PRODUCT

Water = 0.2 for
Energy balance kmol/day
flash 1 :
H2 = 5.7 kmol/day
Energy balance for flash 1 :
33
fla s h1
S t re a m ID F L V
F rom B1 B1
To B1
P ha s e MIXED LIQUID VAP O R
S ubs t re a m: MIXE D
Mole F low lbm ol/ hr
N-B UT-01 9. 185928 8. 801158 . 3847696
IS O BU-01 . 9388018 . 8873431 . 0514586
P RO P A-01 . 7734551 . 0901058 . 6833493
CO . 0202090 7. 19606E-5 . 0201370
H2 . 5107376 5. 74143E-4 . 5101634
C H4 . 7440601 6. 65178E-3 . 7374084
C O2 . 1083939 2. 11193E-3 . 1062820
H2O . 0661386 4. 84910E-4 . 0656537
Tot a l F low lbm ol/ hr 12. 34772 9. 788502 2. 559222
Tot a l F low lb/ hr 783. 6641 702. 7929 80. 87116
Tot a l F low c uft/ hr 71. 31891 13. 60241 995. 6313
Tem pe ra ture F 194. 0000 77. 00000 77. 00000
P re s s ure ps i 227. 7092 14. 69595 14. 69595
Vapor F ra c . 1515923 0.0 1. 000000
Liquid F ra c . 8484077 1. 000000 0.0
S olid F ra c 0.0 0.0 0.0
Ent ha lpy Bt u/ lbm ol -87933. 17 -1.0334E + 5 -46581. 82
Ent ha lpy Bt u/ lb -1385. 510 -1439. 324 -1474. 113
Ent ha lpy Bt u/ hr -1.0858E + 6 -1.0115E + 6 -1.1921E + 5
Ent ropy Bt u/ lbm ol-R -80. 81411 -101. 9268 -31. 97145
Ent ropy Bt u/ lb-R -1. 273339 -1. 419636 -1. 011758
Dens ity lbm ol/ c uft . 1731339 . 7196154 2. 57045E-3
Dens ity lb/ c uft 10. 98817 51. 66680 . 0812260
Ave ra ge MW 63. 46628 71. 79780 31. 59990
Liq Vol 60F c uft/ hr 16. 83240 14. 05376 2. 778639
Distillate :
Butanol = 2.2 kmol/day

BUTYRALDEHYDE COLUMN: Water = 0.7 kmol/day
34 Ethanol = 0.2 k mol/day
Propane = 0.2 k mol/day

OVERHEAD
INPUT B5
Residue :
BOTTOMS
Input : Butaraldehyde = 108.6 kmol/day
Butaraldehyde = 108.6 kmol/day Butane = 1.26 kmol/day
35
d istill
Stream ID FE ED DIST RESI
Temp eratu re K 3 9 3.1 4 1 0.6 4 2 1.1
P res su re atm 2 .1 0 2 .5 0 2 .5 1
Vap o r Frac 0 .00 0 0 .00 0 0 .00 0
Mole Flo w k mol/h r 4 .18 4 3 .02 5 1 .15 9
Mass Flo w k g/h r 3 09 .97 2 2 24 .08 2 85 .89 0
Vo lume Flo w l /min 7 .32 8 5 .48 7 2 .11 4
En thalpy MMBtu /h r -1.2 16 -0.8 71 -0.3 27
Mole Flo w k mol/h r
N -BUT-01 1 .09 9 0 .11 5 0 .98 4
ISOBU -01 3 .01 6 2 .84 1 0 .17 5
N -BUT-02 0 .06 3 0 .06 2 trace
ISOBU -02 0 .00 7 0 .00 7 trace
H 2O
36
HYDROGENATOR AND FLASH 2 :
• Oprating conditions : T = 120 ͦ c & P= 1 atm
• Equillibrium conversion : 98%
C4H8 O + H2 CH3CH2CH2CHO
Butanal(N,iso) Butanol(N,Iso)
B6
INPUT OUTPUT
Input : Out put :
Butaraldehyde = 108.6 kmol/day Butanol = 100 kmol / day
Butane = 1.26 kmol/day Butane = 1.26 kmol / day
FLASH
Syn gas COLUMN 2 : kmol/day
= 216.2 CO2 = 100.7 kmol / day
CO = 1.081 kmol /day
H2O = 0.649 kmol /day
CH4 = 7.35 kmol /day
Butaraldehyde= 64 kmol / day
37
Butaraldehyde = 6.4 kmol / day
VENT
B3
INPUT
Butane = 1.26 kmol / day

PRODUCT
CO2 = 100.7 kmol / day
CO = 1.081 kmol /day CO2 =1.1675 kmol/day
H2O = 0.649 kmol /day H2 = 5.7 kmol/day
CH4 = 7.35 kmol /day Methane = 7.739 kmol/day
Butaraldehyde = 6.4 kmol / day Propane =0.2 kmol/day
Ethanol =0.2 kmol/day
38
HY DRGN TR
Stream ID REAC P ROD VAP O R LIQU ID
39
From HY DRGN TR B1 B1
To HY DRGN TR B1
P h ase VAP O R VAP O R VAP O R LIQU ID
Sub stream: MIXED
Mole Flo w lb mol/h r
N -BUT-01 8 .81 8 49 1 .0 96 3 30 2 .0 26 8 88 1 .0 69 4 42 0
ISOBU -01 .9 02 0 58 1 .3 15 2 70 1 .1 13 5 35 3 .2 01 7 34 8
P RO P A-0 1 .0 90 0 22 0 .0 90 0 22 0 .0 89 8 04 4 2 .1 7 65 3 E-4
H2 9 .76 2 06 9 .4 53 1 20 8 .4 53 0 97 0 2 .3 8 14 1 E-5
CO 9 .24 6 18 7 9 .24 6 18 7 9 .24 4 73 5 1 .4 5 19 8 E-3
CH 4 .6 74 6 14 5 .6 74 6 14 5 .6 74 3 80 9 2 .3 3 59 0 E-4
CO 2 .0 99 2 08 0 .0 99 2 08 0 .0 99 1 12 1 9 .5 8 93 0 E-5
H 2O .0 59 5 24 8 .0 59 5 24 8 .0 54 6 37 8 4 .8 8 69 8 E-3
N -BUT-02 0.0 2 .46 4 10 2 .0 47 1 59 5 2 .41 6 94 3
ISOBU -02 0.0 6 .84 4 84 6 .2 01 4 64 9 6 .64 3 38 1
Total Flo w lb mol/h r 2 9 .6 5 21 7 2 0 .3 4 32 3 1 1 .0 0 48 2 9 .33 8 41 1
Total Flo w lb /hr 9 9 9.8 18 2 9 9 9.8 18 2 3 0 8.5 41 6 6 9 1.2 76 6
Total Flo w cu ft/hr 7 0 32 .97 8 1 0 44 9 .4 0 4 3 08 .11 4 1 3 .7 1 16 2
Temp eratu re F 1 9 4.0 00 0 2 4 8.0 00 0 7 7 .0 0 00 0 7 7 .0 0 00 0
P res su re p si 2 9 .3 9 19 0 1 4 .6 9 59 5 1 4 .6 9 59 5 1 4 .6 9 59 5
Vap o r Frac 1 .00 0 00 0 1 .00 0 00 0 1 .00 0 00 0 0.0
Liq uid Frac 0.0 0.0 0.0 1 .00 0 00 0
Solid Frac 0.0 0.0 0.0 0.0
En thalpy Btu /lbmo l -44 2 07 .37 -78 1 01 .75 -48 2 03 .32 -1 .3 9 91 E+5
En thalpy Btu /lb -13 1 1.0 83 -15 8 9.1 30 -17 1 9.2 78 -18 8 9.9 67
En thalpy Btu /hr -1 .3 1 08 E+6 -1 .5 8 88 E+6 -5 .3 0 47 E+5 -1 .3 0 65 E+6
En trop y Btu /lbmo l-R -14 .04 6 12 -31 .89 4 11 1 4 .3 1 12 2 -12 4 .1 3 06
En trop y Btu /lb-R -.4 1 65 7 38 -.6 4 89 4 72 .5 10 4 41 1 -1.6 76 8 72
Dens ity lb mol/cuft 4 .2 1 61 6 E-3 1 .9 4 68 3 E-3 2 .5 5 44 4 E-3 .6 81 0 58 2
Dens ity lb /cu ft .1 42 1 61 4 .0 95 6 81 8 .0 71 6 18 7 5 0 .4 1 53 9
COPRODUCTION OF N-BUTANOL AND ISO-BUTANOL
Av erage MW 3 3 .7 1 82 1 4 9 .1 4 74 8 2 8 .0 3 69 6 7 4 .0 2 50 8
Liq Vo l 60 F cu ft/hr 3 1 .0 8 02 6 2 3 .4 3 54 5 9 .69 5 02 2 1 3 .7 4 04 3
2012
BUTANOL COLUMN :
Iso butanol = 24.6165 kmol/day
Butaraldehyde = 3 kmol/day
n- butanol =1 kmol/day
water = 0.15 kmol/day
OVERHEAD
B5
INPUT

