Production of Paracetamol from

Para-aminophenol and Acetic Anhydride

Group # 4
Material Balance
Reactor
Compone Stream %age Stream 2 %age Recycle %age
nts 1 (kg/hr) Stream
(kg/hr) (kg/hr)

Paracetamol 354.2 27.3

56.28 7.2
Acetic acid 140.7 10.9
Para amino
phenol 258.3 19.9 2.6 0.19
Recycle stream
Acetic
Anhydride 265.8 20.5 26.6 2.05 Stream 1
Water 774.8 59.6 774.8 59.7 736.1 92.8
Total 1298.9 100 1298.9 100 792.38 100

Input(kg/hr) Output(kg/hr)
1.3x103 1.3x103 Stream 2
Nutchse Filter
Compon Strea %age Stream %age
ents m2 Stream 3 %age 4
(kg/hr) (kg/hr) (kg/hr)

Paracetam
ol 354.2 27.3 353.8 99.4 0.42 0.05
Acetic acid 140.7 10.9 140.7 14.9
Para amino
phenol 2.6 0.19 2.4 0.6 0.21 0.03
Acetic
Anhydride 26.6 2.05 26.6 2.82
Stream 2
Water 774.8 59.7 774.8 82.2 Stream 3
Total 1298.9 100 356.12 100 942.7 100

Input(kg/hr) Output(kg/hr)
1.3x103 356.12+942.7 = 1.3x103

Stream 4
Distillation Column

Distillate
Distillate

Stream 4 Waste
 Distillation Column
Stream4 %age Distillate %age Waste %age
Components (Kg/hr) (Kg/hr) (Kg/hr)
Acetic
Anhydride 0.42 0.05 0.8 0.09 25.8 90.4
Acetic acid 140.7 14.9 138.6 15.2 2.1 7.4
Water 0.21 0.03 774.8 84.7 0
Paracetamol 26.6 2.82 0 0.4 1.47
Para amino
phenol 774.8 82.2 0 0.2 0.73
Total 942.7 100 914.2 100 28.5 1

Input(kg/hr) Output(kg/hr)
942.7 914.2 + 28.5 = 942.7
Mixer
Stream 3(a) %age Stream 3(b) %age Stream 5 %age
Components (kg/hr) (Kg/hr) (kg/hr)
Paracetamol 353.8 99.4 353.8 33.7
PAP 2.4 0.6 2.4 0.23
Activated
charcoal 5.4 0.78 5.4 0.51
Water 688.3 99.22 688.3 65.56
Total 356.2 100 693.7 1 1049.9 100

Input(kg/hr) Output(kg/hr)
356.2 + 693.7 = 1.05 x 103 1.05 x 103
Tube press filter
Components Stream 5 %age Stream 6(a) %age Stream 6(b) %age
(Kg/hr) (Kg/hr) (Kg/hr)
Paracetamol 353.1 0.6
353.8 33.7 33.9 7.5
PAP 2.4 0.23 2.4 28.4
Water 688.3 0.51 688.3 66.1
Activated
Charcoal 5.4 65.56 5.4 64.1
Total 1049.9 100 1041.4 100 8.4 100

Input(kg/hr) Output(kg/hr)
1.05 x 103 1041.4 + 8.4 = 1.05 x 103
Crystalizer
Compounds Stream6(ai) %age Stream 6(aii) %age Stream 7 %age
(Kg/hr) (Kg/hr) (Kg/hr)
Paracetamol 353.1 33.9 353.1 33.9
Water 688.3 66.1 688.3 66.02
Na2S2O3 0.8 100 0.8 0.08
Total 1041.4 100 0.8 100 1042.2 1

Input(kg/hr) Output(kg/hr)
1041.4 + 0.8 = 1.04 x 103 1.04 x 103
Centrifugal separator
Compounds Stream 7 %age Stream 8(a) %age Stream 8(b) %age
(Kg/hr) (Kg/hr) (Kg/hr)
Paracetamol 353.1 33.9 352.3 100 0.8 0.12
Water 688.3 66.02 688.3 99.75
Na2S2O3 0.8 0.08 0.8 0.13
Total 1042.2 1 352.3 100 689.9 100

Input(kg/hr) Output(kg/hr)
1.04x 103 352.3 + 689.9 = 1.04x 103
Evaporator
Compounds Stream8(b) %age Stream 9 %age Stream 10 %age
(Kg/hr) (Kg/hr) (Kg/hr)
Paracetamol 0.8 0.12 0.5 100 0.3 0.04
Water 688.3 99.75 688.3 99.84
Na2S2O3 0.8 0.13 0.8 0.12
Total 689.9 100 0.5 100 689.4 100

Input(kg/hr) Output(kg/hr)
689.9 0.5 + 689.4 = 689.9
Overall Balance
Input (Kg/hr) Output (Kg/hr)
258.3 774.8
265.8 26.6
774.8 140.7
5.4 0.4
688.3 0.2
0.8 5.4
2.4
0.6
352.3
0.8
0.8
688.3
1.2 x 103 1.2 x 103
Energy Balance
Reactor
Steam inlet

P = 4-5 bar
Tsat = 421 K

Stream 1 Stream 2
T = 393 K Products
Reactants P = 1 bar
T = 298 K ∆Hr = -1.1 x 105 (KJ/kmol)
T = 298 K
P = 1 bar Q = -9.7 x 104 (KJ)
P = 1 bar

