Extractive Separation of Azadirachtin from Neem Seed Kernels

1
BHARATI VIDYAPEETH DEEMED UNIVERSITY
COLLEGE OF ENGINEERING, PUNE – 411043
DEPARTMENT OF CHEMICAL ENGINEERING
ACADEMIC YEAR: 2015-2016
A Project Report on Extractive Separation of Azadirachtin from Neem Seed
Kernels
By
THANMAYEE SHASTRY – 1200000233
RAJESH KUMAR - 1100000743
PARMANAND SHARMA – 1100000741
Under the guidance
Dr. P. V. CHAVAN

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BHARATI VIDYAPEETH DEEMED UNIVERSITY
COLLEGE OF ENGINEERING, PUNE
DEPARTMENT OF CHEMICAL ENGINEERING
ACADEMIC YEAR: 2015-2016
CERTIFICATE
This is to certify that THANMAYEE SHASTRY,RAJESH KUMAR AND
PARMANAND SHARMA have satisfactorily carried out the report entitled
“Extractive Separation of Azadirachtin from Neem Seed Kernels” in our premises
under the guidance of Dr. PRAKASH V. CHAVAN for fulfillment of B.Tech Project
report in the final year of Chemical Engineering Bharati Vidyapeeth University
College of Engineering Pune-43.
Date:
Dr. P.V.CHAVAN Dr. P.V.CHAVAN (External)
(Project Guide) (Head of Department)

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ACKNOWLEDGEMENT
First of all, I would like to thank the supreme power the almighty god who is obviously the one has
always guided me to work on the one has always guided me to work on a right path of life. I would
also like to thank my parents because of whom I am studying in this college.Without both of their
grace this project could not have became a reality.
Next to them I would like to specially thank my Project Guide Dr. P.V. Chavan who guided and
motivated us at every point to make this project successfully. I would also like to thank my project
partners who helped me to accomplish this project successfully.

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INDEX:
SR.NO TOPICS PAGE NO.
1. INTRODUCTION 05
2. LITERATURE SURVEY 08
3. SYSTEM SELECTION 10
4. PROCESS FLOW DIAGRAM AND PROCESS DESCRIPTION 12
5. THERMODYNAMIC FEASIBILITY 15
6. QUANTIFICATION 17
7 MATERIAL BALANCE AND ENERGY BALANCE
8 KINETICS AND DESIGN
9 COST ESTIMATION
10 P & ID AND UTILITY DIAGRAM
11. CONCLUSION
12. REFERENCES

5
INTRODUCTION:
With increasing awareness for pesticidal residues in environment due to indiscriminate use of
synthetic pesticides, biopesticides are attaining increased attention as they are safe, natural product
for insect and pest control.The Indian Neem tree, nearly 18.14 million (2014-15) trees, is a fast
growing robust tree found throughout India. Nearly the entire tree roots, leaves and fruits can
potentially be used for agricultural, industrial and commercial products. The neem tree, which yields
about 30-40 kg/year of the seeds, is widely distributed in South Asian and several other tropical
countries
In particular, formulations made from Neem used as Bio pesticides. Neem seeds consists of
liminoids upto 2.5 % such as Azadirachtin (A to K), Nimbin, Salannin, Nimbidin, Nimbindiol,
Gedudin, Salannol etc. Also it contains 15-45% edible oil composed of oleic acid, linoleic acid,
palmitic acid, stearic acid etc. The rest is the waste solid part.
Azadirachtin (AZ) (C35H44016), a tetranortriterpenoid from the Neem tree (Aza-dirachta indica A.
Juss), has generated wide academic and industrial interests. The compound and extracts containing it
have been found to have potent and specific effects against a variety of insect pests. Although AZ is
present to the extent of 0.2-0.6% in Neem kernels, its isolation in a pure state is necessary [1]
. AZ
content in crude neem oils varies from negligible to more than 4000 ppm.[2,3]
Limonoids are soluble
in polar and mid-polar solvents and slightly soluble in water.
This compound is highly potent at low concentrations against more than 200 agricultural pests and it
is eco-friendly. Thus, it has the potential to be a safe alternative to the toxic synthetic pesticides and a
number of commercial formulations are being introduced world-wide.
Unfortunately, the purification of AZ is difficult to accomplish, especially on a preparative scale, due
to the complexity and similarity- in-structure of the chemicals found in the seeds and foliage of the
Neem tree[1]
. AZ, first isolated by Butterworth and Morgan[4]
from Neem (Aza- dirachta indica A.
Juss.) kernels, has been studied intensively during the past 15 years by organic chemists probing and
finally solving its intricate molecular architecture and by entomologists on account of its powerful
antifeedant and hormonal activity towards many species of insects .
Separation of AZ and other limonoids from neem seed or oil can be carried out by using various
methods[1,7,12-15]
. Common features of these methods are that they employed a combination of several
chromatography methods to obtain high purity limonoids. Chromatography steps were applied after
preliminary separation of crude limonoids from oils or seeds. But this couldn’t be applied to
industrial scale.

