1

“Production of Maleic Anhydride from n-Butane”

Project Advisor
Ma’m Hina Muryam

Group Members
Sahreen Shamshad 2012-CH-401
Salman Raza 2012-CH-412
Hammad Fazal 2012-CH-418
Muhammad Faheem Hassan 2012-CH-426

2
 Reactor Design
2012-CH-418

Production of Maleic Anhydride from n-Butane 3

Production of Maleic Anhydride from n-Butane 4
Schematic Diagram

Production of Maleic Anhydride from n-Butane

5
 Reactor Selection

Reactors

Homogeneous Heterogeneous

Fluidized
C.S.T.R PLUG FLOW Fixed bed
bed

Production of Maleic Anhydride from n-Butane 6

 Reactor selection
Fluidized bed reactor Fixed bed reactor
• useful when solid particles which are involved in • Has the ability to process large
reactions must be removed frequently.(online
regeneration)
volumes of fluid
• temperature control is easy as the rate of heat transfer • Effective temperature control of
is relatively higher in fluidized beds. larger fixed beds is difficult
• Excellent solid gas contact .
• In exothermic reactions hot spots are
• temperature uniformity
formed which are bad for catalyst
• low residence time which is more feasible for life
exothermic reactions
• Vulnerability to large-scale catalyst releases from • Pressure drop is high
explosion venting
• Offline regeneration
• backmixing
Production of Maleic Anhydride from n-Butane 7
Kunii-Levenspiel
(bubbling bed) model
In this model, the reactant gas enters the
bottom of the bed and flows up the reactor
in the form of bubbles. As the bubbles rise
mass transfer of the reactant gases takes
place as they flow (diffuse) in and out of
the bubble to contact the solid particles
where the reaction product is formed.
The product then flows back into a bubble
and finally exits the bed when the bubble
reaches the top of the bed

Production of Maleic Anhydride from n-Butane 8

Assumptions of Kunii-Levenspiel model
• All particles are of the same size
• Emulsion phase exists at minimum fluidization velocity
• Gas void fraction is equal to void fraction at minimum fluidization velocity
• Concentration of solids present in emulsion phase is equal to that in the wakes
• Order of reaction Is 1
• rate of change of concentration (w.r.t position) in cloud and emulsion phase is very small

Production of Maleic Anhydride from n-Butane 9

 Fluidized Bed Reactor
• The ability to process large volumes of fluid
• Deals with heterogeneous (gas-solids) system
• Useful when solid particles which are involved in reactions must be removed
frequently.
• Temperature control is easy as the rate of heat transfer is relatively higher in
fluidized beds.

Production of Maleic Anhydride from n-Butane 10

 Chemical Reaction
Vanadium
NAME n-Butane phosphorus Nitrogen Oxygen
oxides

FORMULA C4H10 V1P1.2OX N2 O2

C4H10(g) +3.5 O2(g) C 4H2O3(g)

∆H= -244 kJ at 25°C & 1 atm.

• Catalyst is mixed oxides of vanadium and phosphorous

Production of Maleic Anhydride from n-Butane 11
 Reaction Kinetics
• kcat = 8.1048 x 106 exp(-15649/T)
• Oder of reaction : pseudo first order reaction
• Reaction rate = kC A

Production of Maleic Anhydride from n-Butane 12

 Reaction Specification

Process variables (T,P) 121-410.00C , 3 atm

Nature of reaction Exothermic
Type of operation Steady state
Type of process Adiabatic process
Type of column Fluidized bed
Specified conversion 70%
Nature of catalyst Solid particles

Production of Maleic Anhydride from n-Butane 13

 Design Algorithm
Production of Maleic Anhydride from n-Butane 14
 Specify feed rate, conversion, particle dia, T & P

Calculate umf &Ut

Set Umf <U0< ut

Calculate A & D

Calculate dbm & dbo

Guess h and calculate db at h/2 Guess db

Calculate ub

Calculate Kbc and kce

Calculate ϒc,, ϒe and ᵟ

Us>U0
Calculate kb kc & ke
db >D
Calculate KR
Calculate Us
Calculate db at h/2

Us<U0
Calculate W

Production of Maleic Anhydride from n-Butane 15

 Parameters Used
1. Umf =minimum fluidization velocity
2. Ut = terminal velocity
3. Εmf = porosity at minimum fluidization
4. U0 = superficial velocity
5. Ub = bubble velocity
6. Db = dimeter of column
7. Kbc = mass transfer coefficient b/w bubble and cloud phase
8. Kce = mass transfer coefficient b/w emulsion and cloud phase
9. H= height of column
10. W= weight of column
Production of Maleic Anhydride from n-Butane 16
11. Kbc = mass transfer coefficient b/w bubble and cloud phase

12. Kce = mass transfer coefficient b/w emulsion and cloud phase

13. KR= The overall transport

14. coefficient
15. H= height of column
16. W= weight of column

Production of Maleic Anhydride from n-Butane 17

 Assumptions
• All particles are of same size.
• Emulsion phase exists at minimum fluidization velocity.
• Gas void fraction is equal to void fraction at minimum fluidization velocity.
• Concentration of solids present in emulsion phase is equal to that in the wakes.
• Order of reaction is 1.
• Rate of change of concentration (w.r.t position) in cloud and emulsion phase is very small.

