SYNTHESIS AND DISTILLATION

OF
METHYL ETHYL KETONE

 ANTONY JOSEPH ALDAMAN.R INTERNAL GUIDE

 AKHIL.S Ms M.S VIJAYALAKSHMI,M.TECH.,
 SONNIYA.M DEPT OF PETROLEUM ENGINEERING
 MOHAMMED ASIF
UNDER THE GUIDANCE OF
Mr.T.SUNDARAMOORTHY,
GENERAL MANAGER,CETEX PVT.
 ABSTRACT

o SBA (secondary butyl alcohol) is produced by etherification of butane with

sulphuric acid followed by hydrolysis of n-butane. MEK(methyl ethyl ketone)
is obtained by the dehydrogenation of SBA in the presence of copper
catalyst at 400°c to 500°c
COMPANY PROFILE

 Cetex petrochemicals Ltd was established in 1990 with German Technology.

 Cetex petrochemicals is the largest manufacture of Methyl Ethyl Ketone (MEK)
and Secondary Butyl Alchohol (SBA) in India.
 Cetex is a zero effluent discharge company and has been certified to be an
environment conscious company
METHYL ETHYL KETONE(MEK)

 The chemical formula for MEK is C4H8O. And its structure is CH3-CH2-
CO-CH3.
 MEK is one of the most important solvents in many areas such as paints ,
chemical and other industries . In recent years its importance has
continuously increased
 MEK is a volayile , water-white liquid with a characteristic odour and is
partly miscible with water
 MEK is used as a precipitant at the dewaxing of lubricating oils in
refineries
 It is also widely used in rubber industries
STRUCTURE OF MEK
 MEK PROCESS:

Dehydrogenation process consumes SBA in presence of special

copper catalyst. Hydrogen is generated as by product. The dehydrogenation
reaction is endothermic reaction, requiring 13 kcal per mole of SBA reacted. To
obtain satisfactory reaction rate, the temperature should be about 250 - 270 °C at
nearly atm pressure, so that SBA/MEK are in the vapour phase. At these condition
a conversion of 80% per pass is achieved. The unreacted SBA is separated and
recycled back to the feed.
MEK SYNTHESIS

 Feed SBA is continuously received from the storage tanks

transferred with feed pump
 The flow is controlled by the level of the flash drum
 The SBA is vapourized under constant pressure
 The vaporized SBA flows due to process pressure through
exchanger where it is further heated
 The SBA enters the reactor, which are normally operating in
parallel, at the top The reactor is of the tubular type, the tubes
filled with catalyst.
 On the shell side the reactor are heated with circulating hot oil,
since the reaction, is endothermic.
 The reactor eluent produced, leaving the bottom of the reactor
consists of MEK, some heavy ketone, unreacted SBA, some
butenes
 Both effluent stream are combined and then first cooled by
heat-exchanging with SBA feed, where the most of the MEK
and SBA are condensed
 The mixture flows to the MEK accumulator where the gas and
liquid phase are separated. The raw MEK liquid is pumped to
the distillation section
 The gas, consisting mainly of hydrogen, is saturated with MEK.
Its contacted with a cooled SBA recycled stream from the
distillation column bottom to remove most of the MEK
 The gas is further cooled by cooler using evaporating butane
coming from the Recycle system of the SBA unit to about 5 °C
in order to condense nearly all solvent
 The soivent free hydrogen gas which also contains some butenes
is passed to the heat fuel system
REACTION ROUTES:

MAIN REACTION:
CU
CH3-CH2-CHOH-CH3 → CH3 CH2 COCH3 + H2
230°C-250°C
BY PRODUCT FORMATION:

Besides the main product MEK several by products are also formed
from the SBA feed in different quantities. The important by products
are,

-HYDROGEN
-BUTENE
-HEAVY KETONES
HYDROGEN
This is generated at the dehydrogenation reaction,its separted
from the solvents by chilling to low temperature.

CH3 CH2-CHOH-CH3 → CH3 –CH2CO-CH3 + H2

HEAVY KETONEs
They result from dehydrogenation and condensation reaction
of more than 1 SBA molecule which,hence forming hydrogen and water

BUTENES
Butenes are formed by dehydration of SBA molecule

CH3 CH2 CH(OH)CH3 → CH3 CH=CHCH3 + H2O

REGENERATION OF CATALYST

 After above 1000 operating hours, the catalyst is becoming

inactive due to coke deposits. It has to be regenerated.
 An indication is a significant drop of the conversion rate (<75%).
 The regeneration is done by blowing off the deposits with air and
subsequent reducing of the catalyst with hydrogen.
MEK MANUFACTURING PROCESS
MEK DISTILLATION

 After condensing in accumulator the liquid phases is separated. The raw

MEK obtained in the accumulator contains also unconverted SBA.
 Its pumped to the packed column. In packed column, the water
contained in the raw MEK as well as light en.ds (butenes) will be
removed.
 The heat required for distillation is supplied by the re-boiler, heated
withsteam. The heat input is controlled by the steam flow rate.
 In packed column, the water is separated by azeotropic distillation
using hexane in closed cycle as entrainer.
 Water, hexane and some MEK will vaporize. The upper layer which is
hexane and MEK is returned as reflux to the packed column.
 The lower water layer is obtained discontinuously to sewer
 The dry MEK pumped from packed column bottoms, enters the MEK column in
the middle
 The overhead MEK vapors are condensed and the liquidin the condenser, one
part is refluxed back to the top of MEK column, where as the net MEK product
is pumped under level control to tank storage
 The heat required for the distillation in MEK column is supplied by the
reboiler at the bottom of the MEK column.
 SBA is left with some heavy ketones. This stream is pumped to another SBA
column in the plant
 SBA is recovered in this column along with the butanol
 Heavy ketones remaining in the bottom of MEK column are passed to heavies
column where they are stripped together with heavy compounds from SBA
synthesis.
 One part of MEK column bottom product is circulated, flow controlled by
bottom pump through heat exchanger to MEK condenser for the purpose of
recovery of MEK product from hydrogen gas which leaves the accumulator.
DESIGN OF EQUIPMENTS

DISTILLATION:
-Distillation is a method of separating mixtures based on
differences In their volatiles in a boiling liquid mixture
-Distillation is a unit operation, or a physical separation process,
and not a chemical reaction.

