Professional Documents
Culture Documents
A Final Year Plant Design Project On Production of 75 Tons of Oxalic Acid From Sugar Cane Molasses Using Nitric Acid
A Final Year Plant Design Project On Production of 75 Tons of Oxalic Acid From Sugar Cane Molasses Using Nitric Acid
1
CONTENTS
2
INTRODUCTION
3
MARKET SHARE OF OXALIC
ACID IN MAJOR SECTORS IN
2018.
http://www.pbs.gov.pk/sites/default/files//MONTHLY%20BULLETIN%20OF%20STATISTICS%20%
20NOVEMBER%2C%202018.pdf 5
MANUFACTURING
PROCESSES
http://ethesis.nitrkl.ac.in/5372/1/109CH0030.pdf
6
COMPARISON OF MANUFACTURING
PROCESSES
Designation Temperature Pressure(atm) Time (hrs.) Yield(%)
(C0 )
From 65 1 3 75
Oxidation of
Molasses
Mixing of saw 200-220 2 3 80
dust with
caustic soda
By olefins 60-100 1 2 85
and glycol
From Sodium 2000 150 2 88
Formate
From 250-300 2 2 85
Propylene
By Using 300 1 7days 61
Aspergillus
Niger
7
PROCESS DESCRIPTION
Process of making Oxalic acid:
• Treatment of the raw material(Molasses, Nitric acid, V2O5) in
Batch Reactor.
• Separation of Oxalic acid from unreacted material in 2-stage
Crystallization Process.
• Drying of Oxalic acid Crystals in Drier.
Treatment of Polluting Gas Nitric Oxide(NO):
• Conversion of NO to NO2 in Fluidized bed reactor in presence
of Al2O3 catalyst
• Absorption of NO2 in Water in Absorption Column in making
weak HNO3(by-product)
https://patents.google.com/patent/CN1030747A/en 8
Air Polluting Gas Treatment Section
CYCLON
HNO3/ SEPARATOR
V2O5 P-21 Pure
water NO
Molasses P-11
(glucose)
NO
NO AL2O3 cat E-7
AL2O3
NO+NO2
P-8
P-36
Hot
P-31 water Hot air
out
P-35
Hot air
Feed Holding Tank Crystalizer-1 in
Centrifuge-1 P-34
Centrifuge-2
P-41
10
MATERIAL BALANCE
Raw Material
Sugar cane Molasses Composition:
Glucose : 80%
Sucrose : 2 %
Water 17.8
Others:
Nitric Acid: HNO3(liq.)
Catalyst : V2O5
11
MATERIAL BALANCE
Process Equipment's on which material balance is applied:
• Isothermal Batch Reactor
• Fluidized Bed Reactor
• Absorber
• Crystallizer
• Centrifuge
• Drier
12
OVERALL BALANCE
Production of oxalic acid= 75TPD
C6H12O6 + 6HNO3 V2O5 3[COOH]2*6H2O +6NO
• Glucose Required
66646.8 kg/Batch
• Nitric Acid Required
139954.5 kg/Batch
• Catalyst V2O5
936 kg/Batch
13
BATCH REACTOR
C6H12O6 + 6HNO3 V2O5 3[COOH]2*6H2O +6NO
Yield = 75%
14
FLUIDIZED BED REACTOR
2NO + O2 2N02
Conversion of NO to NO2 is 90%
NO
O2 31.25 1000 (unreacted) 6.9425 208.275
Al2O3 0.347 34.71Al2O3 0.347 34.71
Total 3117.47 3117.47
15
ABSORBER
3NO2 + H2O 2HNO3 + NO
Conversion is 80%
23.4583333
H2O 15 270NO 3 703.75
NO
(unreacted) 6.9425 208.275NO2 (unreacted) 12.5 575
Total 3357.75 3357.75
16
CRYSTALLIZER-1
Balance sheet for crystallizer 1
Input Output
Component Feed in Kg Component Feed in Kg
103476
Oxalic acid 74999.99 Crystals
H2O 29991.65 Mother Liquor 53165
Glucose(unreacted) 16660
Nitric acid(unreacted) 34989
18
TURBO DRIER
Air required
536590 kg/B
19
C6H12O6 NO NO2 H2O
66646.8 kg/B V2O5 2082.75 2874.19 kg/hr 270
Al2O3
HNO3 936 kg/B kg/hr. Unreacted NO kg/hr.