Production of Maleic Anhydride from n-Butane 18

 Design Steps
Production of Maleic Anhydride from n-Butane 19
1. Specify Flow rates, conversion particle size & operating conditions
2. Calculate minimum fluidization and terminal velocity
3. Specify superficial velocity
4. Calculate area and diameter
5. Calculate initial & max bubble diameter
6. Guess height and Calculate bubble diameter
7. Calculate bubble velocity
8. Calculate mass transfer coefficients
9. Calculate KR
10. Calculate height
11. Calculate weight of bed

Production of Maleic Anhydride from n-Butane 20

 Calculations
Production of Maleic Anhydride from n-Butane 21
 Superficial Velocity
•   • Umf = (ε3mf/1−εmf)
• εmf = 0.586ψ−0.72 (µ2/ρgηdp3)0.029(ρg/ρc)0.021
• εmf = 0.633
• Umf =0.124 cm/s
• Ut = (1.78×10−2η2/ρgµ)1/3(dp)
• Ut= 826 cm/s
• UT < U0 < Umf

Production of Maleic Anhydride from n-Butane 22

Bubble Velocity and Bubble Diameter
• Ubr= (0.71)gdb1/2
• Ubr=136.7
• Ub=Ubr+(U0−Umf)
Ub= 145.6
•
• db = dbm − (dbm−dbo )e−0.3h/Dt
• db =38.91cm
• dbm =0.652[As (U0−Umf )]0.4
• dbm =91.53 cm
db0=0.00376(U0−Umf )2
db0 = 0.179 cm
Production of Maleic Anhydride from n-Butane 23
 Mass Transfer co-efficients
•   • Kbc=4.5(umf/db)+5.85(DAB1/2g1/4 /db5/4 )
• Kbc=6.91 s-1
• Kce=6.77[εmf DABUb /db3 ]1/2
• Kce=4.92 s-1
• K R=
• KR= 8.64

Production of Maleic Anhydride from n-Butane 25

Height and Weight of Column

• h = (Ub /kcatKR )ln(1/1−X)

• h = 2.73128 m
W = ρcAch(1−εmf )(1−δ)
W = 13.417 ton

Production of Maleic Anhydride from n-Butane 26

Height and Weight of Column
• A=Q/ U0

• 3.357m2

• h=(Ub /kcatKR )ln(1/1−X)

• h=5.95 m
W=ρcAch(1−εmf )(1−δ)
W= 13.417 ton

Production of Maleic Anhydride from n-Butane 27

 SPECIFICATION SHEET
Identification
Item Reactor
Item number R-101
Type Fluidized bed reactor
Function
Conversion Of butane To Maleic anhydride
Design Specification
Operating temperature 410 °C
Operating pressure 275kPa
Design temperature 430 °C
Design pressure 285 kPa
Diameter 1.23 m
Reactor height 2.76 m
weight of catalyst bed 1.58 m
area of reactor 0.589 m2
space time 683 seconds

Production of Maleic Anhydride from n-Butane 28

 Absorber Design
2012-CH-401

Production of Maleic Anhydride from n-Butane 29

Production of Maleic Anhydride from n-Butane 30
 CO2 = 257.890043 kg/hr
45 CO 59OC
CO = 137.208264 kg/hr
H2O = 7872.805 kg/hr
170kPa O2 = 4338.39464 kg/hr
170kPa
N2 = 25302.1776 kg/hr

C4H2O3 = 1647.844 kg/hr

H2O = 1461.441 kg/hr
C3H4O2 = 17.29516 kg/hr
CO2 = 257.89 kg/hr
CO = 137.2083 kg/hr
CH2O2 = 11.04969 kg/hr 60OC C4H4O4 = 1950.51 kg/hr
C4H10 = 247.9934 kg/hr H2O = 9031.581 kg/hr
95OC
O2 = 4338.395 kg/hr 170kPa C3H4O2 = 17.2951 kg/hr
N2 = 25302.18 kg/hr CH2O2 = 11.04969 kg/hr
200kPa
C4H10 = 247.9934 kg/hr
Production of Maleic Anhydride from n-Butane 31
 ABSORPTION
“Gas absorption is the removal of one or more selected components
from a mixture of gases by absorption into a suitable liquid.”

Applications:
Second major operation in chemical engineering that based on mass transfer.
Purpose of gas absorption may be any of the following:
• For separation of component having the economical value
• For removing of undesired component (pollution)

Production of Maleic Anhydride from n-Butane 32

 Types of Absorption

Physical Absorption Chemical Absorption

• Forces operating in these are weak Vander • forces operating in these cases are similar to
Waal’s forces. those of a chemical bond.
• Process is reversible. • Process is irreversible.
•  Equilibrium is attained readily. • Equilibrium is attained slowly.
• Not very Specific. • Highly Specific.

Production of Maleic Anhydride from n-Butane 33

 Selection of Absorbent
The choice of the process solution is determined by the
process pressure and temperature conditions at which the
gas to be treated is available, its composition with respect
to major and minor constituents and the purity requirement
of the treated gas.