P = 1 bar
Tsat = 373 K
Steam Outlet
 Reactor Basis = 1hr

∆Hf ∆Hf
Reactants n(kmol) (KJ/kmol) Q (KJ) Products n(kmol) (KJ/kmol) Q (KJ)
AA 2.6 -625000 -1627077.8 Para 2.3 -441000 -1033259
PAP 2.4 -190000 -449665.1 Acetic acid 2.3 -487000 -1141037
Total -815000 -2076742.9 Total -928000 -2174297

∆Hr (KJ/kmol)= ∆Hf (products) - ∆Hf (reactants) -928000 – (-815000) = -1.1 x 105

Q (KJ) = Q(products) - Q(reactants) (-2174297) - (-2076742.9) = -9.8 x 104

For steam
Tin = 421 K
Tout = 373 K
Cp∆T = -1.9 x 104 KJ/kmol
Q = -9.8 x 104 KJ
Q = nCp∆T
n = Q/Cp∆T = -9.8 x 104/ -1.9 x 104
n = 5.2 kmol
m = n x M = 5.2 x 18 = 93.6 Kg
 Condenser
Water in
T = 306 K
P = 2 bar

Inlet Outlet
T = 393 K T = 393 k
P = 1 bar P = 1 bar

T = 312 K
P = 2 bar
Water out
Condenser Basis = 1hr
∆H(latent)
Components n (kmol) T (k) (KJ/kmol) Q (KJ)
Water 43 393 39000 1678777.4
Acetic acid 0.9 393 24390 22858.2
Total 1.7 x 106

(Condenser Duty) Mass flow rate of water needed

Inlet temperature 306 K
Outlet temperature 312 K
Cp∆T 1.5 x 103 KJ/kmol
Heat Exchanged = Q = 1.7 x 106 KJ
Mass flow rate ?
n Q/Cp∆T
n 1.7 x 106 /1.5 x 103
n 1.1 x 103 kmol
m 1.1 x 103 x 18
m 2 x 104 Kg
 Cooler

Inlet Outlet

T = 393 K T = 368 K
P = 1 bar P = 1 bar
 Basis = 1hr Inlet
∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) T1(k) Tr(k) (J/kmol) (kJ/kmol) Q = nCp∆T (kJ)
Water 43 393 298 -29815.8 -29.8 -1283.4
Acetic acid 0.9 393 298 -14391.5 -14.4 -13.5
Total Q (-1283.4)+(-13.5) = -1.3 x 103
Outlet
∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) Tr(k) T2(k) (J/kmol) (kJ/kmol) Q = nCp∆T (kJ)
Water 43 298 368 20356.2 20.4 876.2
Acetic acid 0.9 298 368 9825.5 9.8 9.2
Total Q 876.2 + 9.2 = 885.4

Total
Net Q = Qout - Qin -441.6
Distillation Column
Distillate
T = 290 K
P = 0.8 bar

Inlet
T = 298 K
P = 1bar

Waste
T = 413 K
P = 2 bar
 Distillation Column

Distillate Basis = 1hr

∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) Tr(k) T2(k) (J/kmol) (kJ/kmol) Q = nCp∆T (kJ)
Water 43.1 298 290 -1805.247133 -1.8 -77.6
Acetic acid 2.3 298 290 -871.3608358 -0.9 -0.007
AA 0.008 298 290 -1643464480 -1643464.5 -3779967
∆Hd (KJ/kmol) -77.6 + (-0.007) + (-3779967) = -3780045
Waste
∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) Tr (k) T2 (k) (J/kmol) (kJ/kmol) Q = nCp∆T (kJ)
AA 0.3 298 413 32865955737 32865955.7 8299392.3
Acetic acid 0.03 298 413 18488 18.5 0.7
∆Hd (KJ/kmol) 8299393

Outlet ∆Hd (KJ/kmol) 229857.6026 + 8299393 = 8529250.6

Mixer
Steam in
P = 2-3 bar
Tsat = 401 K
Inlet Outlet

T = 298 K T = 363 K
P = 1 bar P = 1 bar

P = 1 bar
Tsat = 373 K
Steam out
 Mixer

Outlet Basis = 1hr

∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) Tr (k) T2 (k) (J/Kmol) (kJ/kmol) Q = nCp∆T (kJ)
Water 38 298 363 18611 18.6 711.7

For steam
Tin = 401 K
Tout = 373 K
Cp∆T = -53.56 KJ/kg
Q = 711.7 KJ
Q = nCp∆T
n = Q/Cp∆T = 711.7/ -53.56 ( negative sign shows
that heat will be
transferred from steam
to mixer)
m = 13.28 kg
Evaporator
Steam in

P = 2-3 bar
Tsat = 401 K
Inlet Outlet
T = 298 K T = 373 K
P = 1 bar P = 1bar

P = 1 bar
Tsat = 373 K

Steam out
 Evaporator
Basis = 1hr
Outlet
∆H = Cp∆T ∆H = Cp∆T
Component n (kmol) Tr (k) T2 (k) (J/Kmol) (kJ/kmol) Q = nCp∆T (kJ)
Water 38.2 298 373 22149.4 22.1 846.9