34.71 kg/hr. 208 kg/hr
139954.5 O2
kg/B 1000 kg/hr
Reactor Fluidized
Absorber
Bed Reactor
Oxalic
acid + C=103476
unreacted kg/B
H2O=47758
material M=53165
C=103476 Kg
156641.97 kg/B
kg/B
kg/B
Crystallizer Centrifuge 1 Crystallizer
1 2
C=76234
kg/B
Air= 536590 kg
M=75000
kg/B
Dry Crystals Drier Centrifuge
75000 kg/day
C=76234 kg/B 2
Moisture =1234kg
ENERGY BALANCE
Specific heat capacity (kJ/kg K) of compounds
21
ENERGY BALANCE
Specific Heat Capacity of component KJ/Kg: T=338 K
Glucose = 1.21 KJ/Kg K
Oxalic acid= 1.62 KJ/Kg K
Nitric acid= 0.92 KJ /Kg K
Nitric oxide= 0.97 KJ/Kg K
Specific Heat Capacity of component KJ/Kg: T=313 K
Nitric oxide= 0.95 KJ/Kg K
Specific Heat Capacity of component KJ/Kg: T=368 K
Nitrogen Dioxide = 0.86 KJ/Kg K
Nitric acid= 0.99 KJ/Kg K
https://webbook.nist.gov/cgi/cbook.cgi?ID=C7697372&Mask=1&Type=JANAF
G&Table=on
22
BATCH REACTOR
Energy Balance For Reactor
Nitric oxide 2082.75 1.34 335 934946.8 Nitrogen- 2874 0.86 70 173024.8
29
DRIER
Amount of Oxalic acid crystal required=75000 kg
Amount of Oxalic acid fed into the drier=76234 kg
Therefore, amount of water evaporated = 76234-75000 =1234 kg
Inlet temperature of feed= 25C0
required temperature of hot air = tC0
∆t= tC0-25C0
Latent heat of vaporization= 2270 kJ/kg
Therefore, heat required to evaporate 1234 kg of
water=q=2270*1234=2801180 kJ
Specific heat of water= 4.187 kJ/kg C
Mass of water =1234 kg
Given temperature ∆t= tC0-25C0
30
DRIER
31
NO
CYCLON
139954kg/Batch HNO3/ SEPARATOR
936kg/Batch V2O5 P-21
T=20C Pure
66646kg/Batch Molasses P-11 water NO
(glucose) 49986.2
NO T=18C
kg/Batch NO AL2O3 cat E-7
AL2O3
P=6 bar
T=65C T= 360C
NO+NO2
3082Kg/hr.
P-8
T=95C
P = 1bar
T= 65C Steam Heater NO Gas
Oxalic ∆ T=360-550C 2082kg/hr.