TYPES OF DISTILLATION
-Simple distillation
-Fractional distillation
-Vacuum distillation
-Azeotropic distillation
-Steam distillation
DISTILLATION COLUMN
DESIGN OF HEAT EXCHANGER
 COST ESTIMATION

 Acceptable plant design must present a process that is capable of rating

under conditions, which will yield profit.
 Since net profit equals total value minus all expenses, it is essential that
the chemical engineer be aware of the many different types of cost
involved in the manufacturing processes.
 There are many factors affecting investment and production cost. These are

-Source of equipment
-price fluctuation
-Company policies
-Operating and rate of production
-Government policies
COST OF PURCHASED EQUIPMENT
 Methyl ethyl ketone plant capacity = 1250 kg/hr = 30000 kg/day
S.NO NAME OF COST OF NO. OF
THE THE THE RUPEES
EQUIOMENT EQUIPMENT EQUIPMENT

1 Pump 52000 6 31200

2 Heat exchanger 450000 2 900000

3 Condenser 120000 5 600000

4 Accumulator 700000 2 1400000

5 Regenerator 2600000 1 2600000

6 Reactor 7562200 2 15124400

7 Cooler 140000 3 4200000

8 Packed 750000 1 7500000

Column
9 Distillation 820000 1 8200000
Column
10 Flash 230000 1 2300000
Drum
11 Storage 820000 4 3280000
Tank
12 Steam 1250000 2 2500000
generator
Total process equipment cost = 71416400
TYPE OF RANGE % ASSUMED % COST IN
COST RUPEES

Purchased - - 71416400
equipment cost
Installation cost 35-45% of PEC 40% 28566560

Instrument |06-30% of PEC 20% 14283280

&control
installed
Piping 10-80% of PEC 60% 42849840
installation cost
Electrical 10-40% of PEC 25% 17854100
installation cost
Building process 10-70% of PEC 50% 35708200
& auxiliary
Services facilities 30-80% of PEC 70% 49991480
cost
Yard 10-15% of PEC 15% 10712460
improvement cost
Land cost 04-08% of PEC 8% 577095632

TOTAL DIRSCT COST = Rs.277095632

 USES OF MEK
 In lube oil dewaxing
 Printing works
 Magnetic audio and video tapes
 Adhesive
 Polyurethane resins
 Artificial leathers
 Transparent papers
 Degreasing of metal surface
 Natural resins
 Alkyl paints
 In pharmaceutical chemical reactant and solvent
 Industrial perfumes
 PHYSICAL PROPERTIES OF MEK
 Name : methyl ethyl ketone
 Appearance : Colourless
 Formula : CH3 COC2H5
 Specific gravity : 0.8255 - 0.806
 Density : 0.8050 g/ml
 Flash point : -9 °C
 Boiling point at I atm : 79.6 °C
 Auto ignition temperature : 515.6 °C
 Critical pressure : 43 atm
 Critical temperature : 260 °C
 Explosive limits in air, vol% : Upper 10
 Freezing point : -86.3 °C
 Molecular weight : 72.104
 Refractive index no : 1.3791
 Specific heat : 0.549 cal/g ℃
 SELECTION OF PLANT SITE
 The major factors in the selection of most plant sites are 1) rawmaterials, 2) markets,
3) energy supply, 4) climate, 5) transportation facilities, and 6) water supply. For a
preliminary survey, the first four factors should be considered
 The location of the plant can have a crucial effect on the profitability of project, and
the scope for future expansion.

The principle factors to consider are :

 Location with respect to the marketing

 Raw material supply.
 Transport facility
 Availability of labor.
 Availability of utilities: water, fuel, power.
 Availability of suitable land
 Environment impact and effluent disposal
 Local community consideration
 Climate.
 Political and strategic consideration
PLANT LAYOUT
 SAFETY MANAGEMENT

MATERIAL SAFETY DATA SHEET

 Product Name : Methyl Ethyl Ketone

 Synonym : 2-Butanone
 Chemical Name : Methyl Ethyl Ketone
 Chemical Formula : C 4 H8 0
 FIRST AID MEASURES:
Eye contact:
 Check for and remove any contact lenses.
 Immediately flush eyes with running water for atleast 15 minutes keeping eyelids open
 Cold water may be used.
 Get medical attention

Skin contact:
 In case of contact, immediately flush kin with plenty of wate
 Cover the irritated skin with an emollient
 Remove contaminated clothing and shoes
 Cold water may be used
 Wash clothing before reuse.
 Thoroughly clean shoes before reuse.
 Get medical attention.
 CONCLUSION

 With a global demand, Methyl Ethyl Ketone is one of the most important
solvent and its widely used in lube oil dewaxing, resins, perfumes and mainly in
artificial leather manufacturing. Methyl Ethyl Ketone is the most preferred
solvent by the paints and printing ink industry.

 Cost estimation for the plant has been carried out and the payback period was
calculated to be 3.2 years (1050 days).
 The design of heat exchanger and distillation column is studied
Thanking you …..