For steam
Tin = 401 K
Tout = 373 K
Cp∆T = -53.56 KJ/kmol
Q = 846.9 KJ
Q = nCp∆T
n = Q/Cp∆T = 846.9/ -53.56 ( negative sign shows
that heat will be
transferred from steam
to mixer)
m = 15.812 kg
Condenser Water (in)

T = 306 K
P = 2 bar
Inlet Outlet
T = 373 K T = 373 K
P = 1 bar P = 1 bar

T = 312 K
P = 2 bar

Water (out)
Condenser
Basis = 1hr
Components n (kmol) T (k) ∆H(latent) (KJ/kmol) Q (KJ)
Water 38.2 373 40000 1.5 x 106

(Condenser Duty) Mass flow rate of water needed

Inlet temperature 306 K
Outlet temperature 312 K
Cp∆T 1.5 x 103 KJ/kmol
Heat Exchanged = Q = 1.5 x 106 KJ
Mass flow rate ?
n Q/Cp∆T
n 1.5 x 106 /1.5 x 103
n 1 x 103 kmol
m 1 x 103 x 18
m 1.8 x 104 Kg
Equipment Design
Reactor Design

Haseeb Mustafa

by
2015-CH-404
Reactor

The reactor is the heart of a chemical process

In a reactor raw materials are converted into

products, and the reactor design is a vital step in
the overall design of the process
Chemical Reactor design considerations

The design of an industrial chemical reactor must satisfy the following:

The chemical factors: the kinetic of the reaction

The mass transfer factors

The heat transfer factors

The safety factors

 Reactor
Types of reactors

Mode of Operation
1. Batch type
2. Continuous type
i. Mixed flow
ii. Plug flow
3. Semi batch type

End use based classification Catalyst based classification

Phases based classification

1. Polymerization reactors 1. Homogeneous

1. Single phase
2. Biological reactors 2. Heterogeneous
2. Multiple phase
3. Electrochemical reactors
 Mode of operation

Mixed flow Semi batch

Batch reactor Plug flow reactor
reactor reactor
• Reactants added and • Reactants flow through
operated at desired • Reactants are added at • Some reactants are
operated conditions and a hollow pipe and are loaded into the reactor
conditions to achieve reacted
required conversion products are removed and the rest are fed
at the same time • No contact of a gradually
• Stirring is done by reactant with the
internal impellers or • Agitation is done by • Once the reactor is full
internal impellers or previous one it is then operated in a
gas bubbles
internal recycling batch mode

Reference:
Chemical Reaction Engineering by Octave Leven Spill
Advantages of Batch Reactor over other Reactors

For small scale production

Very slow reaction

Flexibility in production
Factors Influencing the reaction rate

Concentration
Nature of reaction
Temperature
Pressure
Catalyst
 Heat Transfer
Basic reactor
elements
Mass Transfer
 Material Balance

Reactor Input Reactor Output

Components Mass (Kg/hr)
Components Mass (Kg/hr)
Para-aminophenol 2.6
Para-aminophenol 258.3
Acetic Anhydride 26.6
Acetic Anhydride 265.8 Paracetamol 354.2
Acetic Acid 140.7
Water 774.8
Water 774.8
Total 1298.9
Total 1298.9
 Energy balance

Reactants Energy Products Energy

Components Energy (kJ) Components Energy (kJ)

Para-aminophenol 449665.13 Paracetamol -1033259

Acetic Anhydride 1627077.8 Acetic Acid -1141037

Total 2076742.9 Total -2174297

Overall heat
∆Qt = Qprodcuts – Qreactants
∆Qt = -2174297 + 2076742.9
∆Qt = -97553.7 kJ
 Batch Reactor
Steam inlet

P = 4 bar
Tsat = 421 K

Reactants Stream 1 Stream 2

PAP, AA, Water T = 393 K Products
Reactants P = 1 bar
1298.9 Kg/hr
T = 298 K ∆Hr = -1.1 x 105 (KJ/kmol) T = 298 K
P = 1 bar Q = -9.7 x 104 (KJ) P = 1 bar

Products P = 1 bar
Para, PAP, AA, Acetic Acid, Water Tsat = 373 K
1298.9 Kg/hr Steam Outlet
 Reference:
Omran Moradlou and Mohammad Ali Zare “Kinetic Study of
Design Steps Paracetamol Hydrolysis: Evaluating of the Voltammetric
Data”

Basis : 1hr Temperature: T = 393 K

Para-aminophenol = B, Acetic Anhydride = C, Water = D

• Volume = mass/density
• Volume of reaction mixture: V = VB + VC + VD

• Arrhenius Equation: log k = log A – Ea/2.303RT

• Rate Constant: k = 0.15 min-1

Design Specifications
Quantity Symbol Value
Volume of reaction mixture V 258.3/1.13 + 265.8/1.08 + 774.8/1

Volume of reaction mixture V 1.3 m3

Activation Energy Ea 63.61 kJ/mol

Frequency Factor A 3.11 x 107 min-1

Ideal gas constant R 8.314 J/mol.k

Temperature T 393 K

Order of reaction n 1
For Para-aminophenol
• Moles = nB = 2366.67
• Concentration = CBo = nB/V = 1.89 mol/dm3