6
Extraction of limonoids from seeds or oil was then usually conducted by using solvent partition
with aqueous alcohol and hexane or petroleum ether to produce crude extract with terpenoid content
of 2–6%. And gradually various other methods like Supercritical Solvent[13]
, Pressurized Liquid
Extraction[11]
etc. were also developed.
AZ is thermally unstable and rapidly destroyed by heating in solvent[5]
. Thus, elimination of AZ
heating in solvent is expected to increase separation efficiency of AZ.
Some Properties of AZ are:
Fig 1: Structure of AZ
 Chemical formula: C35H44O16
 Molar mass: 720.714 g/mol.
 Colour: Brownish yellow or Yellow-green.
 Physical state: Powder.
 Odour: Characteristic Neem odour (similar to garlic).
 Solubility: Soluble in water is 0.25g/l(25°C), in Methanol 200g/L(25 °C).
 Bulk density: 0.17 g/mL (25°C).
 Melting Point is -174°C[6]
.
 Flammability: Not flammable
 Corrosion characteristics: Non corrosive on packing material.
Some Characteristics of AZ are:
 It shows the properties of good insecticide.

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 It is now known to affect over 200 species of insect, by acting mainly as an antifeedant and
growth disruptor,
 The compound and extracts containing it have been found to have potent and specific effects
against a variety of insect pests. Thus, we can say it is toxic toward insects.
 AZ is biodegradable (it degrades within 100 hours when exposed to light and water)
 It is environmental friendly as it is biodegradable and doesn’t cause any accumulation inside
mammals like synthetic pesticides do.
 It shows very low toxicity to mammals (the LD50 in rats is > 3,540 mg/kg making it
practically non-toxic).
 It affects the insect's reproductive organ, body development and other endocrine events.

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LITERATURE SURVEY
The isolation of AZ of > 99% purity is possible from Neem seeds via extraction, flash
chromatography in combination with HPLC[7]
. A simple procedure was developed for the isolation
of AZ by direct preparative HPLC, using an column and methanol-water (60:40)[1]
.Accurate
quantification of AZ A in insecticidal formulations has been done from complex matrix containing
oils, surfactants and other liminoids by washing increased column life. AZ A separated from AZ B[8]
.
Reversed-phase HPLC has been conveniently used for separation and quantitation. Quantitation
usually done by external standardization which leads to loss of compound that is overcome by using
Anisole as internal standard[9]
. Traditional Neem preparations are as efficient as commercial
preparation tested for most of the insects but when main target insects are whiteflies higher
concentrations of active ingredient are required[10]
.The Pressurized Liquid extraction is more
efficient than classical methods as we get higher extract yields with less solvent consumption and in
shorter period of time[11]
. AZ is separated from crude Neem Oil using solvent precipitation which
eliminates the evaporation of solvent containing AZ Recovery of AZ is more in this case as
evaporation step generally tends to destroy some amount of AZ[12]
.
Supercritical Fluid Extraction (SFE) became trending as wide range of diverse compound can be
extracted by this as it is simple, fast, cheap etc. It is proved to be better when compared with other
classical liquid extraction methods due to numerous advantages such as rapidity, selectivity,
cleanliness, low solvent volumes requirement etc[13]
.In this, Neem oil is extracted from three
methods namely: Cold Pressing, Soxhlet extraction and SC-CO2 extraction and the yield of AZ from
Neem Oil is compared. The concentration of AZ from SC-CO2 extraction was higher compared to
other two[14]
. Ultrasonic assisted Supercritical extraction may increase both extraction rate and
yield[15]
.Neem tree might be source of production of an effective and cheap formulations for control
of Crinipellis and Phytophthora[16]
. In this, we see various chemistry, analytical way of separation
of AZ, biological properties such as biosynthesis, botany etc, insecticidal effects, its role as Natural
Pesticide and other uses[6]
.