Production of Maleic Anhydride from n-Butane 34

Properties of an ideal Absorber:
 A high solubility for the solute(s)
 A low volatility to reduce loss
 Stability and inertness
 Low corrosiveness
 Low viscosity and high diffusivity
 Low foaming proclivities
 Low toxicity and flammability
 Availability, if possible, within process
 A low cost

Production of Maleic Anhydride from n-Butane 35

Selection of Absorber Column

The Column which are used for absorption purposes are:

 Plate column
 Packed Column
 Spray Tower
 Bubble Column
 Centrifugal Contactor

Major types used in Industries are :

• Packed column
• Plate column

Production of Maleic Anhydride from n-Butane 36

 Packed Column Plate Column

• Provides continuous contact between vapor and • Plate column brings the two phases into contact on
liquid phases. stage wise basis.
• Relatively low pressure drop in packed column as • Additional friction generated as the vapor passes
compared to plate column. through the liquid on each tray.
• In a packed tower the liquid flows as a thin film • Because of the liquid on each plate there may be a
over the packing. Urge quantity of the liquid in plate column.
• For corrosive liquids, a packed column will usually • For corrosive fluids, plate column is usually
be cheaper than the equivalent plate column. avoided.
• Small space requirement. • Relatively large in size and expensive.

Production of Maleic Anhydride from n-Butane 37

38
 Selection of Packing
The packing is the most important component of the system. The packing
provides sufficient area for intimate contact between phases. The efficiency of
the packing with respect to both Height and flow capacity determines to a
significance extent the overall size of the tower. The economics of the
installation is therefore tied up with packing choice.

Production of Maleic Anhydride from n-Butane 39

 Packing Material
Ceramic Metal Plastic
• Superior wettability. • Good wettability. • May have poor
• Corrosion resistance at • Avoided in case of wettability at low liquid
Elevated temperature. corrosive fluids. rate.
• Bad strength. • Superior strength. • Inexpensive.
• Good strength.

Production of Maleic Anhydride from n-Butane

40
 Principal Requirement of a Tower Packing

1) It must be chemically inert to the fluids in the tower.

2) It must be strong without excessive weight.
3) It must contain adequate passages for both streams without excessive
liquid hold up or pressure drop.
4) It must provide good contact between liquid and gas.
5) It must be reasonable in cost.

Production of Maleic Anhydride from n-Butane 41

Common Packing types
are:
a) Berl Saddle.
b) Intalox Saddle.
c) Raschig rings.
d) Lessing rings.
e) Cross-partition rings.
f) Single spiral ring.
g) Double - Spiral ring.
h) Triple - Spiral ring.

Production of Maleic Anhydride from n-Butane 42

 Selection of Packing
For column diameter of greater than 0.9m, recommended
packing size is 2in. to 3in.
Intalox Saddles (2 in.) have been selected because;
 It provides a larger contact area per unit volume.
 It has an open structure, high bed porosity and more
mass transfer efficiency than others.
 Also provides high flooding limits and low pressure
drop.
 Material of packing is ceramic because it resist
corrosion.
Production of Maleic Anhydride from n-Butane 43
 Design Algorithm
Production of Maleic Anhydride from n-Butane 44
Specify separation
Selection of solvent
requirements

Select type of column,

packing type and size

Calculation of Column Mention all inlet and

Height outlet conditions with
flowrates

Evaluation of Pressure
Drop
Calculation of HETP

Calculation of Column
Calculations of N Diameter
(number of Surveying of Equilibrium data
theoretical stages) (equilibrium line and its slope
Production of Maleic Anhydride K)
from n-Butane 45
 Design Steps
Production of Maleic Anhydride from n-Butane 46
1. Flowrates and Compositions
2. Separation Component
3. Selection of Absorbent
4. Packing Selection
5. Selection of Column
6. Pressure Drop Calculations
7. Calculation of Column Diameter
8. Calculation of N
9. Calculation Of HETP
10. Calculation of Height

Production of Maleic Anhydride from n-Butane 47

 Calculations
Production of Maleic Anhydride from n-Butane 48
Composition of Entering Gaseous Mixture

Components Molecular wt. Moles Mole %

C4H2O3 98 16.81474 1.4586
H2O 18 81.19116 7.0433
C3H4O2 72 0.240211 0.0208
CH2O2 46 0.240211 0.0208
C4H10 58 4.275748 0.3709
O2 32 135.5748 11.7610
N2 28 903.6492 78.3909
CO2 44 5.861137 0.5084
CO 28 4.900295 0.4251
So,
Average Molecular Wt. of Gaseous Mixture = (M avg)v = 28.3869 kg/mol ≈ 29 kg/mol.
Production of Maleic Anhydride from n-Butane
49
 Calculations :

Flowrate of Entering Gas = V*w = 33421.295 kg/hr. Flowrate of Absorbent added = L *w = 7872.805 kg/hr.

Temperature of Entering Gas = Tv = 95OC = 368 K Temperature of Absorbent = TL = 45OC = 318 K

Pressure of Entering Gas = Pv = 1.9 atm Pressure of Absorbent = PL = 1.7 atm

Density of Entering Gas = ρv = PvM/RTv = 1.82 kg/m3 Density of Absorbent = ρL = 990 kg/m3 at 45OC

Average Mol. Wt. of Gas = (Mavg)v = 29 kg/mol. Viscosity of Absorbent = µL = 0.6 cp = 0.0006 kg/m.s
  ∗
𝐿 𝜌𝑉
Now, calculating the Flow factor =
𝐹 𝐿𝑉 =
𝑉
𝑊
∗
𝑊 √ 𝜌𝐿 = 0.01

=
  0.115
Estimating ΔP through Kister and Gill Empirical co-relation:
Where,
FP is called a “Packing factor” available in Literature for all type of Packing Elements.