Steam Heater
acid+Unreacted
∆ T=25-65C Reactor material
Compressor Absorber
O2 GAS
T=65C 1000Kg/hr. FBR
156641.9kg Weak
Activated Carbon Filter HNO3 T=95C
156641.9Kg P-36
Hot T=85C
P-31 water Hot air
T=25C 47758kg out
Q=470 P-35
T=37C
KW T=25C
Q=493
KW Hot air
103476kg 76234kg in
Feed Holding Tank T=65C Crystalizer-1 Centrifuge-1 P-34
Centrifuge-2
P-41
32
MATERIAL OF CONSTRUCTION
33
EQUIPMENT DESIGN
• Crystallizer
• Batch Reactor
• Heat Exchanger
• Absorber
34
CRYSTALLIZER
Equipment Crystallizer
Crystallizer Type Agitated Cooler Crystallizer
MOC Mild Steel
Feed rate 1.7 kg/s
Total Cooling Duty 470 kW
Height 4.6 m
Diameter 1.8 m
Thickness of shell 169 mm
Thickness of hemispherical Head 51 mm
Weight 372826 N
35
FORMULAE USED
𝐹𝑖𝑛∗𝐶𝑖𝑛−𝐹0∗𝐶0
• %age yeild of crystals = ∗ 100
𝐹𝑖𝑛∗𝐶𝑖𝑛
• Heat Transfer Area Required = Q/U*∆Tlm
• Height of Crystallizer = ,A= π*D*H , H=2.5D
• H = 1.15*Hreq
• Wall thickness of cylindrical section of vessel = t =(Pi*di) /(f-Pi)
• Thickness of hemispherical head of vessel = t = (Pi * Di) / (4Jf – 1.2Pi)
• Wv = 240Cv*Dm*(Hv+0.8Dm) *t
Cv= a factor account for the weight of nozzels, internal supports,
So, Cv=1.15 for vessels with plate support rings
36
BATCH REACTOR
Equipment Reactor
Reactor Type Batch Reactor
MOC Stainless steel
Weight of Catalyst 936 kg
Volume of Catalyst 0.64 m3
Volume of Reactor 52 m3
Diameter of Vessel 2.1 m
Height of Vessel 6.4 m
Weight of Vessel 209801 N
Pressure 1 bar
Temperature 65 C0
Thickness of Hemispherical Head 37 mm
Thickness of Cylindrical shell 127 mm
37
Thickness of Cooling Jacket 0.35 m
FORMULAE USED
𝑋𝑎 𝑑𝑋𝑎
• Wcat= 𝐹𝐴0 ∗ 0
−𝑟𝑎
𝐹𝐴0 𝑋𝑎 𝑑𝑋𝑎
• Vreaction = ∗ 0 𝑑𝑡
−𝑟𝑎
• Vreactor = 1.15* Vreaction
• V=πd2L/4
• For Reactor, Estimated Ratio , L=3d
• Weight of vessel=Area *Density*thickness
• Wall thickness of cylindrical section of vessel = t =(Pi*di) /(f-Pi)
• Thickness of hemispherical head of vessel = t = (Pi * Di) / (4Jf – 1.2Pi)
38
HEAT EXCHANGER
Fluid Units Shell Side(NO gas) Tube Side(Steam)
Cold Fluid Hot Fluid
Total Flow Kg/hr. 2082 4860
Density Kg/m3 0.97 0.507
Viscosity mNm-2s 4e-4 3.2e-4
Specific Heat KJ/kgC0 1.052 2.2
Capacity
Thermal Conductivity KW/mC0 0.05 0.08
Temperature C0 Inlet =360 C0 Inlet=600 C0
outlet=550 C0 outlet=560 C0
Operating Pressure bar 2 2
Fouling Coefficient W/m2C0 2000 7000
39
Equipment Shell & Tube Heat Exchanger
MOC 304 Stainless steel
Heat load 118 kW
∆Tlm 93.29 C0
Heat transfer area 23 m2
Inner Dia. Of Tube 19 mm
Outer Dia. Of Tube 14.83 mm
Length of tube 1.4 m
No. of tubes 364
ht 238 W/m2C0
1.25 Square Pitch
Bundle Dia. 561 mm