BOTTOMS
Butaraldehyde = 6.4 kmol / day n- butanol =91.4325 kmol/day

(99.5% pure)
Butaraldehyde = 3 kmol/day
Iso butanol = 1 kmol/day
40
d istill
Stream ID FE ED DIST RESI
Temp eratu re K 3 9 3.1 4 1 0.6 4 2 1.1
P res su re atm 2 .1 0 2 .5 0 2 .5 1
Vap o r Frac 0 .00 0 0 .00 0 0 .00 0
Mole Flo w k mol/h r 4 .18 4 3 .02 5 1 .15 9
Mass Flo w k g/h r 3 09 .97 2 2 24 .08 2 85 .89 0
Vo lume Flo w l /min 7 .32 8 5 .48 7 2 .11 4
En thalpy MMBtu /h r -1.2 16 -0.8 71 -0.3 27
Mole Flo w k mol/h r
N -BUT-01 1 .09 9 0 .11 5 0 .98 4
ISOBU -01 3 .01 6 2 .84 1 0 .17 5
N -BUT-02 0 .06 3 0 .06 2 trace
ISOBU -02 0 .00 7 0 .00 7 trace
H 2O
41
CHAPTER
PROCESS EQUIPMENT
DESIGN
42
PROCESS EQUIPMENT DESIGN
DESIGN OF DISTILLATION COLUMN
X 0 0.013 0.075 0.141 0.211 0.28 0.37 0.459 0.555 0.65 0.773 1
8 9
Y 0 0.031 0.161 0.281 0.393 0.49 0.591 0.678 0.757 0.83 0.897 1
6 1
• Feed F= 309.5 kg/hr Feed composition XF =0.721
• Distillate rate, D=223.85 kg/hr Distillate composion XD = 0.995
• Residue rate, B=85.65 kg/hr Residue composition XB = 0.005
• Top allowance for column = 0.5 m Bottom allowance for column = 0.5 m
Feed is saturated liquid i.e., q =1
No of theoretical plate =n-1=14-1=13
Assume efficiency =65%
Actual no of Plate =13/0.65=20 plates
Tray spacing of 0.5m is assumed
43
Height of Distillation Column:
Height of Distillation Column = Tray Spacing*(no of Plate + 1)
Or
• Top allowance for column = 0.5 m Bottom allowance for column = 0.5 m
Column height =Top allowance for column + bottom allowance for column
+(tray spacing*number of spacings)
= 0.5 +0.5 +(19*0.5) = 10.5m
Column Diameter:
L
1. F= ∗√ (lv/¿)
V
FLv = Liquid Vapour flow factor
L = Liquid Mass flow rate (kg/s)
ρV= Density of Vapour (kg/m3)
ρL= Density of Liquid (kg/m3)
¿−lv
2. Umax=Kv∗√( )
lv
Umax= maximum vapour velocity (m/sec)
Kv= constant, which depends on tray spacing and FLV
At the top
Boiling point of n-butanol= 392k

Boiling point of i-butanol = 373k
Boiling Temperature at the Top (T1) = 368.9656k
ΡVT¿ PM /RT
ρvt =Vapour Density at Top
Average molecular weight of Top Product = 72.0496
Vapour Density at top ¿(1∗78.0496)/¿
44
Ρvt= 2.6966 kg/m3
ΡL = Density of n-butanol
Density of n-butanol=880kg/m3
Density of i-butanol = 880kg/m3
ΡL = (880*0.9912) + (870*0.008)
= 879.216
lVT
FLv = Slop of top operating line*
√ lLT
2.6966
√
= 0.11
879.216
= 0.00609
For tray spacing of 0.5m and FLV = 0.00609
Kv is found to be 0.09
¿−lv
Maximum Vapour Velocity, Umax¿ Kv∗√ ( )
lv
¿ 0.09∗√ (( 880−2.6966¿)/2.6966)¿
= 1.6233m/sec
Uactual = 0.75*Umax = 1.2173 m/sec
Vapour mass flow rate

Active area ¿
Uactual∗ρ
Vapour mass flow rate = D(R+1)
= 1390.42(2.82+1)
=1.089

Active area ¿
Uactual∗ρ
1.089
¿
1.2173∗2.6966
45
= 0.33m2
0.33
Total area =
0.65
=0.507
Column Diameter ¿ √ ¿
= 0.8036 m
AT THE BOTTOM:
Boiling Temperature at the Bottom (T2) = 379.426k
PM 2
ΡVT¿
RT 2
ρvt =Vapour Density at Top
Average Molecular Weight of top Product =
= 73.8188
1∗89.8188
Density at Bottom ¿
0.08206∗379.426
Ρvt= 2.8868 kg/m3
ΡL = Density of n-butanol
= 872.868kg/m3
lVb
FLv = Slop of top operating line*
√ lLb
2.8868
= 0.11
√ 872.868
= 0.006328
For tray spacing of 0.5m and FLV = 0.006328
Kv is found to be 0.09
46
¿−lv
Maximum Vapour Velocity, Umax¿ Kv∗√ ( )
lv
¿ 0.09∗√ (( 870−2.8868¿)/2.8868)¿
= 1.5598m/sec
Uactual = 0.75*Umax = 1.1698 m/sec

Active area ¿
Uactual∗ρ
Vapour mass flow rate = D(R+1)
= Feed mass flow(1.82+1)
= Total no of moles*molecular weight*(1.82+1) (for vapour)
= 1390.42(1.82+1)
=1.089

Active area ¿
Uactual∗ρ
0.023088
¿
1.1698∗2.8868
= 0.00683m2
0.00683
Total area = =0.0105m
0.65
Column Diameter ¿ √ ¿
= 0.71575 m
Large value for diameter will be chosen for design, hence D = 0.806m
Height of the Distillation column : 7m

Diameter of the Distillation column : 0.806m
47
CHAPTER
MECHANICAL DESIGN
48
MECHANICAL DESIGN OF DISTILLATION COLUMN
a) shell:
Diametre= 0.806m
operating pressure=0.5atm=50.6625kpa=0.51645 kg/cm2
design pressure=1.1*operating pressure=55.72kpa
operating temperature=124.570c
design temperature=139.0270c
shell material=carbon steel
-tray spacing=0.5m
top disengaging space=0.3m
skirt=3m
allowable stress for shell material=34335kpa
insulation=asbestos
insulation thickness=75mm
b) head: tori spherical head

material: carbon steel
allowable tensile stress=93195kpa
c)skirt support:
material-carbon steel
height=3.0m
d)nozzles:
49
no. of nozzles=4
e) trays:
no. of trays=20
spacing=0.5m=500mm
hole diameter=5cm
thickness=3mm
weir height=50mm
material for trays=material ss
1) calculations of shell thickness:
ts=PDi/2fj-p+c
Ts=thickness of shell(mm)=2.577m
P=design pressure(kg/cm2) Di=diameter of the shell(mm)
F=allowable/permissible tensile stress(kg/cm2)=950 kg/cm2
C=corrosion allowance(mm)=2mm
J=joint efficiency=0.85
ts=2.577mm
Taking the thickness of the shell as ts= 6mm
2)head-shallow dished&torispherical head

Th=PRcW/2fj
Rc-crown radius=outer diameter of the shell=1652mm
Rk=0.06Rc
W=stress intensification factor
W=1.77
Th=1.028mm
50
Thickness of head is th=1.028mm=(6mm taken as per standard thickness.)
Weight of the head:

Diameter=OD+OD/24+2SF+2/3icr
OD=outside diameter of the shell=1652mm=65 inch
Icr=inside cover radius=0.75 inch
Sf =straight flange length=1.5 inch
Diameter=65+65/24+2(1.5)+2/3*(0.75)= 71.20 inch
Diameter(d)=1808.69mm = 1.8087m
Weight of head= Π/4[1.8087]2*[6*10-3]*7700
Weight of head = 144.26kg <2670kg
3) calculation of stress:
1)axial tensile stress due to pressure
Fap= pdi/4(ts-c) = 0.5681*1640/4(6-2) = 58.23 kg/cm2
This is same throught the column height
2)circumferential stress:
2 Fap= 2*58.23 = 116.46 kg/cm2
3)compressive stress e dead loads:
a) compressive stress due to weight of shell up to a distance x in meter
fds=weight o shell= (Π/4(Do2-Di2)* *x)/ (Π/4(Do2-Di2)
= *x = 0.0077*100 = 0.772*X kg/cm2
cross setion area of shell fds
di,do-internal and external diameter of shell
Ss-density of the shell
Fds= 0.7720 *X kg/cm2
Dm=mean diameter of the shell(cm)
Ts=thickness of the shell(cm),
51
C=corrosion allowance
b) Compressive stress due to the weight of the insulation at height(x)m
fd(ins)
dins=diameter of the insulation
tins=thickness of the insulation
sins=density of the insulation
dm=mean diameter of the shell = 1.802 m
sins= Π dins*tins sins(x)/Π DM[ts-c] = 575 kg/m3 = 0.000575 kg/cm3
tins=75mm = 7.5 cm
dins=dc+2ts+2tins
dins=1640+2*6+2*75 = 1802 mm = 1.802 m
dm= DC+(Dc=2ts)/2 = 1640+1640+2*6/2 = 1646 mm = 164.6 cm
C)compressive stress due to liquid&tray in the column upto height(x)m
liquid &tray weight for height(x)
fliq=[(x-0.3)/0.5+1]Π/4di*sliquid
fliq=[x-top disengaging space]/tray spacing)+1] Π/4di*sliquid
fliq= fliq/Πdm(ts-c)= (x+0.16)*5754/(Π*164.6)*(0.6-0.2) = 27.818+4.45 kg/cm2
d)tensile stress due to wind loads in self supporting vessel
fwx=Mw/z
mw=bending moment due to wind load=wind load*distance/2
z=modulus for the area of the shell=Π/4*dm2(ts-c)
fwx=0.7pwx2*2/Π*dm(ts-c) = 1.4*121.9*10-4*104/Π*164.2*(6-2)
fwx=0.825x2kg/cm2
stress due to seismic load are neglected
calculation of resultant longitudinal stress(upwind side)

tensile:
ftmax= fwx+fap-fds
fwx=stress due to wind load=0.825x2
fap=axial tensile stress due to pressure=58.23
fds =stress due to wind load=0.77x
52
ftmax=fj
f=allowable stress=950kg/cm2
j=joint factor=0.85
950*0.85=0.825x2+58.23-0.77x
From this height (H)=30.60m
4) calculation of resultant longitudinal stress(downwind side):

Fcmax= fwx+fap-fds=o.825k2-58.23+0.77x
Fcmax=0.125E(t/do)
E=elastic modulus=2*106kg/cm2
T=shell thickness=6mm
Do=1652mm
Fcmax=907.99cm2
907.99=0.825x2-58.23+0.77x
From this height (X)=33.75m.
 Calculated height is grater than the actual tower height so we conclude that design is
safe and design calculations are acceptable.
 The thickness 6mm is sufficient through out the shell.
DESIGN OF SKIRT SUPPORT:

Total ht of column including skirt height(H)=18+3+0.3
=21.3m
Min weight if vessel = (Wmin) = Π[Di+ts]*ts*[H-skirt height]* +2[2670]
Di=shell dia=1.64m
Ts=0.006m
=shell material density=7700kg/m3
(Wmin)=9711.92kg
Mean weight of column (Wmax) = ww+wj+we+wa
Ww=weight of shell during test=1987.71kg
Wi=weight of insulation = Π/4*[(dins)2-(do)2]*H*
=Π/4*[(1.802)2-(1.652)2]*21.3*575
53
=4983.68kg
We=weight of water during test = Π/4*(di)2[H-pj]*
= Π/4*(1.64)2[21.3-3]*1000
=36657.04kg
Wa =weight attachments=7100kg
Wmax= 52728.42kg =517.26KN
Period of vibration at min dead wt
Tmin= 6.35*10-5(H/D)3/2 * Wmin1/2/ts1/2
Tmin= 6.35*10-5(21.3/1.64)3/2 * 950271/2/0.0061/2
Tmin= 0.374sec
K1=0.7 cylindrical vessel
K2=1.0 [vibration period less then 0.5 sec]
K2=2
P1=40-100kg/m2 p2=100-200kg/m2
Period of vibration max dead wt:

Tmax = 6.35*10-5*(23.1/1.64)1.5*(517.26/0.006)0.5
Tmax = 0.9856
K2=2
Total head due to wind acting on the
Mean weight of column (Wmax) = ww+wj+we+wa
Ww=weight of shell during test=1987.71kg
Wi=weight of insulation = Π/4*[(dins)2-(do)2]*H*
=Π/4*[(1.802)2-(1.652)2]*21.3*575
=4983.68kg
We=weight of water during test = Π/4*(di)2[H-pj]*
= Π/4*(1.64)2[21.3-3]*1000
=36657.04kg
Wa =weight attachments=7100kg
Wmax= 52728.42kg
=517.26KN
54
Period of vibration at min dead wt

Tmin= 6.35*10-5(H/D)3/2 * Wmin1/2/ts1/2
Tmin= 6.35*10-5(21.3/1.64)3/2 * 950271/2/0.0061/2
Tmin= 0.374sec
K1=0.7 cylindrical vessel
K2=1.0 [vibration period less then 0.5 sec]
K2=2
P1=40-100kg/m2 p2=100-200kg/m2
Period of vibration max dead wt:
Tmax = 6.35*10-5*(23.1/1.64)1.5*(517.26/0.006)0.5
Tmax = 0.9856
K2=2
Total head due to wind acting on the bottom & upper part of vessel:
Plm=k1k2P1H1D (up to 20)
Puw= k1k2P2H2D k1=0.7(cylinder)
Pw= wind pr load
P1=wind pr =100kg/m2
Min weight condition=Di=1.64m
Max weight condition=Dins=1.802m
Pw(min)= 0.7*1*100*1.64*21.3
= 2445.24kg
Pw(max)=0.7*2*100*1.802*21.3
=5373.564kg
bottom & upper part of vessel:
Plm=k1k2P1H1D (up to 20)
Puw= k1k2P2H2D k1=0.7(cylinder)
Pw= wind pr load
P1=wind pr =100kg/m2
Min weight condition=Di=1.64m
Max weight condition=Dins=1.802m
Pw(min)= 0.7*1*100*1.64*21.3
55
= 2445.24kg
Pw(max)=0.7*2*100*1.802*21.3
=5373.564kg
Min & max wind momentum:

(Mw)min= Pw(min)*H/2 + puw[(h1)+(h2/2)]
(Pum)min=0.7*1*200*1.3*1.64=298.48kg
(Pum)max=0.7*1*200*1.3*1.802=655.928kg
(Mw)min = (2445.24*20)/2+298.48[20+(1.3/2)]
= 24771.53kg-m
(Mw)max =(5373.564*20)/2 + 655.928[20+(1.3/2)]
= 67280.55kg-m
As the thickness of the skirt is expected to small, assumed Di=Do=1.64
fzwm(min)=4Mw(min)/ΠD2t=4*24771.53/Π*(1.64)2*t
= 11726.68/t kg/m2
Fzwm(max) =4Mw(min)/ΠD2t= 4*67280.55/Π*(1.64)2*t
=31850.18/t kg/m2
Minimum and maximum dead load stresses:
Fzm(min)=Wmin/ ΠDt= 9711.92/Π*1.64*t = 1885/t kg/m2
Fzm(max)=Wmax/ ΠDt=5272.42/Π*1.64*t = 10234.19/t kg/m2
Maximum tensile stress without any eccentric load is computed as follows.
(Tensile) fz= σzwm(min)-fzw(min)
Fz=fj
950*104(0.85) = 11726.68/t-1885/t
t = 1.218*10-3m = 1.218mm
Maximum compressive load:
compressive(fz) = fzwm(max) = fzw (max)
fz = 0.125ϵ(t/do)
= 0.125*2*105*106*t/1.64
=1.5244*1010*t kg/m2
56
1.5244*1010t = 31850.18 + 10234.19/t

t = 1.66*10-3m=1.66mm
As per is 2855-1969, minimum corroded skirt thickness is 7 mm.
Providing 1mm corrosion allowance, a standard 8 mm thick plate can be used for
skirt.
CHAPTER
COST ESTIMATION
57
COST ESTIMATION :
An acceptable plant must design a process that is capable of operating under conditions, which
yield a profit. Capital must be allocated for direct labor and equipment. Besides many plant expenses
many other indirect plant expenses are included and these must be included in the total cost analysis of
the plant.
A capital investment is required for any other industrial process. the capital investment plus
working capital which must be available pay salaries , keep raw materials and product on hand handle
other special items required a direct cash outlay thus in an analysis of costs, manufacturing costs and
general expenses including income tax must be taken into consideration.
Capital investment is defined as the total amount of money needed to supply the necessary plant
and manufacturing facilities plus the amount of money required as working capital for operating of the
facilities.
TOTAL CAPITAL COST = FIXED CAPITAL INVESTMENT + WORKING CAPITAL
FIXED CAPITAL INVESTMENT =DIRECT COST + INDIRECT COST
Fixed capital investment represents the capital necessary for the installed process equipment with
all auxiliaries that are neede for complete process operation.
Expenses for piping; instruments, insulation, foundations and site preparation are typical
examples of costs included in the manufacturing fixed capital investment.
58
DIRECT COST :
1.Purchased Equipment Cost : (in crores)
Equipment Units Cost per unit Total cost

1 Oxo reactor 1 0.53 0.53
2 Hydrogenator 1 0.45 0.45
3 Distillation column 2 0.0781 0.1562
4 Heater 1 0.036 0.036
5 Compressor
2 0.036 0.072
6 Mixer 3 0.02 0.06
7 Flash columns 2 0.03 0.06
8 Miscellaneous
0.1028
(storage and handling)
TOTAL= 1.467
Equipment installation cost : (other costs , oc)
For fluid processing unit
1.Installation cost :
Installation cost is 10-15% of PEC
Assuming 15%
Therefore IC = Rs. 0.22005 crores
2. PIPING & INSTALLATION COST
It is 25 - 18% of PEC.
59
Assuming 20%
Therefore PIC = Rs. 0.2934 crores
3. INSTRUMENT & CONTROL INSTALLED
It is 50 - 70% of PEC.
Assuming 60%.
Therefore ICI=Rs.0.8802 crores.
4. ELECTRICAL EQUIPMENT COST
It is 10-40% of PEC
Assuming 25%.
Therefore EEC=Rs.0.36675 crores.
5.BUILDING PROCESS AUXILIARY
It is 10-70% of PEC
Assuming 45%
Therefore BPA=Rs.0.66015 crores.
6.SERVICE FACILTIES
It is 30-80% of PEC.
Assuming 55%
Therefore SF=Rs.0,80685 crores.
7.YARD IMPROVEMENT
It is 10-20% of PEC
Assuming 15%.
Therefore YI=Rs0.22005 crores.
8.LAND
It is 10-20% of PEC
Assuming 15%.
Therefore LC=Rs.0.22005 crores.
9.TECHNOLOGY & ENGG FIELD
60
It is 15% of PEC
Therefore TEF=Rs.0.22005 cores.
TOTAL=OC=Rs.3.88755 crores.
TOTAL DIRECT PLANT COST(DPC):
DPC=PEC+OC=1.467+3.88755=5.35455 crores.
INDIRECT COST :
These include expenses which are not directly involved with materials and labor of actual installation complete
facility.
1.ENGG.&SUPERVISION COST :
It is 15-35% of DC.
Assuming 25%
Therefore ESC = Rs. 1.33864 crores
2. CONSTRUCTION EXPENSES & CONTRACTORS FEE
It is 30% of DC.
Therefore CEC = Rs. 1.60636 crores
3. CONTINGENCY
It is 8-20% of DC.
Assuming =15%
Therefore contingency=Rs. 0.80318 crores.
TOTAL INDIRECT COST = Rs. 3.74818 crores
Therefore FIXED CAPITAL INVESTMENT (FCI)
FCI = DIRECT COST + INDIRECT COST
= Rs. 9.10273 crores
WORKING CAPITAL INVESTMENT
It is 10 - 20% of FCI
Assuming 15%
Therefore WCI =Rs. 1.36541 crores
TOTAL CAPITAL INVESTMENT
61
TCI = FCI + WCI
=Rs. 10.46814 crores
ESTIMATION OF TOTAL PRODUCT COST
Total product cost = manufacturing cost + general expenses
Manufacturing cost = fixed charges + direct production cost + plant overhead cost
1. FIXED CHARGES
a) DEPRICATION
It is 10% of FCI
Therefore deprecation = Rs. 0.91027 crores
b) LOCAL TAXES
It is 3 - 4% of FCI
Assume 3.5%
Therefore local taxes=Rs. 0.3186 crores
c) INSURENCE
It is 0.4-1% of FCI
Assume 0.5%
Therefore insurence = Rs. 0.04551 crores.
Total fixed charges=Rs.1.27438 crores.
But fixed charges=15% of TPC
Therefore TPC=fixed charges*(100/15)
=Rs.8.49587 crores.
DIRECT PRODUCTION COST :
A) Raw Materials
Assuming 300 Working days per year
It is 20% of TPC
=Rs.1.69917 crores
b}OPERATING Labour
62
It is 10-20% of TPC
Assuming 15%
Therefore O.L=Rs.1.27438 crores
c) Direct Supervisory & Electrical Labour
It is 20% of operating labour
Therefore DS & EL = Rs. 1.69917 crores
d) Utilities:
It is 10-20% of TPC
Assuming 15%
Therefore cost of utilities = Rs. 1.27438 crores
e) MAINTENANCE:
It is 2 - 10.5% of FCI.
Assuming 6%
Therefore MC = Rs. 0.50975 crores.
f}OPERATING SUPPLIES:
it is 10-20% of maintaince cost
Assuming 15%
Therefore OSC=Rs.1.27438 crores
g)LABORATORY CHARGES:
it is 10-20% of operating labor cost
Assuming 15%
h)PATENTS AND ROYALTIES:
It is 2-6% of TPC
Assuming 4%
TOTAL DIRECT PRODUCTION COST=Rs.9.34544 crores.
3.PLANT OVERHEAD COST:
63
It is 50-70% of operating labor,supervisory and maintenance.
Assuming 60%
Therefore POC=Rs.2.08998 crores
TOTAL MANUFACTURING COST=FC+DPC+POC
=1.27438+9.34544+2.08998=12.7098 crores.
GENEREL EXPENSES
ADMINISTRATION COST:
It is 20-30% of operating labor
Assuming 25%
Therefore AC=Rs.0.3186 crores.
DISTRIBUTION & MARKETING COST:
It is 2-20% of TDPC
Assuming 15%
Therefore DAMC=Rs.1.40182 crores.
RESEARCH AND DEVELOPMENT COST:
It is 3% of TDPC
Therefore RDC=Rs.0.28036 crores.
Total general expenses=Rs.2.00078. crores.
Therefore,TOTAL PRODUCTION COST=MC+GE
=2.00078+12.7098
=14.71058 crores.
product cost/kg production(kg/day) cost of kg(production/day)
n-butanol 425 2055 873375
i-butanol 380 5370 2040600
total 2913975.
total selling price=2913975*300
=87.41925 crores
64
gross earnings=selling orice-production cost
=87.41925-12.7098
= 74.70945
let tax rate be 12%
net profit = GE(1-0.12) =65.74432 crores
Rate of return = (net profit/total capital investment) × 100 = 76.09%
Break even point:
Let ‘N’ be the break even production rate in TPA