Production of Maleic Anhydride from n-Butane 50

51
 CONT…
  From Table, FP = 40 ft-1 = 131.1 m-1
Now, (ΔP) = 1.18 inch of H2O/ft = 98.33 mm of H2O/m of packing height
Determining the value of K4 from the Graph to calculate Area of the Column using superficial gas flowrate V* w .

Now,
K4 ≈ 3.8
We Know that,
= 

So, 𝑲 𝟒 𝝆𝑽 ( 𝝆 𝑳 − 𝝆𝑽 )
  w=
V
[ 𝟏𝟑 .𝟏 𝑭 𝑷 ( 𝝁 𝑳 / 𝝆 𝑳 ) 𝟎 . 𝟏 ] 𝟎.𝟓

Vw = 4.081152 kg/m2.s
&
Vw = 33421.295 kg/hr / 3600 sec/hr

Vw = 9.28369 kg/s

Production of Maleic Anhydride from n-Butane

52
CONT…

We can now evaluate the Area of Column as:

Area Of Column = A = ( V*w / Vw ) = 9.28369 / 4.081152 = 2.274 m2

Now,

Tower Dia = D = ( 4 × A / π )1/2

D = 1.7 m

The Height of the Column can be calculated using a relation :

Z = HETP ( N )
Where,
HETP = Height equivalent to a theoretical stage.
N = Number of Theoretical stages required.

HETP can be determined using a Thumb Rule mentioned in Timmerhaus edition fifth.

HETP = D0.3 For Absorption Column with D > 0.5

HETP = D0.3 = ( 1.7 ) 0.3 = 1.1725

Production of Maleic Anhydride from n-Butane 53
 CONT…
Now,
  N

& NOG can be determined from a Graph:

Y1 / Y2 = P1 / P2 = 200 / 170 = 1.8

&
mGm / Lm = 1.92

Gm = 14692.1472 kg/hr
Lm = 3473.851075 kg/hr

Where,
m = Slope of Operating line (L / V)
(L / V) can be evaluated from the Operating line eq. which
is :
V ( Yn+1 – Y1) = L (Xn – X0)
Where,
X and Y are the mole fractions of solute inProduction
phase respectively.
liquid ofand vapor
Maleic Anhydride from n-Butane 54
CONT…
m = (L / V) = (0.003709 – 0) / (0.00817 – 0) = 0.45397 X Y T
Now, 0 0 0
A is called the ‘Absorption factor’ and can be obtained by :
A=L/KV 0.993 0.00007 340
Where,
0.994 0.000095 350
K is the slope of Equilibrium line.
K = 0.0002 0.995 0.00015 360
&
A = 117.8127 0.996 0.00015 370
Now,
0.99 0.00016 380
N = 9.138851722
And ultimately, 0.997 0.0002 390
Height of the Column = Z = 1.1725 × 9.138851722
1.009 0.00023 400
Z = 10.72 m
From the Graphical representation of
Allowance for liquid distribution = 1.2 m
this data, we obtained an equation :
Hence,
Total height of the Column = 11.9 ≈ 12 m y = 0.0002 x

Production of Maleic Anhydride from n-Butane 55

 CONT…

Liquid Distributors (Number of Streams required for liquid distribution) inside the column = N S = (D / 6)2 = ( 67/6
)2 = 125 (D in inches)

Liquid Hold Up by Packing = htw = 0.0004(L / dp) 0.6 = 0.0004(7872.805/0.0508)0.6 = 0.5203 m3 of water/m3 of
column volume

Production of Maleic Anhydride from n-Butane 56

 SPECIFICATION SHEET
Identification
Item Absorption Tower
Item number T-101
Type Packed bed Absorber
Function
Absorption of n-Butane from gaseous mixture
Design Specification
Operation Continuous Total Pressure Drop 8.68 kPa/m of packing
Operating Temperature 60OC Operating Pressure 170 kPa

Number of Theoretical 9 Height Equivalent to Stages 1.17

Stages (HETP)

Column Diameter 1.7 m Column Length 12 m

Number of Streams for liquid distribution (Liquid 125
Distributor)
Packing Specification
Type of Packing Intalox Saddle Material of Packing Ceramic
Arrangement of Packing Dumped Packing Support Simple grid & perforated
support 57
 Using ABSBR1
Equipment Model
from the Radfrac
Columns, I simulate
my Column to cross
check my design
parameters.
 Results are here:

Production of Maleic Anhydride from n-Butane

58
Heat Exchanger Design
2012-CH-418

Production of Maleic Anhydride from n-Butane 59

Production of Maleic Anhydride from n-Butane
60
 150◦C
Saturated steam 5 bar

C4H4O4 C4H4O4
C4H10 C4H10
C3H4O2 C3H4O2
CH2O2 Organic Stream Organic stream CH2O2
in out
H2O H2O

60 ◦C 120 ◦C

Saturated water
out 150 ◦C

Production of Maleic Anhydride from n-Butane 61

 Heat Exchanger

Why we need to exchange Heat? How heat exchanger work?

• You can see heat exchangers in all kinds of • One thing that all heat exchangers have in
places, usually working to heat or cool common is that they all function to directly
buildings or helping engines and machines or indirectly expose a warmer medium to a
to work more efficiently. cooler medium, hence, exchanging heat.
• A heat pump extracts heat from a natural • This is usually accomplished by using a set
geothermal hot spring, used to heat of tubes housed within some type of casing.
buildings at Hot Springs Lodge and Pool in Heat exchanger fans, condensers, belts,
Glenwood Springs. coolants, additional tubes and lines.