-rB = kCBn

• Conversion: xB = 0.99

Reference
Chemical Reaction Engineering
By: Octave Leven Spill
 From “xA” vs “1/-rA” curve we have:

xa 1/ra

0.9 35.27337

0.85 23.51558

0.7 11.75779

0.6 8.818342

0.45 6.41334

0.3 5.039053

0.2 4.409171

0.1 3.919263

0 3.527337
 V = (π/4)D2L
Quantity Symbol Value

Slope t/CB0 28.17 min.dm3/mol

Reaction time tr 53.24 min = 0.88 hr

(Charging + Discharging + Cleaning) time t 1 hr

Batch time tb = tr + t 1.88 hr ≈ 2hr

Batches per day nb 24/2 = 12

Volume of reactor Vr = v0t 0.88 x 1.3 = 1.14 m3

Safety allowance 20%

Reactor volume V 1.14 x 1.2 = 1.4 m3

Length to diameter ratio L/D 3

Reactor Diameter D 0.83 m

Reactor Length L 2.51 m

Design of Agitator

• Impeller diameter Da = 0.9D = 0.75m

• Impeller height above vessel floor E=Da = 0.75m
• Length of Impeller blade L=Da/4 = 0.21m
• Width of Impeller blade W=Da/5 = 0.17m
• Number of Impellers = 1
• Number of impeller blades = 3
• Baffle width 0.1D = 0.083m

Reference:
Anqi Zhou “Experimental determination of the mixing requirements
for solid suspension in pharmaceutical stirred tank
reactors”
 continue
Design of Agitator
• Tip velocity = 4m/s
• Tip velocity = πDaN
• Speed of Impeller =N = 4/(ᴨ x 0.75) = 1.7 ≈ 2 rev/sec
• Power number =Np = 6
• Power = Np x N3 x Da5 x ρ/gc = 1.13 hp
• Assume impeller is 85% efficient:
• Actual Power required = 1.13/0.85 = 1.33 hp
Condenser
Design

Minahil
By: 2015-CH-430
Qumreen
Heat Exchanger

A heat exchanger is a device used to transfer heat between two or more

fluids.

These are used for both cooling and heating purposes

i.e. space heating, refrigeration, air conditioning, power stations, chemical plants,
petroleum refineries, natural-gas processing.
 Heat exchanger Types

Shell and tube heat Plate and frame heat

exchanger exchanger
Spiral heat exchanger
It has one shell and no. It has plates on which
Double pipe heat It has circulated tubes tunnels are present for
exchanger of tubes
It is applied for fluid flow
•It has a single shell and It needs less space for moderate pressure
installment It is suitable for low
a single pipe. drop applications mass flow rates.
It needs large space for It builds high pressure
its installment. drop.
It has less pressure
drop. Reference:
Process Heat Transfer by D.Q. Kern
Chemical Engineering Design by Coulson and Richardson
 Able to withstand high
pressure

Less expensive

Easy to disassemble and

inspect
Reason for the selection of shell
and tube heat exchanger
Flow can be co-current,
counter current

Less fouling

High heat transfer

efficiency
 Wills and
Design Methods Kern Method Bell Delaware Johnston
Method Method

Give reasonably
satisfactory
Why kern prediction of the Applicable for all
Simple to apply. flow types and
method? heat-transfer
coefficient of flow rates.
standard design.
 Start
Accept all design parameters END

Collect the physical properties

and HE specifications Calculate Tube side and
Shell-side pressure drop

Calculate unspecified flowrates

Calculate ΔTlmtd Estimate tube ide and shell
side heat transfer coefficient

Assume values of overall

coefficient Determine fouling factors

Reference
Calculate Heat Transfer Area Process Heat Transfer
Shell size and tube count
and number of tubes by D.Q Kern
Fluid Placement

Cooling water inlet

Steam Inlet

Cooling water
Condensate outlet
outlet
Shell and head type

Hence a type AJS exchanger is specified.

Front Head A:For dirty tube side fluid placements

Shell type J: Used often for shell side condensers.

Rear Head S: Gives higher tube bundle to shell

clearance

TEMA standard
Design Specifications
Quantity Symbols Values (fps) Values (SI Units)
Tube outer diameter Do 0.75 in 0.019 m
Tube inner diameter Di 0.584 in 0.015 m
Tube Bundle square - -
geometry
Pitch Pt 1 in 0.025 m
Thermal Conductivity k 0.03 Btu/hr.ft.oF 0.016 J/s.m.K
Tube length Lt 8 ft 2.44 m

BWG - 14 -
Baffle cut Bc 20 % -

Density ρ 62.6 (lb/ft3) 1004 (kg/m3)

 Hot stream In Temperature= 248 oF
Acetic acid Flow rate=1909.91btu/hr
Acetic anhydride Pressure= 1 bar
water

Temperature= 80.6 oF
Cold stream out Flow rate=51040.1 btu/hr
Water Pressure= 2 bar

Temperature= 113 oF
Cold stream In
Flow rate=51040.1 btu/hr Water
Pressure= 1.99 bar

Temperature= 248 oF Condensed stream out

Flow rate=1909.91 btu/hr Acetic acid
Pressure= 0.703 bar Acetic anhydride
Water
Design Calculation
Mass flow (lb/hr) Latent heat
Compounds Mass flow (Kg/hr) M (Btu/lb)