Raw material cost per ton of product = 282.82*24.31+717.171*10.15 = 14154.63 RS
Total fixed cost = total depreciation cost + Plant overhead cost + Administration cost
+Distribution and selling cost + Research and development cost
= 131.3039556 crores
Direct production cost = (raw material cost per ton of product) × N = 14154.63N
Selling cost = Selling price × 1000 × N = 110000 N
At break even point,
Fixed charges + Direct production cost = Selling cost
131.3039556*e7 + 14154.6 N = 30000 N
Then, N = 82898.82 TPA
The break even production is 82898.082 TPA
At Breakeven Point, Capacity = 82898.082 TPY In order to get profit, production rate should be
greater than 82898.082 TPY
Annual Rate of Income =100 * (NP/IC)
=100* (15569392/121713026)
=12.79
=13
Payout Period =Depreciation fixed investment /( Profit * Depreciation)
=(127798677/(15569392-121.71))
= 8 years
65
CHAPTER
10
SITE CONSIDERATIONS
AND PLANT LOCATION
66
SITE CONSIDERATIONS AND PLANT LOCATION
Plant location and plant site selection:
The other considerations are as follows:

1. Location, with respect to the marketing
2. Raw material supply
3. Transportation facilities
4. Availability of labor
5. Availability of utilities: water, fuel, power
6. Environmental impact, and effluent disposal
7. Local community considerations
8. Climate
9. Availability of suitable land
10. Political and strategic considerations
Plant layout:
The parameters considered to arrive at the plant layout are:
1.Economic considerations:
Construction and operating costs .The cost of construction can be minimized by adopting
a layout that gives the shortest run of connecting pipe between equipment and the least of
structural steel work.
2. Process requirements:
The locations of certain pieces of equipment are based on the process requirement. For
example, a condenser is placed sufficiently high so as to have a barometric leg.
3. Operation:
Equipment that needs t have frequent operator attention should be located convenient the
control room. Valves, sample points and instruments should be located at convenient positions
and heights. Sufficient working space and headroom must be provided to allow easy access to
equipment.
4. Maintenance:
Heat exchangers need to be sited to do that the tube bundles can easily be removed.
Vessels that require frequent replacement of catalyst or packing should be located on the outside
of buildings. Equipment that requires dismantling for maintenance, such as compressors and
large pumps, should be placed under cover.
67
5. Safety:
Blast walks way may be needed to isolate potentially hazardous equipment, and confine
the effects of an explosion. At least two escape routes for operators must be provided from each
level in process buildings.
6. Plant expansion:
Equipment should be located so that it can be conveniently tied in with any future
expansion of the process. Space should be left on pipe alleys for future needs, and service pipes
over-sized to allow for future requirements.
7. Modular construction:
In recent years, there has been a move to assemble sections of the plant as the plant
manufacturer’s site. These modules will include the equipment, structural steel, piping etc.
1.Parking
2. Canteen
3. Security
4. Training center
5. Administrative building
6. Laboratories(RAD)
7. Fire section
8. Boilers
9. Control room
10. Process
11. Storage
12. Work shop
13. Expansion
14. Lab
15. Raw materials
The various needs and conditions must be defined clearly before considering a
site to locate a factory. The main factor that is to be considered for a factory is to be
considered for deciding the location of site for a factory is that it should yield maximum
possible benefit with minimum possible efforts.
The many number of factors that are to be taken into account to satisfy the statement are broadly
divided into two groups.
1. Primary factors
68
2. Secondary factors
1. Primary factors:
a) Availability of raw materials:
The location f the factory is influenced by source of raw materials. It is definitely
advantageous thing if the factory is located near the source of raw material.
For the purpose of locating a factory the raw materials are classified as:
 Materials included in the manufactured articles without loss of weight

 Materials found almost everywhere
 Materials included in the manufactured articles with some loss of weight
Therefore if the raw materials are of:

Class-a: in the above 3 points, factory may be located at source of raw materials
Class-b: the location of factory at market area is advantageous
Class-c: The location of factory at the source of materials is advantageous.
b) Availability of power, water and fuel:

Power is an essential requirement for a factory. Therefore sufficient quantity of power
should be available for the needs of factory without failure. The source of power may be
classified as:
o External source
o Internal source
c) Availability of labor:
Availability of required labor in the requisite type is also an essential consideration.
Density of population is not only consideration. The people in the surrounding areas willing to
work in the factory depends on maturity of citizens, influence of local industries, live hood etc.
d) Climate and atmospheric conditions:
If the climate and atmospheric conditions are not favorable, employees may not be
willing to work. The second consideration is precision machines get spoiled.
o If there is such fluctuation of temperature.
o If the factory is within vicinity of sea breeze it requires a cool atmosphere.
In modern the temperature inside the factory is regulated by scientific
methods.
e) Market facilities:
Facilities for marketing the finished quota should be available. If the markets are near to
the factory.
o The cost of transportation will be less
o The finished goods will be known in market.

o The factory can give quick service to the customers.
69
f) Transportation facilities:
Economical conveyance and quick transport facilities should always be available.
Whenever the raw materials etc. are to be transported to the factory or finished products to the
markets, road, rail, water consideration.
g) Scope of expansion:
The scope of future expansion should be considered when the increase of demand for
finished good is anticipated either in short or long run.
2. Secondary factors:
The following factors are also to be taken into account before selecting a site for a
factory.
1. Cost of land
2. Laws governing the area
3. Fire protection
4. Availability of water for the employees and factory purposes
5. Availability of proper daily necessities to the employees
6. Progressive attitude of citizens of the area towards the industry
7. Mental development of people of area
8. Residential housing to employees
9. Educational facilities to the children of employees
10. Health and welfare services
Conclusion:
Practically it is not possible to select a site which will satisfy all the above conditions.
Sometimes a site satisfying all the above conditions may not be possible. In such cases
advantages and disadvantages should be weighed carefully while selecting the best site possible.
In some cases one or two factors may play greater importance.
The layout of a chemical plant is not an exact science but rather an art as it
embraces high degree of experience coupled with the need to anticipate the human element in
both in operation and maintenance. It is however the most important factor in a process plant
project in that a carefully planned functional arrangement of equipment, building and pipe work
is the key to economical construction and efficient operation.
70
Plant layout plays an important role in determining the construction and