Production of Maleic Anhydride from n-Butane 62

Types of Heat Exchangers

• Shell & Tube Heat exchanger.

• Double pipe Heat exchanger.
• Pin type heat exchanger.

Production of Maleic Anhydride from n-Butane 63

 Why we need Heat Exchanger?
• They are used as components of air conditioning and cooling systems or of
heating systems.
• Within industrial plants and factories heat exchangers are required to keep
machinery, chemicals, water, gas, and other substances within a safe operating
temperature.
• . Heat exchangers may also be used to capture and transfer steam or heat
exhaust that is released as a byproduct of a process or operation so that the
steam or heat can be put to better use elsewhere, thereby increasing efficiency
and saving the plant money.

Production of Maleic Anhydride from n-Butane 64

 Selection Criteria
• Material of construction.
• Operating Pressure & Temperature.
• Thermal & Hydraulic Requirements.
• Material Availability.
• Operational Maintenance.
• Environmental Health & Safety Consideration & Regulations.
• Availability.
• Cost.

Production of Maleic Anhydride from n-Butane 65

 Shell and Tube Heat Exchanger
• Shell and Tube heat exchangers are most commonly used in heating or cooling
process fluids and gases. Typically found in applications where a need to heat
or cool large volumes exist, however small volume applications are also very
common.
• Shell and tube exchangers come in many variations to meet process
requirements in almost every industry or application. They deliver reliable heat
transfer performance by utilizing a high turbulence and counter flow, making
one or more passes. While one (1), two (2) and four (4) pass models are
standard, multi-pass custom models of any size are available.

Production of Maleic Anhydride from n-Butane 66

Why a Shell and Tube Heat Exchanger?
• The reasons for general acceptance of S&THX are several.
• The shell and tube heat exchanger provides a comparatively large ratio of
heat transfer area to volume and weight.
• It provides this surface in a form which is relatively easy to construct in a
wide range of sizes and which is mechanically rugged enough to withstand
normal shop fabrication stresses, shipping and field erection stresses, and
normal operating conditions.
• The shell and tube exchanger can be reasonably easily cleaned.
• Those components often subject to failure - gaskets and tubes – can be
easily replaced.
• Shop facilities for the successful design and construction of shell and tube
exchangers are available throughout the world .
Production of Maleic Anhydride from n-Butane 67
Production of Maleic Anhydride from n-Butane 68
 Design Algorithm
Production of Maleic Anhydride from n-Butane 69
• HX Selection • LMTD

Tube
Function
selection

Overall
Shell &
Heat
Tube side
Transfer
coefficient
coefficient
• Heat Transfer Area • Shell & Tube
side Pressure
Drop

Production of Maleic Anhydride from n-Butane 70

 Design Steps
Production of Maleic Anhydride from n-Butane 71
• Heat Exchanger Selection. • Pitch.
• Shell side Heat transfer coefficient.
• Function.
• Tube side Heat transfer coefficient.
• Flow Arrangements.
• Shell side & Tube side Pressure Drop.
• LMTD.
• Dirt Coefficient.
• Heat Transfer Area.
• Overall Heat transfer Coefficient.
• Tube Selection.

Production of Maleic Anhydride from n-Butane 72

General Design Consideration
Factor Tube-side Shell-side

Corrosion More corrosive fluid Less corrosive fluids

Fouling Fluids with high fouling Low fouling and scaling

and scaling

Fluid temperature Low temperature High temperature

Operating pressure Fluids with low pressure Fluids with high pressure
drop drop

Viscosity More viscous fluid less viscous fluid

Stream flow rate High flow rate Low flow rate

Production of Maleic Anhydride from n-Butane

73
 Calculations
Production of Maleic Anhydride from n-Butane 74
Log mean temperature : Heat Duty :
•Q  = mCp ∆t
•  ∆Tm =Ln []
Where

m = Mass Flow Rate

∆Tm = 31◦C
Cp = Heat capacity
∆t = Tem. Diff
Q = 675504

Production of Maleic Anhydride from n-Butane 75

Tube sizing : Birmingham Wire Gage

Production of Maleic Anhydride from n-Butane

76
 Cont….

Mass Flow Rate Of Steam : Tube Configuration :

•  
ms λ = Q  
•Outer Dia = O.D = 0.002 m
λ = Latent Heat of vaporization of Inner Dia = I.D = 0.016 m
Steam Lengths of Tubes = 4.88 m
= 2107.42 @ 150oC and 5 bar Area of one Tube = L * O.D *

Q = Hat Duty = 675504 = 0.303m2

Tube per pass = 44/2 = 22
ms = Mass Flow Rate Of Steam
Triangular Pitch = 1.25
= 0.086

Production of Maleic Anhydride from n-Butane 77

Guidelines for placing the fluid in order of priority

Production of Maleic Anhydride from n-Butane 78

 Cont…

Bundle & Shell Dia :

•  
Bundle Dia = (O.D) Tube (
Bundle Diametrical Clearance
K1 = 0.249
= 0.052 m
n1 = 2.207
Shell Dia = Bundle Dia + Clearance
Nt = 44
= 0.21 + 0.052 = 0.262 m
Db = 0.21 m

Use Split Ring Floating Head Type

Production of Maleic Anhydride from n-Butane 79

Cont...