Water 751.58 1653.47 973.72

Acetic Acid 112.58 247.68 169.81

Acetic Anhydride 3.98 8.76 185.46

Total 1909.91
 Temperature oC oF

t1(cold) 27 80.6
t2(cold) 45 113
T1(hot) 120 248
T2(hot) 120 248

T1 – t2 = 135 oF
T2 – t1 = 167.4 oF
Tlmtd = 150.62 oF
 Quantity Symbol Value

For hot stream Q = M*λ 1.7 x 106 btu/hr

For cold stream m = Q/Cp ΔT 51040.1 lb/hr

Assume design heat Ud 90 Btu/hr.ft2.oF

transfer coefficient
Heat Transfer Area A = Q/(Ud)*(Tlmtd) 121.9 ft2

Number of tubes nt = A/πDoL 78

Reference for Ud value:

https://www.engineeringpage.com/technology/thermal/transf
er.html
 Quantity Symbol Value

Reynold Number Re = 4m(np/nt)/πDiµ 5.7x 105 np

Number of tube passes np 1

Checking of tube side fluid v = 4m(np/nt)/ πρDi2 1.6 ft/s

velocity

Shell Inner diameter ds 12 in = 1 ft

Tube count nt 81

Required overall coefficient Ureq = Q/nt*π*Do*L*ΔTlmtd 86.3 Btu/hr.ft2.oF

 Quantity Symbol Value

φi (µ/µw)0.14 =1.0

Reynold Number Re 573134

Inner heat transfer hi = (k/Di)*0.023Re0.8*Pr1/3*(µ/µw)0.14 262.3 Btu/hr.ft2 oF

coefficient

Condensate loading Г* = M/L*nt0.667 12.7 lbm /hr.ft

• Calculate ho
Average film temperature
Assume Tw = 125 oF

Tf = 0.75 Tw + 0.25 Tv = 155.75 oF

• Condensate viscosity
µL = 0.00941exp(1668/T) = 0.14 cp
• Outside heat transfer coefficient
ho = 1.52*kL3*ρL(ρL - ρv)*g/4*µL Г*
= 390 Btu/hr.ft2 oF
• Calculate Tw and Tf
Tw = (hi(t,av) + ho(Do/Di)Tav)/(hi + ho(Do/Di))
= 196 oF
Tf = 0.75 Tw + 0.25 Tv = 209 oF
• Recalculate ho
µL = 0.00941exp(1668/T)
= 0.11 cp
 ho = 1.52*kL3*ρL(ρL - ρv)*g/4*µL Г*
= 419 Btu/hr.ft2 oF

Since this value is close to the previous one, no further iterations are
required

• Overall coefficient
• Fouling factor for the cooling water is = 0.001 h · ft2 · oF/Btu

• For condensing vapor a fouling factor is = 0.0005 h · ft2 · oF/Btu

Reference
http://www.hcheattransfer.com
Ud = [(Do/hiDi) + (Doln(Do/Di)/2ktube) + (1/ho) + (Rdi*Do/Di) + Rdo]-1
= 107 Btu/hr.F.ft2

Since UD >Ureq , the condenser is thermally acceptable

• Tube side pressure drop

f = 0.4137Re-0.2585 = 0.013
G = m(np/nt)/Af = 338917.4 lbm/h. ft2
ΔPf = f*np L*G2/7.5*1012Di*s*Φ = 0.13 psi
• For turbulent flow in U-tube
αr = 1.6np-1.5 = 0.1

ΔPr = 1.334*10-13αr*G2/s = 1.5x10-3 psi

• Table indicates that 10-in. nozzles are appropriate for this unit.
Assuming that schedule 40 pipe is used, the Reynolds number
for the nozzles is
Ren = 4*m/π*Di*µ= 44689
Gn= m/(π/4)*Di2 = 93254.5 lbm/h.ft2
ΔPn= 2*10-13NsGn2/s = 1.7 x 10-3 psi
• The total tube-side pressure drop

ΔPi = ΔPf + ΔPr + ΔPn = 0.13 psi

• Shell-side pressure drop
G = M/as = 38198.2 lbm/h.ft2
Re = DeG/µv = 52066
f1 = (0.0076 + 0.000166*ds)Re-0.125 = 0.037

f2 = (0.0016 + 5.8*10-5*ds)Re-0.157 = 0.012

f= 144(f1-1.25(1.B/ds)(f1-f2)) = 1.828
• Baffle Clearence
nb + 1 = L/B = 40
• Shell Side pressure drop for the total flow as vapor

(ΔPf)vo = f*G2 *ds*(nb+1)/7.5*1012De*s = 13.04 psi

Φ-2vo =0.33 for a total condenser

ΔPf = φ-2vo(ΔPf)vo = 4.3 psi
 Ktube = 26 Btu/hr.ft.oF

• Clean overall coefficient

Uc = [(Do/hiDi)+((Do*ln(Do/Di))/2ktube)+1/ho]-1
= 131.8 Btu/h.F.ft2

• Over surface and over design

Over-surface = Uc/Ureq -1
= 0.52 = 52%
Over-design = Ud/Ureq -1
= 0.24 = 24%

Reference for Ktube: https://www.google.com/search?rlz=1C1GGRV_enPK752PK752&ei=ZdG0XLjsEsSvkwWR-4roDQ&q=conductivity+of+

carbon+chart&oq=conductivity+of+carbon+chart&gs_l=psy-ab.3...9781.13594..14034...0.0..0.380.3544.2-7j5......0....1..
gws-wiz.......0i71j0i7i30j0i7i5i30j0i8i7i30.eDQoiT3b4kA
Centrifuge Design