manufacturing costs. Since each plant differs in many ways and no two plants sites are exactly
alike there is nothing like an ideal plant layout. However proper layout in each case will include
arrangement of processing areas, storage area and handling areas in an efficient manner.
Rational design must include arrangement of processing areas storage areas and handling areas
in efficient coordination and with regard to such factors as:
o
o New site development or additional to previously developed site
o Future expansion
o Economic distribution of services- water, process steam, power and gas.
o Weather conditions are they amenable to outdoor conditions.
o Safety consideration possible hazards of fire, expansion and flames
o Building code requirements
o Waste disposal problems
o Sensible use of floor and elevation of space
The storage facilities for the raw material, intermediate and finished products may be
located in isolated areas or in adjoining areas reduce materials handling. It may reduce an
obstacle future expansion of the plant. So here the storage tanks are laid our conveniently so that
they may not become an obstacle to future expansion site.
Expansion is kept in mind and as the question of multiplying the number of units r
increasing the size prevailing unit, is more important a site for future expansion is also provided.
Road ways of correct capacity and the right location are made so that the transportation is easier
and convenient.
71
PLANT LAYOUT
72
UTILITIES
The word "Utilities" is now generally used for the ancillary services needed in the operation of
any production process. These services will normally be supplied from a central site facility; and
will include:
 Electricity.
 Steam, for process heating.
 Cooling water.
 Water for general use.
 Demineralised water.
 Compressed air.
 Inert-gas supplies.
 Refrigeration.
 Effluent disposal facilities.
Electricity
The power required for electrochemical processes; motor drives, lighting, and general use, may
be generated on site, but will more usually be purchased from the local supply company (the
national grid system in the UK).
The voltage at which the supply is taken or generated will depend on the demand. For a large site
the supply will be taken at a very high voltage, typically 11,000 or 33,000 V. Transformers will
be used to step down the supply voltage to the voltages used on the site. In the United Kingdom a
three-phase 415-V system is used for general industrial purposes, and 240-V single-phase for
lighting and other low-power requirements. If a number of large motors is used, a supply at an
intermediate high voltage will also be provided, typically 6000 or 11,000 V.
A detailed account of the factors to be considered when designing electrical distribution systems
for chemical process plants, and the equipment used (transformers, switch gear and cables).
Steam
The steam for process heating is usually generated in water tube boilers; using the most
economical fuel available. The process temperatures required can usually be obtained with low-
pressure steam, typically 2.5 bar (25 psig), and steam is distributed at a relatively low mains
pressure, typically around 8 bar (100 psig). Higher steam pressures, or proprietary heat-transfer
fluids, such as Dowtherm, will be needed for high process temperatures. The generation,
distribution and utilization of steam for process heating in the manufacturing industries.
Combined heat and power (co-generation)
The energy costs on a large site can be reduced if the electrical power required is generated on
site and the exhaust steam from the turbines used for process heating. The overall thermal
efficiency of such systems can be in the range 70 to 80 per cent; compared with the 30 to 40 per
cent obtained from a conventional power station, where the heat in the exhaust steam is wasted
in the condenser. Whether a combined heat and power system scheme is worth considering for a
73
particular site will depend on the size of the site, the cost of fuel, the balance between the power
and heating demands; and particularly on the availability of, and cost of, standby supplies and
the price paid for any surplus power electricity generated.
On any site it is always worth while considering driving large compressors or pumps with steam
turbines and using the exhaust steam for local process heating.
Cooling water
Natural and forced-draft cooling towers are generally used to provide the cooling water required
on a site; unless water can be drawn from a convenient river or lake in sufficient quantity. Sea
water, or brackish water, can be used at coastal sites, but if used directly will necessitate the use
of more expensive materials of construction for heat exchangers.
Water for general use
The water required for general purposes on a site will usually be taken from the local mains
supply, unless a cheaper source of suitable quality water is available from a river, lake or well.
DemineraLised water
Demineralised water, from which all the minerals have been removed by ion-exchange, is used
where pure water is needed for process use, and as boiler feed-water. Mixed and multiple-bed
ion-exchange units are used; one resin converting the cations to hydrogen and the other removing
the acid radicals. Water with less than 1 part per million of dissolved solids can be produced.
Refrigeration
Refrigeration will be needed for processes that require temperatures below those that can be
economically obtained with cooling water. For temperatures down to around 10°C chilled water
can be used. For lower temperatures, down to-30°C, salt brines (NaCl and CaCl2) are used to
distribute the "refrigeration" round the site from a central refrigeration machine. Vapour
compression machines are normally used.
Compressed air
Compressed air will be needed for general use, and for the pneumatic controllers that are usually
used for chemical process plant control. Air is normally distributed at a mains pressure of 6 bar
(100 psig). Rotary and reciprocating single-stage or two-stage compressors are used. Instrument
air must be dry and clean
Inert gases
Where large quantities of inert gas are required for the inert blanketing of tanks and for
purging this will usually be supplied from a central facility. Nitrogen is normally used, and is
manufactured on site in an air liquefaction plant, or purchased as liquid in tankers.
74
Effluent disposal
Facilities will be required at all sites for the disposal of waste materials without creating a public
nuisance.
ENVIRONMENTAL CONSIDERATIONS
All individuals and companies have a duty of care to their neighbours, and to the
environment in general. In the United Kingdom this is embodied in the Common Law. In
addition to this moral duty, stringent controls over the environment are being introduced in the
United Kingdom, the European Community, the United States, and in other industrialized
countries and developing countries.
Vigilance is required in both the design and operation of process plant to ensure that legal
standards are met and that no harm is done to the environment.
Consideration must be given to:
 All emissions to land, air, water.

 Waste management.
 Smells.
 Noise.
 The visual impact.
 Any other nuisances.
 The environmental friendliness of the products.
Waste management
Waste arises mainly as byproducts or unused reactants from the process, or as off
specification product produced through mis-operation. There will also be fugitive emissions from
leaking seals and flanges, and inadvertent spills and discharges through mis-operation. In
emergency situations, material may be discharged to the atmosphere through vents normally
protected by bursting discs and relief value
The designer must consider all possible sources of pollution and, where practicable,
select processes that will eliminate or reduce (minimize) waste generation.
Unused reactants can be recycled and off-specification product reprocessed. Integrated

processes can be selected: the waste from one process becoming the raw material for another.
For example, the otherwise waste hydrogen chloride produced in a chlorination process can be
used for chlorination using a different reaction; as in the balanced, chlorination
oxyhydrochlorination process for vinyl chloride production. It may be possible to sell waste to
75
another company, for use as raw material in their manufacturing processes. For example, the use
of off-specification and recycled plastics in the production of lower grade products, such as the
ubiquitous black plastics bucket.
Processes and equipment should be designed to reduce the chances of mis-

operation; by providing tight control systems, alarms and interlocks. Sample points, process
equipment drains, and pumps should be sited so that any leaks flow into the plant effluent
collection system, not directly to sewers. Hold-up systems, tanks and ponds, should be provided
to retain spills for treatment. Flanged joints should be kept to the minimum needed for the
assembly and maintenance of equipment.
When waste is produced, processes must be incorporated in the design for its
treatment and safe disposal. The following techniques can be considered:
1. Dilution and dispersion.

2. Discharge to foul water sewer (with the agreement of the appropriate authority).
3. Physical treatments: scrubbing, settling, absorption and adsorption.
4. Chemical treatment: precipitation (for example, of heavy metals), neutralisation.
5. Biological treatment: activated sludge and other processes.
6. Incineration on land, or at sea.
7. Landfill at controlled sites.
8. Sea dumping - (now subject to tight international control).
Gaseous wastes
Gaseous effluents which contain toxic or noxious substances will need treatment before
discharge into the atmosphere. The practice of relying on dispersion from tall stacks is seldom
entirely satisfactory. Witness the problems with acid rain in Scandinavian countries attributed to
discharges from power stations in the United Kingdom. Gaseous pollutants can be removed by
absorption or adsorption . Finely dispersed solids can be removed by scrubbing, or using
electrostatic precipitators. Flammable gases can be burnt.
Liquid wastes
The waste liquids from a chemical process, other than aqueous effluent, will usually be
flammable and can be disposed of by burning in suitably designed incinerators. Care must be
taken to ensure that the temperatures attained in the incinerator are high enough to completely
destroy any harmful compounds that may be formed; such as the possible formation of dioxins
when burning chlorinated compounds. The gases leaving an incinerator may be scrubbed, and
acid gases neutralised.
In the past, small quantities of liquid waste, in drums, has been disposed of by dumping at sea or
in land-fill sites. This is not an environmentally acceptable method and is now subject to
stringent controls.
Solid wastes
76
Solid waste can be burnt in suitable incinerators or disposed by burial at licensed land-fill
sites. As for liquid wastes, the dumping of toxic solid waste at sea is now not acceptable.
Aqueous wastes
The principal factors which determine the nature of an aqueous industrial effluent and on
which strict controls will be placed by the responsible authority are:
1. pH.
2. Suspended solids.
3. Toxicity.
4. Biological oxygen demand.
The pH can be adjusted by the addition of acid or alkali. Lime is frequently used to
neutralise acidic effluents. Suspended solids can be removed by settling, using clarifiers. For
some effluents it will be possible to reduce the toxicity to acceptable levels by dilution. Other
effluents will need chemical treatment.
The oxygen concentration in a water course must be maintained at a level sufficient
to support aquatic life. For this reason, the biological oxygen demand of an effluent is of utmost
importance. It is measured by a standard test: the BODS (five-day biological oxygen demand).
This test measures the quantity of oxygen which a given volume of the effluent (when diluted
with water containing suitable bacteria, essential inorganic salts, and saturated with oxygen) will
absorb in 5 days, at a constant temperature of 20°C. The results are reported as parts of oxygen
absorbed per million parts effluent (ppm). The BODS test is a rough measure of the strength of
the effluent: the organic matter present. It does not measure the total oxygen demand, as any
nitrogen compounds present will not be completely oxidised in 5 days. The Ultimate Oxygen
Demand (UOD) can be determined by conducting the test over a longer period, up to 90 days. If
the chemical composition of the effluent is known, or can be predicted from the process flow
sheet, the UOD can be estimated by assuming complete oxidation of the carbon present to carbon
dioxide, and the nitrogen present to nitrate:
UOD = 2.67C + 4.57N
where C and N are the concentrations of carbon and nitrogen in ppm.

Activated sludge processes are frequently used to reduce the bilogical oxygen demand ofan
aqueous effluent before discharge.
Where waste water is discharged into the sewers with the agreement of the local water
authorities, a charge will normally be made according to the BOD value, and any treatment
required. Where treated effluent is discharged to water courses, with the agreement of the
appropriate regulatory authority, the BODS limit will typically be set at 20 ppm.
Noise
77
Noise can cause a serious nuisance in the neighborhood of a process plant. Care needs to
be taken when selecting and specifying equipment such as compressors, air-cooler fans, induced
and forced draught fans for furnaces, and other noisy plant. Excessive noise can also be
generated when venting through steam and other relief valves, and from flare stacks. Such
equipment should be fitted with silencers. Vendors' specifications should be checked to ensure
that equipment complies with statutory noise levels; both for the protection of employees, as well
as for noise pollution considerations. Noisy equipment should, as far as practicable, be sited well
away from the site boundary. Earth banks and screens of trees can be used to reduce the noise
level perceived outside the site.
Visual impact
The appearance of the plant should be considered at the design stage. Few people object
to the fairyland appearance of a process plant illuminated at night, but it is a different scene in
daylight. There is little that can be done to change the appearance of a modern style plant, where
most of the equipment and piping will be outside and in full view, but some steps can be taken to
minimize the visual impact. Large equipment, such as storage tanks, can be painted to blend in
with, or even contrast with, the surroundings. Landscaping and screening by belts of trees can
also help improve the overall appearance of the site.
Legislation
It is not feasible to review the growing body of legislation covering environmental
control in this short chapter. All that can be done is to give a brief resume of the principal
legislation current in the United Kingdom. Legislation and control procedures in other countries
are likely to be similar in scope and practice.
Stricter legislation and tighter control of discharges into the environment are being introduced
in most countries. The specialist texts brought out by publishers catering for management topics,
and by the government departments, should be consulted for up-to-date information on
environmental legislation.
The key legislation in the United Kingdom is:
 The Environmental Protection Act (EPA), 1991, which subsumes previous acts; such as
the alkali act (1906), and the clean air act (1956/68). The act covers air pollution, noise,
and other matters causing a statutory nuisance.
 The Water Resources Act, 1991, which covers discharges into inland water ways.
Consent from the National Rivers Authority (NRA) is needed for such discharges. 3. The
Water Industries Act, 1991, and the Trade Effluent Regulations, 1989, which cover
discharges into the sewers.
 The Town and Country Planning Act, 1990, which covers planning consents.
 Some aspects of the Control of Substances Hazardous to Health Act (COSHH)
regulations and the Health and Safety at Work Act, will also apply to waste handling,
treatment and disposal.
Legislation and control procedures in the United Kingdom are increasingly being derived
from regulations promulgated by the European Commission (E.C). All the legislation embodies
78
the concept of Best Practicable Means (BPM). This requires the designer to use the most
appropriate treatment to comply with the regulation, whilst taking into account: local conditions,
current technology and cost. The concept of BPM also applies to the installation, maintenance
and operation of the plant.
Environmental auditing
An environmental audit is a systematic examination of how a business operation affects the