Tube side Cross Sectional Area : Mass Velocity of Organic Liquid :

•A t = •mass
  flow rate of Organic Liquid

= 0.201 mm2 mt = 3.12

Tube Per pass = 22 Mass Velocity = Gt =

Total Flow Area = At *tube per pass = 585.3

= 0.00533 m2

Production of Maleic Anhydride from n-Butane 80

 Bundle diameter clearance
Production of Maleic Anhydride from n-Butane 81
 Cont….

Equivalent Diameter : Reynolds Number:

•D   =1.10 [  
•Re =
e t

= 0.0144 m = 4214.599

prandtal Number: Pr =

= 14.36

Choose 25% cut baffle.

Production of Maleic Anhydride from n-Butane 82

 Cont….

Tube Side Film Coefficient: Shell Side Film Coefficient:

 
•From Fig:  
•Baffle Spacing = Ds /5 =0.052m
Re =4214.592 Tube pitch = 1.25 * (O.D)tube
Jh = 6 * 10-2 = 1.25*0.002 = 0.025m
h t = Jh Cross- Flow Area =
= 3644 w/m2.0C As =
= 0.00274 m2

Production of Maleic Anhydride from n-Butane 83

 Cont…
• Thermal conductivity of cupro-nickle alloys = k w •  Over all Heat transfer Coefficient
= 50 w/m.◦C
Uo = 1538 w/m2.◦C
• Fouling coefficient :
Actual Heat Transfer Area =
For Organic Stream = hod
Ac =
= 300 w/m2.◦C = 14.16 m2
For Sream = 5000 w/m2.◦C

Production of Maleic Anhydride from n-Butane 84

H.T.C Of Heat exchanger

Production of Maleic Anhydride from n-Butane 85

Production of Maleic Anhydride from n-Butane 86
 Tube-side heat transfer factor

Production of Maleic Anhydride from n-Butane 87

 Cont…

Tube Side Pressure Drop : Shell Side Pressure drop :

At Re = 4214.599 •At  Re = 57142

jh = 5.5*10-3 Jh = 6 * 10-3

IB = 0.164 m Ds = 0.262 m
 

= 1972.81 Pa. = 49024.50 Pa

Production of Maleic Anhydride from n-Butane 88

 SPECIFICATION SHEET

Identification
Unit : Heat Exchanger H.T.A = 14.16 m2 Heat Duty = 675504 kJ/ hr
Item no. : E-102
Type : Shell & Tube
Function : To heat fluid from 60OC to 120OC
Operation : Continuous.
Parameters Shell Side Tube Side
Fluid Circulated Steam Organic Liquid & Water
Flow Rates 0.086Kg/sec 3.12Kg/sec
Temperature 150 C 60 to 120OC

Pressure Drop 0.48 atm 0.020 atm

Specifications Ds = 0.262 m I.D = 0.016m ,Length=4.8m
O.D = 0.002m, Nt= 44
17BWG, Pitch = 0.025m
Triangular pitch,

Production of Maleic Anhydride from n-Butane

89
 Distillation Design
2012-CH-426

Production of Maleic Anhydride from n-Butane 90

 To Atmosphere
Water 8

11 To waste treatment

T-101
2
E-103
Butane
4

V-102
3
To waste
treatment
1 R-101
C-101
14
P-101 A/B
AIR

6
T-102
9 10
5
V-101
13
E-101 E-102
12

R-102 E-104
PFD For Maleic Anhydride Production
Maleic Anhydride

Production of Maleic Anhydride from n-Butane 15 91

 Water out
350C E-103

Water in
250C
Malic anhydride 65.76197kg
V-102 Butane 0.707058079kg
Malic anhydride 1565.761kg Acrylic acid 1.09773E-11kg
Butane 0.707058kg Formic acid 0.304161159kg
Acrylic acid 1.929258kg Water 549.8561609kg
Formic acid 0.387177kg Total 616.629347kg
Water 555.4103kg
Total 2124.19kg 14

P-101 A/B

T-102

13

Sat. steam in
1640C

E-104
Sat. water out
1640C
Malic anhydride 1499.999kg
Acrylic acid 1.929258kg
15 Formic acid 0.083016kg
Water 5.554103kg

Production of Maleic Anhydride from n-Butane

Total 1507.57kg
92
 Distillation
“Distillation is the process of purification of compounds based on their relative volatility.”
In the project under consideration “Production of Maleic Anhydride from n-butane”,
Separation of Maleic anhydride from water is carried out using distillation.

Production of Maleic Anhydride from n-Butane 93

 Applications of Distillation
Few industrial applications are mentioned below:

• Salt water is turned into fresh water through distillation.

• Various forms of fuel, such as gasoline, are separated from crude oil by distillation.
• Alcoholic beverages are made through distillation.
• Separation of Maleic anhydride from water is done in distillation.