By
Ali Ihsan
Reg No. 2015-CH-439
 Liquid-Solid separators

The need to separate solid and liquid phases is probably the most
common phase separation requirement in the process industries, and a
variety of techniques is used. Separation is affected by either the
difference in density between the liquid and solids, using either gravity
or centrifugal force or for filtration depends on the particle size and
shape.
Centrifuge
Centrifuges are classified into two
types according to mechanism used
for separation:

Sedimentation Centrifuges:
In it, separation is done on the basis of difference
in densities between solid and liquid phases.

Filtration Centrifuges:
In it, separation is done by filtration process.

Reference:
“Chemical Engineering Design ” by Coulson and Richardson Vol 6
Sedimentation has further four types
Tubular Bowl:
High speed, vertical axis
,used for the separation
of immiscible liquids or
fine particles. Disc Bowl:
Solid Bowl Batch
It split the liquid flow into a
Centrifuge:
number of very thin layers
It is used in our which increases separating
Process efficiency. Used for
separating fine solids and for
Scroll discharge: solids classification.
In this type, solids deposited on
walls are removed by scroll. It is
designed so that solids can be
washed and relatively dry solids be
discharged.
 Reason to use Sedimentation
Centrifuges
We use Sedimentation Solid Bowl Batch Centrifuge
because we are using batch process in our project.

Sedimentation Process is used when L/D ratio is less

than 1.

When we require sufficient residence time for our

process.
 Material Balance
Input Output Stream 1
Paracetamol 352.2
Components Mass
Flowrate(kg/hr)
Output Stream 2
Paracetamol 353.1
Components Mass
Flowrate(kg/hr)
Water 688.3
Paracetamol 0.84
Na2S2O3 1.3
Water 688.3
Na2S2O3 1.3
Total 1042.7
Total 690.5
 Paracetamol Water Na2S2O3
Density(kg/m3) 1260 997 1670

Mass 353.1 688.3 1.3

Flowrate(kg/hr)
• Paracetamol = X, Water = Y, Na2S2O3 = Z
• Volumetric Flowrate= Q = Mass Flowrate/Density
• Total Volumetric Flowrate = Q = Qx+ Qy+ Qz
• Total Volumetric Flowrate = 0.97 m3/hr
 Design Steps
• Diameter of Particle = ds = 5μm = 5 x 10-6 m
• Viscosity of Water = 0.89 cp = 8.9 x 10-4 Kg/m.s

By Stoke’s law:
• Settling Velocity = ug = ds2(ρp-ρs)g/18μ

• Settling Velocity = 0.14 m/hr

References:
1. “Chemical Engineering Design” by Coulson and Richardson
Vol 6
2. Henry H Y Tong and Albert Chow “Particle Size Analysis in
Pharmaceutics: Principles, Methods and Applications” 3
• Now Area of the centrifuge: A= Q/2ug
Area = 3.47m2

• Diameter of the centrifuge = [4A/π]0.5

= 2.1 m
• Radius
R = D/2 = 2.1/2 = 1.05m
• Pressure
P = 100 N/m2
• Force
F = PA
F = 100 x 3.47 = 347 N
• Linear Velocity
F = mv2/2 v = √(2F/m)
v = 0.81m/s
• Angular velocity
ω = v/R = 0.77 rad/sec
ω = 2πrad = 2 x π x 0.77 = 4.8rev/sec

Pressure Reference:
CITI Pharmaceuticals Industrial Limited
• Radius of Inner Surface of liquid (ri)
P = ρω2(R2 – ri2)
ri = 0.9 m
•h
h = R – ri = 1.05 - 0.9 = 0.15m

• Residence time
tR = 18μh/d2(ρs – ρ)Rω2
tR = 0.41 hr

Refrence:
“Chemical Engineering ” by Coulson and Richardson Vol 2
• Volume of Centrifuge
Q = ug Rω2V/h*g
V = 0.43m3
• Height of Centrifugal Column
V=πD2H/4
H = 0.12m
Distillation Column Design

Muhammad
Sohaib Riaz

by
2015-CH-441
Distillation Column

Distillation is a process where a

mixture made of two or more
liquids with different boiling points
can be separated from each other
 Distillation Column

Types of Columns

Mode of Operation

1. Batch type
2. Continuous type

The nature of the feed The number of product streams Where the extra feed exits

Binary column Extractive distillation

Multi-product column Azeotropic distillation
Multi-component
column
Advantages of Batch over Continuous Column

For small scale production

High level of chemical purity

Provides large amount of flexibility

Why Plate Column!

Packed Column Plate Column

Handle wide Range

Suitable for high
of Liquids and Gas
liquid flow rates Flow rates

Packings are Cleaning is easier

generally more than Packed
expensive Column

Smaller diameter
High liquid
column less than
Residence Time
0.60 m
 Why sieve Plate !