environment. It will include all emissions to air, land, and water; and cover the legal constraints,
the effect on community, the landscape, and the ecology. Products will be considered, as well as
processes.
When applied at the design stage of a new development it is more correctly called an
Environmental impact assessment.
The aim of the audit or assessment is to:
 Identify environmental problems associated with manufacturing process and the use of
the products, before they become liabilities.
 To develop standards for good working practices.
 To provide a basis for company policy.
 To ensure compliance with environmental legislation.
 To satisfy requirements of insurers.
 To be seen to be concerned with environmental questions: important for public
 relations.
 To minimize the production of waste: an economic factor.
79
CHAPTER
11
SAFTEY
CONSIDERATIONS
80
SAFETY
Safety is defined as Positive activity Towards Minimizing loses
The International Safety Rating System (ISRS) was established in 1864 with the
collaboration of DENTNORSKE VERITAS. It is the most comprehensive safety Management
Evaluation system and its primary objective is to measure the organization levels of the loss
activity against a set of internationally accepted criteria.
Special Safety Equipments:

The following safety equipments are provided in the refinery, these equipments are to be
used depending upon the hazards involved.
Breathing apparatus sets
Proximity suit
Fire Entry Suit
Low temperature Suit
Water jet Blanket(-790c)
Description of Safety Management:
1. Breathing apparatus Sets:
This emergency equipment is designed to be used in toxic or unbeatable

contaminated atmosphere. This set consists of:
 Black plate fixture with pressure gauge and demanded regular

 Cylinder
 Face mask
 Cylinder is filled with the filtered atmospheric air at 200kg/cm 2g.This 200kg/cm2g
pressure is reduced to breathable air pressure by two stages of pressure reduction
provision given the set. Working during of this set is 20min and safety margins 10min.
This safety margin can be acknowledged by warning whistle given in the pressure gauge line.
Once this warning whistle starts blowing user has to come out of the contaminated place within
10min.In LPG plant this set is to be used along with fire entry suit, fire proximity and low
temperature suit.
2. Proximity suit:
The fire proximity suit is designed to give protection to the personnel for the
carrying out emergency operations in close proximity of fire radiant temperature up to 28 0c.This
suit is made with aluminized fabric at outer surface and insulation layers at inner surface to give
maximum radiant heat protection. This suit consists of coat, pants, hoods, hand gloves and boots.
It should be always used along with the breathing apparatus set.
3. Fire Entry suit:
81
The fire entry suit is designed rescue and emergency operations in the case of fire
emergency. This suit is made with aluminized fabric at outer surface and more insulation layers
at inner surface and more insulation layers at inner surface to give maximum heat protection and
radiant heat protection. This suit consists of coat, pants, hoods, hand gloves and boots. It should
be always used along with the breathing apparatus set.
4. Low Temperature suit:

The low Temperature suit is designed for handling minor LPG propylene leaks.
This is one-piece cover all made of butyl rubber designed to protect the personnel against the
temperature as low as 790c.it should always be used with breathing apparatus set.
5. Water Jet Blanket:

The water jet blanket is designed for temporary protection from fire, heat or
suitable for emergency care on heat burns and scalds.
WARNING: Electricity must be shut off before application of water based jet blanket.
Instrumentation:
Inculcated all the IS and OSID recommendations. The P & id attached such that
instrument actions incorporated as pressure level indication valve open or close indication pump
running indication firewater on/off.
GENERAL INFORMATION DEFINITIONS:
 Accidents: An event, which could or does result in unintended harm or damage.
 Major Accidents: An injury within the refinery area causing disablement for a period
more than 48hrs.From the shift in which the injured worked on the day of injury or any
dangerous occurrence.
 Hi-Po Accidents: An event, which have high potential (HI-PO) to cause major accident.
 Fatality: Any event causing a loss of life.
 Injury: A bodily harm to any person, where first-aid treatment is required.
 Incident: An event which slightly different circumstances may have resulted in harm to
personnel, damage to property or loss of production.
 Property Damage: Any loss property damage more than rupees one lakh.
 Industrial illness: Any illness resulting from exposure to the working environment.
 Dangerous occurrence:
 Dangerous occurrence as per the factories act:
82
 Bursting of plant used containing or supplying team under pressure greater than
atmospheric pressure.
 Collapse or failure of a crane, derrick which hoist or the other appliances used in raising
or lowering persons of goods any part or thereof, or the overturning of a crane.
 Expolosion, fire, bursting out, leakage or Escape of any molten metal or hot liquor or gas
causing bodily injury to any person or damage to any room or place in which persons are
employed or fire in rooms of cotton pressing factories, where a cotton opener is in use.
 4.Explosion of a receiver or container used for the storage at pressure of any gas or
gases(including air) or any liquid or solid resulting from the compression of gas.
 Collapse or subsidence of any floor, gallery, roof, bride, tunnel, chimney, wall, building,
or any other substance.
HYDROGEN:
The safe handling of hydrogen

Like any fuel, the safe handling of hydrogen requires that the three
necessary conditions for combustion be prevented. The wide flammability ranges of hydrogen
imply that a mixture of hydrogen and air might ignite more easily than other fuels. Consequently,
the following precautions must be adhered to:
 Hydrogen should not be mixed with air.
 Contact of hydrogen with potential ignition sources should be prevented.
 Purging of hydrogen systems should be performed with an inert gas such as nitrogen.
 Venting of hydrogen should be done according to standards and regulation.
 Because the hydrogen flame is invisible, special flame detectors are required.
Although hydrogen has a wide "detonatability" range, it is difficult to detonate a

hydrogen vapor cloud in an open area without turbulent conditions. However, hydrogen should
be handled with special care in confined, unvented areas. Various safety assessments are
available to serve as a guide in setting up and designing hydrogen systems.
Achieving Safe Hydrogen Systems
It is in the very nature of a fuel to have some degree of danger associated with it. The hazards
they represent are neither good, nor bad; they just exist and must be handled.
Hydrogen is not significantly more or less hazardous than other fuels. By knowing
something about its use in the past, learning some of its basic properties and behaviour, and
making comparisons with other fuels, a public made up of knowledgeable individuals can assess
hydrogen's applications and participate in the public acceptance process. Hydrogen has over the
years acquired an image of an immensely powerful and possibly threatening substance. There are
still some, for example, who can recall the experience of the Hindenburg in 1937, as well as the
cold war and the threat of the hydrogen bomb (H-Bomb). The nuclear fusion reactions involved
in the H-bomb have, of course, nothing to do with the chemical reactions involved in the use of
hydrogen as a fuel for internal combustion engines and hydrogen fuel cells.
83
MATERIAL SAFTEY DATA SHEET
FOR N-BUTANOL :
Section 1: Chemical Product and Company Identification :
Product Name: 1-Butanol

Catalog Codes: SLB3157, SLB1489
CAS#: 71-36-3
RTECS: EO1400000
TSCA: TSCA 8(b) inventory: 1-Butanol
CI#: Not applicable.
Synonym: Propylcarbinol
Chemical Name: N-Butyl alcohol
Chemical Formula: CH3(CH2)2CH2OH
Contact Information:
Sciencelab.com, Inc.
14025 Smith Rd.
Houston, Texas 77396
US Sales: 1-800-901-7247
International Sales: 1-281-441-4400
Order Online: ScienceLab.com
CHEMTREC (24HR Emergency Telephone), call:1-800-424-9300
International CHEMTREC, call: 1-703-527-3887
For non-emergency assistance, call: 1-281-441-4400
Section 2: Composition and Information on Ingredients :
Composition:
Name CAS # % by Weight

{1-}Butanol 71-36-3 100
Toxicological Data on Ingredients: 1-Butanol: ORAL (LD50): Acute: 790 mg/kg [Rat.].
DERMAL (LD50): Acute: 3400 mg/kg
[Rabbit.].
Section 3: Hazards Identification :
Potential Acute Health Effects:

Very hazardous in case of skin contact (irritant, permeator), of eye contact (irritant), of ingestion,
of inhalation. Slightly hazardous in case of skin contact (sensitizer). Inflammation of the eye is
characterized by redness, watering, and itching. Skin inflammation is characterized by itching,
scaling, reddening, or, occasionally, blistering.
Potential Chronic Health Effects:

CARCINOGENIC E
84
FFECTS: Not available. MUTAGENIC EFFECTS: Not available.