Production of Maleic Anhydride from n-Butane 94

 Types of Distillation
The three main types of distillation are:
• Fractional distillation
• Azeotropic Distillation
• Extractive Distillation
• Reactive Distillation

Production of Maleic Anhydride from n-Butane 95

 Fractional Distillation
Fractional distillation is the separation of a mixture into its component parts,
or fractions, separating chemical compounds by their boiling point by heating
them to a temperature at which one or more fractions of the compound
will vaporize. It uses distillation to fractionate. If the difference in boiling points
is greater than 25 °C, a simple distillation is used.
Examples :
Crude oil separation
Water-Maleic anhydride

Production of Maleic Anhydride from n-Butane 96

 Azeotropic Distillation
The term azeotropic distillation has been applied when specific azeotropic behavior is showed.
Azeotropic distillation techniques-in which an entrainer may be self or added externally-are
used throughout the petrochemical and chemical processing industries for the separation of
close-boiling, pinched, or azeotropic systems for which simple distillation is either too
expensive or impossible.
Examples
• Ethanol-water
• Nitric acid-water

Production of Maleic Anhydride from n-Butane 97

 Extractive Distillation
Extractive distillation is a partial vaporization process in the presence called the solvent, which
is added to alter the volatilities of the key components without the formation of any additional
azeotropes. Extractive distillation is used throughout the petrochemical and chemical
processing industries for the separation of close-boiling, pinched, or azeotropic systems for
which simple single-feed distillation is either too expensive or impossible.
Examples
• Benzene-cyclohexane
• Ethyl acetate-ethanol

Production of Maleic Anhydride from n-Butane 98

 Reactive Distillation
Reactive distillation is a unit operation in which chemical reaction and distillation are carried
out simultaneously within a fractional distillation apparatus. Reactive distillation may be
advantageous for liquid-phase reaction systems when the reaction must be carried out with a
large excess of one or more of the reactants, when a reaction can be driven to completion by
removal of one or more of the products as they are formed, or when the product recovery or
by-product recycle scheme is complicated or made infeasible by azeotrope formation.
• Methyl acetate from methanol and acetic acid
• Diphenyl carbonate from dimethyl carbonate and phenol

Production of Maleic Anhydride from n-Butane 99

 Selection of Distillation Column

Vapor liquid mass transfer operation may be carried either in:

 Plate Column.
 Packed Column.

Production of Maleic Anhydride from n-Butane 100

 Packed Column Plate Column

• Provides continuous contact between vapor and • Plate column brings the two phases into contact on
liquid phases. stage wise basis.
• Relatively low pressure drop in packed column as • Additional friction generated as the vapor passes
compared to plate column. through the liquid on each tray.
• In a packed tower the liquid flows as a thin film • Because of the liquid on each plate there may be a
over the packing. Urge quantity of the liquid in plate column.
• For corrosive liquids, a packed column will usually • For corrosive fluids, plate column is usually
be cheaper than the equivalent plate column. avoided.
• Small space requirement. • Relatively large in size and expensive.

Production of Maleic Anhydride from n-Butane 101

 Selection of Internal Plates Comparison
Factors Sieve Tray Valve Tray Bubble cap Tray Dual flow Tray

Capacity High High Moderate high Very high

Efficiancy High High Moderate high Least
Turn down ~50% ~25-30% 10% Least
Entrainment Moderate Moderate High Low to moderate
Pressure drop Moderate Moderate High Low to Moderate
Cost Low ~1.2 times sieve ~2-3 times of Least
trays sieve trays
Maintenance low Low to moderate Relatively high Low

Fouling tendency Low Low to moderate High: tends to Extremely low

collect solids
Effect of corrosion Low Low to moderate High Very low

Design information Well known Proprietary, but Well known Some information
readily available available. In stability can
occur in large diameter

Production of Maleic Anhydride from n-Butane

102
 Sieve Tray

Production of Maleic Anhydride from n-Butane 103

 Valve Tray

Production of Maleic Anhydride from n-Butane 104

 Bubble Cap

Production of Maleic Anhydride from n-Butane 105

 Design Algorithm
Production of Maleic Anhydride from n-Butane
106
 Start
Specified feed

Specify splits
of two key components

Estimate splits
of nonkey components

Determine column pressure and type of

condenser Bubble point / Dew point calculation

Repeat only if
estimated and Flash the feed
at column pressure Adiabatic flash procedure
calculated splits of
nonkey components
differ considerably
Calculate minimum theoretical stages
Fenske equation

Calculate
splits of nonkey components Fenske equation

Calculate
minimum reflux ratio Underwood equations

Calculate actual
theoretical stages
for specified reflux Gilliland correlation
ratio > minimum value

Calculate
feed stage location Kirbride equation

Calculate condenser
and reboiler duties Energy-balance equations

Exit
107
 Design Steps
Production of Maleic Anhydride from n-Butane 108
 Analytically Determining the
Specifications for a Distillation Column
• Step 1. Determine Process Operation Variables
• Step 2. Determine minimum number of plates using Fenske eq.
• Step 3. Determine the Minimum Reflux Ratio, Underwood Equation
• Step 4. Choose Theoretical Reflux Ratio
• Step 5. Determine Actual Number of Trays
• Step 6. Determine Feed-Stage Location using Kirkbride Empirical Equation
• Step 7. Principal Dimensions of the Column (Diameter/Height)

Production of Maleic Anhydride from n-Butane 109

 Calculations
Production of Maleic Anhydride from n-Butane 110
 Determine Process Operation Variables

• Selecting L.K and H.K

• Water (H­2O) & Maleic Anhydride (C4H2O3)
• Write equations for known variables and solve them for other unknown variables and
find them i.e distillate (D), bottom product (W) etc.