• Sieve Plate: Valve Plate : Bubble-Cap Plate

Cost • 3 : 1.5 : 1.0

Capacity • Sieve Plate > Valve Plate > Bubble-Cap Plate

Pressure Drop • Bubble-Cap Plate > Valve Plate > Sieve Plate

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11
 Distillate
Material Balance Component Mass
s (Kg/hr)
Acetic
Column Input
Anhydride 26.2
Component Mass Acetic Acid 4.2
s (Kg/hr) Water 774.8
Acetic Total 805.2
Anhydride 26.6
Acetic Acid Waste
140.7
Water Component Mass
774.8 s (Kg/hr)
Total 942.1
Acetic
Anhydride 0.4
Overall Mass Balance Acetic Acid 136.5
Massoutlet = Massinlet Water 0
136.9+805.2 = 942.1 Total 136.9
 Distillate
Energy balance Components Energy (kJ)
P = 0.8 bar Water -77.6
Inlet stream Energy Acetic Acid -0.007
T = 393 K
Acetic -3779967
Componen Energy (kJ)
Anhydride
ts
Total -3780045
Water 0 T = 298 K

Acetic Acid 0 P = 1 bar

Acetic 0 Waste
Anhydride Components Energy (kJ)
Total c0 Water 0
P = 2 bar
Overall heat Acetic Acid 0.7
T = 413 K
∆Qt = Qoutlet – Qinlet Acetic 8299392
∆Qt = 4519348 - 0 Anhydride
∆Qt = 4.52*106 kJ Total 8299393
 Design steps

Minimum Number of Stages

Minimum Reflux
Ratio

Actual reflux ratio

Theoretical Number of Stages

Location of Feed Plate

Diameter of Column

Height of Column

Pressure Drop
Design Steps
Components Feed (Kmol) Distillate(Kmol) Waste(Kmol)
Acetic Anhydride 0.26 0.26 0.004
Acetic Acid 2.34 0.07 2.27
Water 43.04 43.04 0
Total 45.64 43.37 2.274

Basis: 1 hr

F = 45.64 kmol
D= 43.37 kmol
W= 2.274 kmol
Acetic Acid=A , Acetic Anhydride= B Water=C

Heavy Key: Acetic Acid Reference:

Light Key: Acetic Anhydride 1.Principle of mass transfer and separation process By Binay K. Dutta
2. Chemical Engineering Design By Coulsen and Richardson 3rd Ed. Vol. 6
• Minimum No of Plates:
log(((na,d)∗(nb,w))/((nb,d)∗(na,w)))/
Nmin =
log(αAB)av

na,d & na,w = moles of acetic acid in distillate and Retentate

Nb,d & nb,w = moles of acetic anhydride in distillate and Retentate

Nmin= 7
• Underwood Equation:
Σ(αi*Zi/αi-ø)=1-q

Vmin =Σ(αi*Dxi,d/αi-ø)

Vmin = 121 kmol

• Minimum Reflux Ratio:

Vmin = (Rmin + 1) D

Rmin = 1.79
• Optimum Reflux Ratio:
R = 1.2Rmin

R= 2.15
• Gilliland Equation For Theoretical Number Of Plates:
R − Rmin
X = ( R + 1 ) = 0.11

1+54.4X x−1
Y =1 - exp{(11+117.2X )*( x0.5 ) =0.54

Y = (N - Nmin)/(N + 1)

N = 16.4≈ 16
• Feed Tray Location:

• KirkBrid Equation

ZHk xLk,w W
NR/Ns = {( Z /)*((xHk,d)2)*( D )}0.206
Lk

NR/Ns = 0.2605676

Ns = 12.96 ≈ 13
NR =3.3073052 ≈ 3
Flow rates inside the column:
For Rectifying Section:
• Ln = R (D) = 2.15(43.4) = 93.2 Kmol/hr
• Vn = D(R+1)= 43.4(2.15+1)=136.6 Kmole/hr

For Stripping Section:

• Lm = Ln + F = 93.2 + 45.6 = 138.8 Kmole/hr

• Vm = Lm – W =138.8 - 2.3 = 136.5 Kmole/hr
 Flooding Velocity and Column Diameter

Lw=liquid flow rate

Vw=Vapor flow rate
Vapor density
Liquid density

Top Bottom
FLV=0.1 FLV=0.04

97
From fig 11.27

K1 (Top) = 0.065 K1 (Bottom) = 0.058

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 568
 𝑽n x M.W
• Maximum volumetric flow-rate (V) = ῥ x 3600
𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒
• Area required = 𝑣𝑎𝑝𝑜𝑟 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦

Area × 4
• Diameter = 𝜋
ρL − ρV
Uf = K1 ρV
Top Condition Bottom Condition

Uf = 1.64m/s Uf =1.8 m/s

Uf = Flooding Velocity
Ṹf = 1.4 m/s Ṹf =1.5 m/s
K1 = Coefficient obtained from
chart V =1.1 m3/s V =1.6 m3/s

Ac =0.8 m2 Ac =1.2 m2

Ắc =0.9 m2 Ắc =1.36 m2

D =1.04 m D =1.32 m
Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical 99
Engineering Design R. K. SINNOTT ,chapter 11
Plate Design
Column diameter = Dc = 1.32 m
Column area = Ac = 1.36 m2
Down comer area = Ad =0.12 X 1.36= 0.16 m2
Net area = An = Ac - Ad
= 0.9 – 0.16
= 0.74 m2
Active area = Aa = Ac - 2Ad
= 0.9 - 2(0.16) = 0.58 m2