9
Following block diagram indicates the methods available in the literature survey to isolate AZ
from Neem Seeds:
Azadirachtin
Separation From
Neem Seed
Kernel
Chromatographic
Methods
Using flash
Chromatography
along with HPLC.
Direct HPLC.
Extraction
Methods
Supercritical
Solvent
Extraction
Solvent
Precipitation
Pressurized
Liquid
Extraction.

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SYSTEM SELECTION
PROCESS SELECTED
The process we choose is “SOLVENT PRECIPITATION” because of the following advantages of
this process against other processes:
 The solvent to be evaporated contains no AZ so thermal degradation of AZ can be avoided.
Separation is carried out under vacuum condition. The temperature selected for this process is
less than 50o
C
 It gives better recovery compared to other process (nearly around 70%) of upto 80%.
 The process is carried out at ambient temperature so it doesn’t require any external heating.
The operating cost is reduced to a certain extent.
 This Solvent Precipitation method is better than other methods of isolation of AZ.
The chromatography techniques cannot be industrially used as they require very large
columns that may not be economical.
And other extraction techniques have the following disadvantages:
Supercritical Fluid Extraction Pressurized Liquid Extraction
Operated under high pressure. High pressure increases cost.
Expensive. Temperature also high resulting degradation of Az.
Complete recovery not possible. Vaporization of Extractant occurs.

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CHOICE OF SOLVENT
Solvent we choose for this process are “Methanol” and “Hexane”. At initial stages we use Methanol
because:
 Methanol has a very high affinity to AZ. The solubility of AZ in methanol is 200g/L (25 °C).
 The cost of Methanol is less. This makes the process economical.
 It can be easily recovered. It has a less boiling point (64o
C).
Similarly, Hexane has following advantages:
 AZ is completely insoluble with Hexane. So it gives proper separation. If hexane is added to
solution containing AZ it gives precipitate containing AZ. Thus, this precipitate can be easily
separated by filtration.
 It is quite inexpensive.
 It also easily recoverable substance. It has low boiling point (68o
C).

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PROCESS FLOW DIAGRAM AND BLOK DIAGRAM
Fig 2: Process Flow Diagram of Process
Various unit operations involved in the process are:
1. Pretreatment:
This includes size reductions operations, crushing and milling, in which the Neem seed
Kernels are first crushed using a crusher and then it is further reduced to 100µm size using a
Ball Mill.
2. Solvent Extraction:
In this, Methanol is added with the fine sized Neem Seeds Powder and stirred for proper
mixing. This gives a Methanolic Extract and Sludge. All the Limonoids are soluble in
Methanol as it is a polar solvent and Limonoids have an affinity to polar solvents. The Sludge
contains the oil and all insoluble solids. Here it is assumed that Methanolic Extract contains
negligible amount of oil.

13
3. Vacuum Distillation-I:
The Limonoids contained in the Methanolic extract can be separated from Methanol in this
step. Here the extract is subjected to Vacuum Distillation to maintain low temperature as the
AZ which is to be separated thermally degrades at high temperatures giving lower yield. The
temperature is kept upto 64o
C. This step is necessary as if hexane is added with extract
containing Methanol the AZ sticks to Methanol and it will be difficult to separate AZ. The
Methanol can be recovered easily from this step and reused.
4. Precipitator:
The Methanol free extract goes to Precipitator where Hexane is added. This solvent is added
as AZ is completely insoluble in Hexane so we get a precipitate cake containing AZ. The
content of the precipitator is subjected to filtration where the precipitate and the waste
solution can be separated.
5. Filtration:
Here the precipitate and the waste solution can be separated easily. The cake separated is
again subjected to Hexane washing for more recovery of AZ. The waste solution containing
hexane is sent to Vacuum Distillation- II from where Hexane can be recovered and reused.
6. Oil Extraction:
The sludge from solvent extraction step is sent to the filtration unit where any methanol
present can be filtered and sent back to Vacuum Distillation-I. The product obtained is dried
and then sent to oil extraction process. This sludge contains oil and all the insoluble solids
present. In this step, hexane is also added and the mixture is mixed. This gives out sludge
containing insoluble that exits the system with traces of oil and hexane. The product
containing solvent and hexane goes to next stage.
7. Vacuum Distillation –II:
In this process, separation of hexane and oil occurs. In this, the solution from filtration step is
also. The distillation column is subjected to 68o
C under vacuum so separation of hexane
from oil occurs. Hexane comes out in the form of distillate and oil as bottom product. Thus,
hexane can be recovered from this process and the oil obtained as bottom can be directly sold
in market that can be used for various purposes.