TERATOGENIC EFFECTS: Not available.
DEVELOPMENTAL TOXICITY: Not available. Repeated or prolonged exposure is not known
to aggravate medical condition.
Section 4: First Aid Measures :
Eye Contact:
Check for and remove any contact lenses. Immediately flush eyes with running water for
at least 15 minutes, keeping eye lids open. Cold water may be used. Get medical attention
immediately.
Skin Contact:
In case of contact, immediately flush skin with plenty of water for at least 15 minutes
while removing contaminated clothing and shoes. Cover the irritated skin with an emollient.
Cold water may be used.Wash clothing before reuse. Thoroughly clean shoes before reuse. Get
medical attention immediately.
Serious Skin Contact:
Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial
cream. Seek immediate medical attention.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult,
give oxygen. Get medical attention if symptoms appear.
Serious Inhalation:
Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a
collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not
breathing, perform mouth-to-mouth resuscitation. Seek medical attention.
Ingestion:
Do NOT induce vomiting unless directed to do so by medical personnel. Never give

anything by mouth to an unconscious person. If large quantities of this material are swallowed,
call a physician immediately. Loosen tight clothing such as a collar, tie, belt or waistband.
Serious Ingestion: Not available.
Section 5: Fire and Explosion Data :

Flammability of the Product: Flammable.
Auto-Ignition Temperature: 343°C (649.4°F)
Flash Points: CLOSED CUP: 28.9°C (84°F). OPEN CUP: 36.1°C (97°F) (Cleveland).
Flammable Limits: LOWER: 1.4% UPPER: 11.2%
Products of Combustion: These products are carbon oxides (CO, CO2).
85
Fire Hazards in Presence of Various Substances:

Highly flammable in presence of open flames and sparks. Flammable in presence of heat, of
oxidizing materials, of reducing materials, of combustible materials.
Explosion Hazards in Presence of Various Substances:
Risks of explosion of the product in presence of mechanical impact: Not available. Risks of
explosion of the product in presence of static discharge: Not available.
Fire Fighting Media and Instructions:
Flammable liquid, soluble or dispersed in water
SMALL FIRE: Use DRY chemical powder.
LARGE FIRE: Use alcohol foam,water spray or fog. Cool containing vessels with water jet in
order to prevent pressure build-up, autoignition or explosion.
Special Remarks on Fire Hazards: May form explosive mixtures with air. CAUTION: MAY
BURN WITH NEAR INVISIBLE
FLAME
Special Remarks on Explosion Hazards: Not available.
Section 6: Accidental Release Measures :

Small Spill:
Dilute with water and mop up, or absorb with an inert dry material and place in an appropriate
waste disposal container.
Large Spill:
Flammable liquid. Keep away from heat. Keep away from sources of ignition. Stop leak
if without risk. Absorb with DRY earth, sand or other non-combustible material. Do not touch
spilled material. Prevent entry into sewers, basements or confined areas; dike if needed. Be
careful that the product is not present at a concentration level above TLV. Check TLV on the
MSDS and with local authorities.
Section 7: Handling and Storage :

Precautions:
Keep away from heat. Keep away from sources of ignition. Ground all equipment
containing material. Do not ingest. Do not breathe gas/fumes/ vapor/spray. In case of insufficient
ventilation, wear suitable respiratory equipment. If ingested, seek medical advice immediately
and show the container or the label. Avoid contact with skin and eyes. Keep away from
incompatibles such as oxidizing agents, reducing agents.
Storage:
Store in a segregated and approved area. Keep container in a cool, well-ventilated area.
Keep container tightly closed and sealed until ready for use. Avoid all possible sources of
ignition (spark or flame).
Section 8: Exposure Controls/Personal Protection :

Engineering Controls:
Provide exhaust ventilation or other engineering controls to keep the airborne
concentrations of vapors below their respective threshold limit value. Ensure that eyewash
stations and safety showers are proximal to the work-station location.
Personal Protection:
86
Splash goggles. Lab coat. Vapor respirator. Be sure to use an approved/certified

respirator or equivalent. Gloves.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing
apparatus should be used to avoid inhalation of the product. Suggested protective clothing might
not be sufficient; consult a specialist BEFORE handling this product.
Exposure Limits:
CEIL: 152 (mg/m3) Consult local authorities for acceptable exposure limits.
Section 9: Toxicological Information :
Routes of Entry: Dermal contact. Eye contact. Inhalation. Ingestion.
Toxicity to Animals:
WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A
4-HOUR EXPOSURE. Acute oral toxicity (LD50): 790 mg/kg [Rat.]. Acute dermal toxicity
(LD50): 3400 mg/kg [Rabbit.]. Acute toxicity of the vapor (LC50): 8000 4 hours [Rat.].
Chronic Effects on Humans: Not available.
Other Toxic Effects on Humans:
Very hazardous in case of skin contact (irritant, permeator), of ingestion, of inhalation. Slightly
hazardous in case of skin
contact (sensitizer).
Special Remarks on Toxicity to Animals: Not available.
Special Remarks on Chronic Effects on Humans: Can cause gastrointestinal disturbances.
Special Remarks on other Toxic Effects on Humans: Exposure can cause nausea, headache
and vomiting.
Section 10: Ecological Information :

Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term
degradation products may arise.
Toxicity of the Products of Biodegradation: The products of degradation are more toxic.
Special Remarks on the Products of Biodegradation: Not available
Section 11: Transport Information :

DOT Classification: CLASS 3: Flammable liquid.
Identification: : Butanol UNNA: UN1120 PG: III
Special Provisions for Transport: Not available.
Section 12: Other Regulatory Information :

Federal and State Regulations:
Pennsylvania RTK: 1-Butanol Massachusetts RTK: 1-Butanol TSCA 8(b) inventory: 1-Butanol
Other Regulations: OSHA: Hazardous by definition of Hazard Communication Standard (29
CFR 1910.1200).
Other Classifications:
WHMIS (Canada):
87
CLASS B-2: Flammable liquid with a flash point lower than 37.8°C (100°F). CLASS D-2B:
Material causing other toxic effects (TOXIC).
DSCL (EEC):
R10- Flammable. R22- Harmful if swallowed. R38- Irritating to skin. R41- Risk of serious
damage to eyes.
HMIS (U.S.A.):
Health Hazard: 1
Fire Hazard: 3
Reactivity: 0
Personal Protection: h
National Fire Protection Association (U.S.A.):
Health: 1
Flammability: 3
Reactivity: 0
Specific hazard:
Protective Equipment:
Gloves. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent.
Wear appropriate respirator when ventilation is inadequate. Splash goggles.
Section 13: Other Information :

References: -Manufacturer's Material Safety Data Sheet.
Other Special Considerations: Not available.
Created: 10/10/2005 08:15 PM
Last Updated: 11/01/2010 12:00 PM
MATERIAL SAFETY DATA SHEET
FOR ISO-BUTANOL
Version 1.04 Revision Date 20.11.2006
1. Identification of the substance/preparation and of the company/undertaking
Trade name Iso-Butanol
Synonyms Iso-Butanol, 2-Methyl-propan-1-ol, 2-Methylpropyl alcohol, 1
Hydroxymethylpropane, Isopropyl Carbinol, i-Butyl alcohol
Use Solvents, industrial use, raw material for washing and cleaning agents, raw material for
fragrances, Paint related material Company Hitech Chemicals
2. Composition/information on ingredients
2-methylpropan-1-ol; iso-butanol
content: 99.50 %W/W
CAS-No. 78-83-1 Index-No. 603-108-00-1 EG-Nr.: 201-148-0
Symbol(s) Xi R-phrase(s) -R10 -R37/38 -R41 -R67
For the full text of the R phrases mentioned in this Section, see Section 16.
Print Date 20.12.2006 100000000534 1/6
88
3. Hazards identification
Identification of the risks
R10 Flammable.
R37/38 Irritating to respiratory system and skin.
R41 Risk of serious damage to eyes.
R67 Vapours may cause drowsiness and dizziness.
4. First aid measures

General advice If you feel unwell, seek medical advice (show the label where
possible).Inhalation Move to fresh air in case of accidental inhalation of vapours. If
breathing is irregular or stopped, administer artificial respiration. Call a physician immediately.
Skin contact Wash off immediately with plenty of water for at least 15 minutes. Call a physician
immediately. Eye contact Rinse immediately with plenty of water, also under the eyelids, for at
least 15 minutes. Remove contact lenses. Call a physician immediately. Ingestion If swallowed,
seek medical advice immediately and show this container or label. Do not induce vomiting
without medicaladvice. Never give anything by mouth to an unconscious person.
5. Fire-fighting measures
Suitable extinguishing media.Specific hazards during fire fighting,Special protective
equipment for firefighters Water spray, Dry chemical, Alcohol-resistant foam Flash back
possible over considerable distance. Do not allow run-off from fire fighting to enter drains or
water courses.Wear self-contained breathing apparatus and protective suit. Further information
Standard procedure for chemical fires. In the event of fire, cool tanks with water spray.
6. Accidental release measures

Personal precautions Use personal protective equipment. Do not breathe vapours or
spray mist. Ensure adequate ventilation. Keep away fromsources of ignition - No smoking.
Environmental precautions. Avoid subsoil penetration. Do not flush into surface water or
sanitary sewer system. Methods for cleaning up Soak up with inert absorbent material (e.g. sand,
silica gel, acid binder, universal binder, sawdust). The material taken up must be disposed of in
accordance with regulations.
7. Handling and storage

Handling
Safe handling advice Wear personal protective equipment. Avoid contact with skin
and eyes. Keep away from sources of ignition - No smoking. Advice on protection against fire
and explosion .Use explosion-proof equipment. Provide sufficient air exchange and/or exhaust in
work rooms. Keep away from open flames,hot surfaces and sources of ignition.
Storage
Requirements for storage areas and containers:
Keep containers tightly closed in a cool, well-ventilated place.
Keep away from sources of ignition - No smoking.
8. Exposure controls / personal protection

Components with workplace control parameters
NATIONAL OCCUPATIONAL EXPOSURE LIMITS:no data available
89
EUROPEAN OCCUPATIONAL EXPOSURE LIMITS:no data available