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 572
Take hole area as 10% of active area
Hole area = Ah = 0.58 x 0.1 = 0.058 m2

from figure 11.31

lw/Dc = 0.75
lw = 0.75 x1.32 = 0.99 m
lw = Weir length

Assumption:
Weir height = 50 mm
Hole diameter = 6 mm
Plate thickness = 5 mm
Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 573
 Weeping
Lm ×M.W
Lw = 3600

Maximum liquid rate = 5.6 kg/s

Minimum liquid rate (at 70% turndown ratio)(Lwd) = 5.6 x 0.7 = 3.9 kg/s

Lw 2/3
how = 750 ρL ×lw

Maximum , how = 22.38 mm

Minimum , how = 40.33 mm

At Minimum rate hw+ how = 22.38 + 40.33 = 62.71 mm

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 571
From fig. 11.30, K2 = 30.3

Minimum vapor velocity =

K2 −0.90(25.4−dh )
uො h min = ρv

= 10.9 m/s

Minimum vapor rate

Actual minimum vapor velocity =
Hole area

=0.7* Maximum volumetric Flow rate/ dh

= 13 m/s
As actual minimum vapor velocity is greater than minimum
vapor rate, So, there is no weeping
Check Flooding

uv = max. volumetric flow rate / net area

= 1.1/0.9
uv = 1.2 m/s
𝑢𝑣 (𝑏𝑎𝑠𝑒𝑑 𝑜𝑛 𝑛𝑒𝑡 𝑎𝑟𝑒𝑎)
Percentage flooding =
𝑢𝑓
= 1.2/1.7

= 75 %

As the percentage flooding is well below the design figure of

85, the Column diameter could be reduced, but this would
increase the pressure drop. Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 570
 Perforated Area
lw/Dc = 0.75

Fig. 11.32 gives c = 101o

Angle subtended at plate edge by unperforated strip =

=180 - 101 = 79
Mean length, unperforated edge strips
=(Dc- 0.05) π* c /180
= (1.32 – 50 × 10-3)π × 79/180
= 1.75 m

Area of unperforated edge strips = 50 × 10-3 × 1.75 = 0.087 m2

Mean length of calming zone = lw + width of unperforated strip

= 0.99 + 50 x 10-3 = 1.04 m

Area of calming zone = 2(1.04 × 50 × 10-3) = 0.104 m2

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 574
Total area for perforations = Ap =Hole Area –Area of edge strips

- Mean length of calming zone

= 0.58– 0.087- 0.104 = 0.389 m2

Ah/Ap = 0.058/0.389 = 0.149,

from fig 11.33

lp/dh = 2.55

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION
Chemical Engineering Design R. K. SINNOTT ,chapter 11,page 575
Plate Pressure Drop

Downcomer pressure loss

Take hap = hw - 10 = 62.71 - 10 = 52.71 m
Area under apron,
Aap = hap x lw
Aap = 0.047 m2
As this area is less than Ad = 0.1 m2, we use Aap in the following equation.

2
𝐿𝑤𝑑
hdc = 166
𝑝𝐿 × 𝐴𝑎𝑝

hdc = 2.02 mm
Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
Engineering Design R. K. SINNOTT ,chapter 11,page 576
Dry plate pressure drop
Max. flow rate 1.1
uො h = = = 18.96 m/s
𝐴ℎ 0.058
Ah 0.058 ∗100
= = 14.9
Ap 0.389

From fig. 11.34, for plate thickness/hole diameter =0.82

Co= 0.77

𝜌 uh 2
hd = 51 𝜌𝑣 =36.85 mm Liquid
𝐿 CO

12.5 ×103
hr = = 11.57 mm Liquid
ρL
Total plate pressure drop

ht = hd + ( hw + max how ) + hr

ht = 36.85 + ( 62.71 + 22.38 ) + 11.57

Reference:
Coulson & Richardson’s CHEMICAL ENGINEERINGVOLUME 6 FOURTH EDITION Chemical
ht = 133.51 mm liquid Engineering Design R. K. SINNOTT ,chapter 11,page 575
Backup in down comer
hb = ht + hd + ( hw + max how )
hb = 133+ 36.85 + ( 62.71 + 22.38 )
hb = 254.94 mm = 0.254m
0.254 < ½ ( plate spacing + weir height )
0.254 < ½ (0.3 + 0.005)
So, plate spacing is acceptable.

Residence time
𝐴𝑑 × ℎ𝑏 ×
𝜌𝐿
ℎ𝑟 =
𝐿𝑤𝑑

ℎ𝑟 = 2.8 s
 Height of the column

Height (z) of the distillation column can be find by the given below formula,
Hc = (Nact -1)Hs + ΔH
Where;
Hc = actual column height
Nact = actual no of trays
Hs = plate spacing
ΔH = additional height requires for column operation (10ft top and bottom)

Hc = (15 x 0.3) +6
=10.5 m

110
 Specification Sheet
Tray Type Sieve Tray
Number of Trays 16
Diameter of Column 1.32 m
Tray Spacing 0.3 m
Total Pressure drop 0.89 psi , 0.06 bar
Weir Height 0.05 m
Weir Length 0.99 m
Height of Column 10.8 m
Hole-area 0.058 m2

111