Clearance(split ring floating head) 50 mm
Shell Dia. 611 mm
Baffle Spacing 122 mm
Equivalent Dia. 11.46 mm
hs 278 W/m2C0
Over all heat transfer co-efficient 100 W/m2 C0
40
FORMULAE USED
• Heat load = m*Cp*∆T
• Heat transfer area A = Q/U*∆Tlm
• For 1.25P0 Square Pitch, Db = d0(Nt/k1) ^1/n1
𝜋
• Cross sectional area of tube = ∗ 𝑑𝑖2
4
4200∗ 1.35+.02∗𝑡𝑚 𝑢𝑡 .8
• Tube-Side Heat Transfer Co-efficient =hi=
𝑑𝑖
𝑝𝑡−𝑑0
• Cross flow area of shell side =As = ∗ 𝑙𝑏 ∗ 𝑑𝑠
𝑝𝑡
𝐾 .33
• Shell Side Heat Transfer Co-efficient =hs = ∗ 𝑅𝑒 ∗ 𝑗ℎ Pr
𝐷0
1 1 𝑑0∗𝑙𝑛𝑑0/𝑑𝑖 𝑑0 1 𝑑0 1
• 1/Uo = + + + * + *
ℎ𝑠 5000 2∗50 𝑑𝑖 2000 𝑑𝑖 ℎ𝑡
41
ABSORBER
Equipment Absorber
MOC Stainless steel
Column Packed Column
Temperature 95 C0
Pressure 1 bar
Feed Gas Rate 3082 kg/hr.
NO2 93 %wt.
NO 7 %wt.
Mole Fraction of NO2 in feed 0.89
Partial Pressure of NO2 in feed 0.89 bar
Solubility data of NO2 in water:
Mass fraction NO2 Partial
of NO2 in Pressure in Source: Data from Perry, J.H.1973.Chemical
water gas(bar) Engineers’ Handbook .5th.edn,.McGraw-
0.12 0.1 Hill,.New.York.
0.18 0.2 https://coifpm.com/wp-content/uploads/2018/07/26.-
0.35 0.5 Tan_2013_2.pdf
0.79 0.89
42
0.83 1
Mole.Fraction.of.NO2.in.Liquid.Phase.and.Gas.Phase.at.Equilibrium
Mole fraction of NO2 in Mole Fraction of NO2 in
water(x) Gas Phase(Y)
0 0
0.115 0.2
0.3 0.5
0.46 0.75
0.65 1
𝐿 𝐿𝑚
=1.57
1 = 1.80 𝐺𝑚
𝐺
0.8
0.6
0.4
0.2
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Mole fraction of NO2 in liq phase(x)
P = 1 bar
Series1 operaing line(min) Operating line(max) T = 95 C0
NOG = 6
44
So, number of theoretical stages are 6.
ABSORBER
Equipment Absorber
Gas Flow rate 0.874 kg/s
Liquid Flow rate 1.62 kg/s
Type of Packing Intelex saddles
Material of Packing Ceramic
Size of Packing 38mm
HOG 0.75 m
NOG 6
Height of Packing 4.5 m
Height of Column 5.1
Diameter of Column 1.1 m
45
FORMULAE USED
46
COST ESTIMATION
It includes: It includes:
Design Start up
Equipment and interaction Catalyst cost
Piping instrumentation and Raw material
control system Finished
Building and structure product inventories
Auxiliary facilities such as
utilities
47
OXALIC ACID PLANT COST
INDEX
48
DIRECT COST
https://www.alibaba.com/trade/search?f0=y&IndexArea=product_en&CatId=&SearchText=batc
h+reactor&isPremium=y&refine_attr_value=1477-8225 49
INDIRECT COST
50
COST ESTIMATION OF OXALIC
ACID PLANT
Fixed Capital Investment Rs. 19.48*108
Working Capital Rs. 2.119*108
Total Capital Investment Rs. 21.598*108
Annual Production Cost Rs. 30.96 * 108
51
RISK ASSESSMENT
52
HAZARDS OF OXALIC ACID
54
HAZOP STUDY FOR REACTOR
Guide word Parameter Deviation Causes Consequences Action
57