Engineering measures Provide sufficient air exchange and/or exhaust in work rooms.
Personal protective equipment:Respiratory protection suitable respiratory equipment:
Hand protection gloves suitable for permanent contact:
Material: butyl-rubber
Break through time: 4 h
Material thickness: 0.5 mm
unsuitable gloves
Material: leather, nitrile rubber/nitrile latex, Polyvinylchloride, natural rubber/natural latex
Eye protection :Safety glasses with side-shields Skin and body protection protective suit, Safety
shoes
Hygiene measures :Wash hands before breaks and immediately after handling the
product.
Protective measures : Wear suitable protective equipment.
9. Toxicological information
Acute oral toxicity LD50 rat: 2,460 mg/kg; literature value
LD50 rabbit: 74.1 mg/kg; literature value
Acute inhalation toxicity LC50 rabbit: 2,630 mg/m3; ; 4 h; literature value
LCLo rat: 8,000 mg/m3; ; 4 h; literature value
LC50 rat: 19,200 mg/m3; ; 4 h; literature value
Acute dermal toxicity LD50 rabbit: 3,400 mg/kg; literature value
Assessment of mutagenicity.
Experiments showed mutagenic effects in cultured bacterial Cells.
10. Ecological information

Ecotoxicity effects
Toxicity to fish Pimephales promelas: 1,430 g/l; 96 h; literature value
12. Disposal considerations

Product In accordance with local and national regulations. Contaminated packaging
Packaging that cannot be cleaned must be disposed of in the same way as the material itself.
13 Transport information
ADR UN-No.: 1212; Class: 3; Packaging group: III; F1; Description of
the goods: ISOBUTANOL
RID UN-No.: 1212; Class: 3; Packaging group: III; F1; Description of
ADNR UN-No.: 1212; Class: 3; Packaging group: III; F1; Description of
IMDG UN-No.: 1212; Class: 3; EmS: F-E, S-D; Packaging group: III;
Description of the goods: ISOBUTANOL
ICAO/IATA UN-No. : 1212; Class: 3; Packaging group: III; Description of the
goods: Isobutanol
90
14. Regulatory information

Labelling
Regulatory base 67/548/EEC
Symbol(s) Xi: Irritant
R-phrase(s) R10: Flammable.
R37/38: Irritating to respiratory system and skin.
R41: Risk of serious damage to eyes.
R67: Vapours may cause drowsiness and dizziness.
S-phrase(s) S 2: Keep out of the reach of children.
S 7/9: Keep container tightly closed and in a well-ventilated
place.
S13: Keep away from food, drink and animal feedingstuffs.
S26: In case of contact with eyes, rinse immediately with plenty
of water and seek medical advice.
S37/39: Wear suitable gloves and eye/face protection.
S46: If swallowed, seek medical advice immediately and show
this container or label.
Hazardous components which must be listed on the label 2-methylpropan-1-ol; iso-butanol
15. Other information:Full text of R-phrases referred to under sections 2 and 3

R10 Flammable.
R37/38 Irritating to respiratory system and skin.
R41 Risk of serious damage to eyes.
R67 Vapours may cause drowsiness and dizziness.
This MSDS summarises at the date of issue our best knowledge of the health, safety and
environmental hazard information related to the product, and in particular how to safely handle,
use, store and transport the product in the workplace. Since we cannot anticipate or control
conditions under which the product may be handled, used, stored or transported, each user must,
prior to usage, review this MSDS in the context of how the user intends to handle, use, store or
transport the product in the workplace and beyond, and communicate such information to all
relevant parties.If clarification or further information is needed to ensure that an appropriate
assessment can be made, the user should contact this company.We shall not assume any liability
for the accuracy or completeness of the information contained herein or any advice given unless
there has been gross negligence on our part. In such event our liability shall be limited only to
direct damages suffered. Our responsibility for product as sold is subject to our standard terms
and conditions, a copy of which is sent to our customers and is also available upon request. All
risk associated with the possession and application of the product passes on delivery.
Print Date 20.12.2006 100000000534 6/6
91
CONCLUSIONS
 Liturature survey has been done.

 Process selection from various available processes has been done based on various
considerations like catalyst selectivity, raw materials,process conditios etc.,
 The properties of n-butanol and iso-butanol are specified.
 Detailed description has been given for the total PFD.
 Detailed mass and energy balances have done for total PFD.
 Detailed process equipment design has done for distillation column.
 Detailed mechanical equipment design has done for distillation column.
 Detailed cost estimation has been done for the for the whole process and the plant.
SCOPE OF FUTURE IMPLEMENTS:
 Heat integration for the whole process .
92
REFERENCES
 n-Butanol Product Information, The Dow Chemical Company, Form No. 327-
00014-1001, page 1.^ Evans D., Osborn J. A., Wilkinson G. (1968).
"Hydroformylation of Alkenes by Use of Rhodium Complex Catalyst". Journal of
the Chemical Society 33 (21): 3133–3142. doi:10.1039/J19680003133.
http://www.rsc.org/ejarchive/J1/1968/J19680003133.pdf
• Journal of molecular catalysis.9(1960)265 -274 "Hydroformylation of Alkenes by
Use of Rhodium Complex Catalyst". L A. GlCRRETSEN, W. KLUT, 56. H. VR!
XJGDENiiIL and J. d. F. SCEfOLTEN*
• De~enCofChemi~Technolo~.DelfC UniuersibofTeehno~~.Jut~naLcan 136.
 Dryden’s outlines of chemical otechnology by Gopal rao
 Shreve,s chemical process industries
 Introduction to chemical engineering thermodynamics, smith J.M,, Van Ness,H.C.,
and Abbott,M.M., 6th edition,McGraw Hill
 Perry’s chemical engineers handbook , Perry Rober H,7 th edition,McGraw Hill
 http://www.cbu.edu/ ̴rprice/lectures/distill7.html, Trays probably aren’t a good idea
for columns less than about 1.5 ft in diameter (you can’t work on them) –
these are normally packed
 www.neiwpcc.org/tanksconference/presentations/monday
%20presentations/Adair.Biofuels.monday.pdf
BIBLIOGRAPHY
 http://www.wikipedia.com
 http://www.google .co.in
 http://www.adm.com
 http://www.sciencedirect.com
 “Perry’s1 chemical engineers handbook” by ,Robert H,Perry,Don W.Green
 “Chemical process principles”,part2 by Hougen , K.M.Watson , R.A.Ragatz
 Chemical Engineering Thermodynamics by smith &Vannes,Abbot
 Heat transfer process by Kern
 Coulson and Richard’s chemical engineering by R.K Sinnot 6th volme,chemical

engineering design
93
 Process economics and industrial management by S.M.Jhomby.
 Process of gases and liquids,5th edition,Bruce E.Poling, John M Praunsnitz, John

P.O’Connel
 Chemical Safety Data, Edition II. -Supplier MSDS
94

Co-Production of N-Butanol and Isobutanol

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Co-Production of N-Butanol and Isobutanol

Uploaded by

Copyright:

Available Formats

COPRODUCTION OF N-BUTANOL AND ISO-BUTANOL 2012

This design problem refers to coproduction of N-butanol and I-butanol by

N-butanol, iso-butanol, and tert-butanol have multiple uses in industrial and

Butanol is an aliphatic saturated C4 alcohol. It is termed normal butyl alcohol, n-

n-Butanol occurs in nature in compound form. It also occurs sometimes in high

COMMON USES OF BUTANOL:

N-butanol finds applications as:

Production intermediate for:

Degreasers and cleaning solutions

Iso-butanol finds application as:

Butanol also resists water absorption, allowing it to be transported in pipes and

Quantifying advantages of butanol:

In 1914 Weizmann established a fermentation process in USA using 'Clostridium

By 1930's synthetic production began and fermentation process using molasses

The next improvement came with the range of catalyst to phosphine-modified

PROCESS OF MANUFACTURE AND RAW MATERIALS

Propylene is a co-product of ethylene from a naphtha cracking unit or

STRUCTURE AND STATUS OF INDIAN INDUSTRY

DEMAND / EXPORT / IMPORT

 Oxo-synthesis or propylene hydroformylation

The most important and widely commercialised technology is the oxo-synthesis.

The technologies for Somaiya Organics plant is from Melle-Beznos, France.

TECHNOLOGY SUPPLIERS AND ENGINEERING CONSULTANTS

Internationally there are several technology suppliers. Some of the technology

USA is the largest producer of butanol as well as isobutanol followed by

R&D EFFORTS, TECHNOLOGY ABSORPTION AND GAPS

In the area of oxo synthesis (hydroformylation), NCL, Pune has considerable

The processes of manufacture of butanol are propylene hydro-formulation (oxo

1.Oxo-synthesis (propylene hydroformylation):

 Most of the aldehydes produced are either reduced to alcohol directly

2. Hydrogenation starting from acetaldehyde or ethanol:

 The aldol process uses acetaldehyde as the precursor. Acetaldehyde is

 Acetaldehyde is aldolized followed by hydrogenation in the presence of

 Fermentation process uses molasses or starch grains to produce

 The butanol production by 'Clostridia' was made by Pasteur and acetone

 In Reppe process, propylene, carbon monoxide and water are made to

 The difference between this process and classic hydroformylation is

 Oxo process is the process commercialized successful due to high yields.

Petrochemical production of solvents became much easier and cheaper

Physical state and appearance: Liquid. (Z)

Stability and Reactivity Data :

Stability: The product is stable.

Stability and reactivity :

Materials to avoid Oxidizing agents, Reducing agents, Acids and bases

OXO PROCESS OR PROPYLENE HYDROFORMYLATION

Catalyst: triphenylphosphine rhodium hydro carbonyl

Reaction proceeds as:

Propylene Syn gas Butyraldehyde(N ,iso)

COBALT BASED RHODIUM BASED

TEMPARATURE(˚C) 145-180 60-100

Kinetics of the heterogeneous hydroformylation of propylene:

Using hydrocarbonyltri(triphenylphosphine)rhodium(I), dissolved in

PA = 8.75 * 10(-5) bar

XA = 1 – (pA /pA0) = 0.998 Conversion = 99.8%

C3 H6 + H2 +CO  C4 H8O (N – Bal and I – Bal)

Undesired side Reaction

FLOWSHEET FOR BUTANOL PRODUCTION:

Butanol campaign overview.

i) Vapor phase hydrogenation.

N-Butanol specification: (wt%):

I – Butanol specification: (wt%):

Vapor phase hydrogenation:

MATERIAL AND ENERGY BALANCES

118.7* 0.915 = D0.1+ 107.460.99

116.0490.784 = W0.995 + (116.049-W)*0.001