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BLOCK DIAGRAM:
Fig3: Block Diagram of the Process

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THERMODYNAMIC FEASIBILITY
 BASIS: 10 Kg of AZ as product.
The Percent Recovery for AZ is reported to be 80%[12]
. Therefore, the amount of AZ in
Methanol extraction unit can be estimated as follows:
% Recovery = Concentration of AZ in Methanol
(in terms of Concentration) Concentration of AZ in Feed
0.80 = (Amount of Az/1500)
(10/2500)
Amount of AZ in Methanol = 4.8 Kg.
 We know there is a solid liquid equilibrium in this case. So for this extraction we have the
equilibrium reaction:
 Insoluble Solid+Az+Methanol [Az+Methanol]+Insoluble Solid
 We know activity(effective concentration) ai = γ [C]/[CƟ
].
Usually, [CƟ
] is taken 1 as it at standard state.
 Consider a general equilibrium reaction,
aA+bB cC+dD
 For this, equilibrium constant, is given by K = ∏i (ai)vi
.
In practical terms, each activity is replaced by the product of a concentration and an activity
coefficient. So equilibrium constant becomes:
K= [C]c[D]d γc γd
[A]a[B]b γaγb
 In practice, equilibrium constants are determined in such a way that the ratio of activity
coefficient is constant and can be ignored. Also activity of pure solvents and solids are unity.
So, K= [C]c[D]d
[A]a[B]b
 Applying this for our case,
Equilibrium Constant, K = [AZ] Methanol
[AZ] Solid
= 4.8

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 We know,
Δ G = -RT ln K.
 We know,
R = 8.314 J/mol K.
T = 298 K.
Δ G = - 8.314* 298* ln (4.8)
= -3886.359 J/mol
 As ΔG is “Negative” we can say our Physical transformation is Feasible.

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QUANTIFICATION
BASIS: 10 Kg of AZ as product
Fig 4: Quantified Block Diagram of Process
Sr. No. OPERATION INPUT OUTPUT
1. Pre treatment
(Crushing and
Milling)
2500 Kg Neem Seed
Kernels.(AZ content is 0.4% in
Neem Seeds)
2500 Kg Powder.
2. Solvent Extraction 2500 Kg of Neem Seed Powder
and 1500Kg Methanol (AZ to
Methanol Ratio is 1:5)
1560Kg of Methanol
Extract and 2440Kg of
Sludge
3. Vacuum Distillation 1560 Kg of Methanol Extract
(1500kg Methanol, 10Kg AZ
and 50kg other Limonoids) at
64°C.
1200Kg of Methanol for
recovery and 360
Kg≈300Kg of Product(AZ
and other Limonoids)

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4. Precipitator 300 Kg of Product(AZ and
other Limonoids) and 900 Kg of
Hexane (1:3)
1200 Kg of Product
containing AZ, Limonoids
and Hexane.
5. Filtration 1200 Kg of Product containing
AZ, Limonoids and Hexane.
10Kg of AZ, 50 Kg of
Limonoids and rest oil sent
to Vacuum Distillation.
6. Oil Extraction Sludge from Solvent Extraction
(2440Kg) and 5000 Kg of
Hexane.
1440 Kg of Insoluble solids
and ≈ 6000Kg of remaining
product.
7. Vacuum Distillation 6000Kg of remaining product
of previous operation vacuum
distilled at nearly 68°C and part
of oil sent from filtration
process.
1000 kg of oil and 5500 kg
of Hexane.
Overall Material Balance:
Neem Seed (2500 Kg) 10 Kg of AZ+ 50 Kg Limonoids + 1420 kg of Insoluble
+ 1000Kg of Oil Solids