Production of Maleic Anhydride from n-Butane 111

 Minimum Equilibrium Stages Nmin
•  

Nmin = 3
where,

= minimum number of stages

= mole fraction of distillate w.r.t heavy key component

= mole fraction of distillate w.r.t light key component

= mole fraction of bottom w.r.t light key component

= mole fraction of bottom w.r.t heavy key component

= relative volatility , = volatility of light component, = volatility of heavy component

Production of Maleic Anhydride from n-Butane 112

 Underwood Equation for Minimum
Reflux R D,Min

•  

=1
Where,
= feed condition
= volatility of each component w.r.t heavy component
= fraction of each component
= common root

Production of Maleic Anhydride from n-Butane 113

 Minimum Reflux Ratio
•  

= 0.29161651
Where,
= Minimum Reflux ratio
= distillate

Production of Maleic Anhydride from n-Butane 114

 Actual Reflux Ratio

•  

Gilliland Correlation for Actual Reflux Ratio and Equilibrium Stages actual reflex
Rule of thumb

= 0.37910146

Production of Maleic Anhydride from n-Butane 115

 Actual Number of Equilibrium Plates
•  

N =08
where,

Production of Maleic Anhydride from n-Butane 116

 Kirkbride Empirical Equation Feed-
Stage Location
•  

N= +
=2
=6
where,
= number of plates in rectifying section
= number of plates in stripping section
Feed stage = 6

Production of Maleic Anhydride from n-Butane 117

 Height of Column
•  
• [ft]
• = 18.4 [ft]

Production of Maleic Anhydride from n-Butane 118

 Diameter Of Column
•  
• FP = 0.000422

• = 0.052778
• = mass flow rate of liquids
• = mass flow rate of vapors
• = volumetric flow rate of liquids
• = volumetric flow rate of vapors

Production of Maleic Anhydride from n-Butane 119

 Diameter Of Column
•  
• = 32.32272 ft/s
• where,
• = surface tension in dynes/cm
• = capacity factor

• 7.388974 ft/s

Production of Maleic Anhydride from n-Butane 120

 Diameter Of Column
•  
• , ft/s

• , ft
• Dia = 4.69 ft

Production of Maleic Anhydride from n-Butane 121

 Tray Design
Production of Maleic Anhydride from n-Butane 122
 Tray Design
 
•Determine Flv

Flv = 0.032267754
(calculated from the diameter calculations)
From figure, (Separation Process Engineering by Phillip C. Wankat)
Fractional entrainment is .08 for 75 % flooding, Ψ = .08
Solving for e,

Production of Maleic Anhydride from n-Butane 123

Estimate flooding Calculate Ψ (fractional entrainment)

Production of Maleic Anhydride from n-Butane

124
 Tray Design
 
•Calculate Atotal

Calculate tray efficiency, η

From table 10-1 calculate lweir/Dia, and calculate lweir

lweir/Dia = 0.726 lweir = 3.63

Production of Maleic Anhydride from n-Butane 125

 Tray Design
•Calculate
  Active area

Choose value of β (0.07 ≤ β ≥ 0.16), initial guess 0.1

Calculate hole area on the tray

Calculate vapor velocity through the holes

Choose hole size and tray thickness (best to choose from the given standards) and calculate
• Calculate orifice coefficient, C0

Production of Maleic Anhydride from n-Butane 126

 Calculate F weir

Production of Maleic Anhydride from n-Butane 127

 Tray Design
•Calculate
 

Calculate hcrest

Assume hgrad ~ 0, for Valve tray and specify down comer with appropriate gap (for Valve tray 1-in gap is suitable)

• Calculate

• Calculate

Production of Maleic Anhydride from n-Butane 128

 Tray Design
•Calculate
  total pressure drop across the tray

Results
Convert the value in terms of ∆P, and check. If the value of ∆P is such that 0.7 kPa ≤ ∆P ≤ 1.4
kPa the calculations are valid. Otherwise revise the calculations and the approximations.
The pressure drop calculated for single tray is 1.01 kPa. Since, the typical pressure drop for
valve trays in the range from 0.7 to 1.4 kPa per tray. The calculated pressure drop is reasonable
hdc = 1.01 kPa

Production of Maleic Anhydride from n-Butane 129

 Specification sheet
identification
Item Distillation
Item no. T-102
No. required 1
Tray type valve
Operation continuous
Function
Separation of maleic anhydride from water
Material Handled
Parameters Feed Top Bottom
Quantity 1565.761 kg/hr 65.761967 kg/hr 1499.9992kg/hr
Composition of Maleic Anhydride 32% 2% 98%
Temperature 160⁰C 98⁰C 162⁰C
Design Data
No. of trays 8
Pressure 1.2 atm
Height of column  18.4 ft
Diameter of column 4.694626 ft
Reflux ratio 1.3
Tray spacing 0.5 m 130
131
Acknowledgements

132
 Column Control System
• The control system in the distillation column is important in order to have a
sharp separation between the components in the incoming feed.
• The control system of distillation column is controlled based on three
purposes:

Material balance control

• Product quality control

Satisfaction of constraints

Production of Maleic Anhydride from n-Butane 133

Fair’s procedure
this method first calculate vapor velocity that will cause flooding due to excessive
entrainment, then use rule of thumb to determine the operating velocity, and from this
calculate the column diameter
use English units
ch 10 staged and packed column design
tray spacing
it is selected according to maintenance required because it has been little effects on tray
efficiency.
Tray spacing is usually greater in large diameter columns. A minimum of 0.4572m with
0.6096m typical is used.
With the typical 24-inch tray spacing Csb,f ~ 0.33ft/s

134