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MATERIAL BALANCE
SECTION 1:
OPERATION INPUT OUTPUT
Pre treatment 2500 Kg Neem Seed Kernels. 2500Kg Powder.
SECTION 2:
Solvent Extraction 2500 Kg of Neem Seed
Powder and 1500Kg
Methanol
1560Kg of Methanol
Extract and 2440Kg of
Sludge
SECTION 3:
Vacuum
Distillation
1560 Kg of
Methanol
Extract at
64°C.
1200Kg of Methanol for
recovery and 360 Kg≈300Kg of
Product(Az and other
Limonoids)

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SECTION 4:
SECTION 5:
Filtration 1200 Kg of Product
containing Az,
Limonoids and
Hexane.
10Kg of Az, 50 Kg of
Limonoids and rest oil sent
to Vacuum Distillation.
SECTION 6:
Precipitator 300 Kg of
Product(Az and other
Limonoids) and 900
Kg of Hexane (1:3)
1200 Kg of
Product containing
Az, Limonoids
and Hexane.
Oil Extraction Sludge from
Solvent Extraction
(2440Kg) and 5000
Kg of Hexane.
1440 Kg of
Insoluble solids and
≈6000Kg of
remaining product.

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SECTION 7:
Vacuum
Distillation
6000Kg of remaining
product of previous
operation vacuum
distilled at nearly 68°C
and part of oil sent from
filtration process.
1000 kg of
oil and
5500 kg of
Hexane.

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ENERGY BALANCE
1. HEAT ENERGY BALANCE:
Vacuum Distillation-I:
Cp extract = ∑xi*Cp
= 0.9615*2450+0.0385*2359.42
= 2446.51 J/kg K
Energy Balance equation states,
Heat required Q = mCpΔT + mλ
= 1560Kg*2446.51J/Kg k*(337-298)K+ 1200*1126.72*1000 J/Kg
= 1500909.69 KJ
Q = mλ
So,
150197.73 = m*2257.92,
m = 664.73 Kg
Steam required having 70 % efficiency will be 949.6 Kg
So, to raise the temperature, we require 949.6 Kg of Steam
Vacuum Distillation-II:
Component Mole
Fraction
Cp
(J/Kg K)
Density
(Kg/m3)
Methanol 0.9615 2450 792
Limonoids 0.0385 2359.42 700

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Cp extract = ∑xi*Cp
= 0.833*2260+0.167*2053
= 2225.431 J/kg K
Energy Balance equation states,
Sensible heat required Q = mCpΔT + mλ
= 2440Kg*2225.431J/kg k* (341-298)k+ 4500Kg*2481.1*1000 J/Kg
= 11398442.12 KJ
Q = mλ
So, 11398442.12 = m*2257.92
m = 5048.2 Kg
Steam required with 70 % efficiency will be 7211.72 Kg
Component Mole
Fraction
Cp
(J/Kg K)
Density
(Kg/m3)
Hexane 0.833 2260 655
Oil 0.167 2053 919

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2. ELECTRICAL ENERGY BALANCE:
Pre-treatment Section:
For Crusher,
Von Rittinger for d < 0.05 mm
W = Cr (1/ De – 1/Da),
Where,
W = Grinding Work in kJ/kg,
c as grinding coefficient,
dA as grain size of the source material and dE as grain size of the ground material.
Cr= Grinding Coefficient = 0.5* Cb (dBL) ½
with the limits of Bond's range: lower dBL = 0.05 mm.
Assuming Cb = 1 and De = 0.001mm Da =10 mm
C = 0.5* (0.05) ½ = 0.11
W = 0.11(1/0.001 – 1/10)
= 109.99 KJ/Kg
= 26.25 Kcal/Kg
= 122.01 KWh
For Ball Mill,
E=10×Wi( 1/√P80 − 1/√F80 )
where:
E is the specific energy consumption, kWh/tonne;
Wi is the work index,
P80 is the mill circuit product size in micrometers
F80 is the mill circuit feed size in micrometers.
∴ E = 10* 7*(1/ √100 − 1 /√1000)
= 4.786 KWh/Tonne

25
In this case, 2.5 tonne feed is fed,
So power requirement P = 11.97 KWh
Extraction of AZ:
Density of Suspension or mixture = Fraction of solid*Density of Solid+ Fraction of Liquid *
Density of Liquid
= 2500/4000*700+ 1500/4000*792
= 734.5 Kg/m3
Volume of Tank = (Mass of Solid + Mass of liquid + Mass of Void space)/ρmixt
= (2500+1500+500)/734.5
= 4500/734.5 = 6.127 m3
Also we know, V=∏/4*D2*H
Usually H/D=1.2, so H=1.2 D
6.127 = ∏/4*D2
*1.2 D
D3
= 6.5
D = 1.86 m
Taking 30% Excess Diameter, we get DT= 2.43 m
Diameter of Impeller = 1/3 DT = 0.809 m
And
We have Power No = P/ρsN3
D5
P = NP*ρsN3
D5
= 6*734.5*(120/60)3
*.8095
= 212.21KW
So Power required in rotating impeller operated for 3 hrs in this section is 36.65 KWh

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Extraction of Oil:
Density of Suspension or mixture = Fraction of solid*Density of Solid+ Fraction of Liquid *
Density of Liquid+ Fraction of oil*Density of oil
= 1440/7440*1500+ 5000/7440*792+1000/7440*655
= 910.62 Kg/m3
Volume of Tank = (Mass of Solid + Mass of liquid + Mass of Void space)/ρmixt
= (2440+5000+550)/ 910.62
= 8000/ 910.62
= 8.785 m3
Also we know, V=∏/4*D2
*H
= ∏/4*D2
*1.2 D
D3
= 9.321
D = 2.104m
Taking 30% Excess Diameter, we get DT = 2.104m
Diameter of Impeller = 1/3 DT = 0.701 m
And
We have Power No = P/ρsN3
D5
P= NP*ρsN3
D5
= 6* 910.62*(120/60)3
*0.7015
= 7.4 KW
So Power required in rotating impeller operated for 6 hrs in this section is 44.4 KWh

27
So, we can conclude the total energy requirement as:
S. NO EQUIPMENTS HEAT ENERGY
(kJ)
1 Vacuum Distillation-I 150197.73
2 Vacuum Distillation-II 244657.17
S.NO EQUIPMENTS TIME
(h)
ELECTRICAL
ENERGY(kWh)
1 (a) Crushing 3 122.01
1 (b) Milling 3 157.5
2 AZ Extraction 4 10555757.1
3 Oil Extraction 6 9624569.418

28
KINETICS
In Solvent extraction part we have :
Insoluble Solid+Az+Methanol→ [Az+Methanol]+Insoluble Solid. Time required for extraction will
be 40 min as seen from given data. The time and concentration relation of Methanol is given as:
Sr.
No
Time(min) Concentration
Ca(mol/l)
-ln (Ca/Cao) 1/Ca
1. 0 0 0 -
2. 10 5.8 0.8947 0.222222
3. 20 13.01 1.2 0.124844
4. 30 16.55 1.43 0.063291
5. 40 24.7549 1.71 0.040404
6. 50 24.752 1.704 0.040396
7. 60 22.752 1.704 0.040396
Using Integral Method of Analysis, if we assume our equation is first or second order
respectively and plot graphs we get:
 By plotting 1/Ca vs t we get a straight line, so we can say the assumed order is correct and the
order of reaction is 2nd
order.
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
2
0 50 100
-lnCa/Cao
t
Series1
0
0.05
0.1
0.15
0.2
0.25
0 20 40
1/Ca
t
Series1

29
i.e, dCa/dt = kCa 2
So we get,
K= slope of graph
= (0.22-.125)/(20-10)
= 0.0095 L·mol−1
·min−1.
= 0.00016 L·mol−1
·sec−1.
Rate of reaction is :
dCa/dt = kCa 2
= 0.00016* 24.75 2
= 0.09801 mol/Ls
DESIGN:
This includes designing of:
 Extractors
 AZ Extractor
 Oil Extractor
 Batch Distillation Equipment
For, AZ EXTRACTOR,
True Density of Neem Seeds = Fraction of Limonoids * Density of Limonoids
+ Fraction of solid*Density of Solid
= 60/2500*700+ 2440/2500*1500
= 1408.8 Kg/m3
V Solid = Mass/ Bulk Density of Solid = 2500/1408.8 =1.775 m3
Total volume of Solid = 30% V Solid + V Solid = 2.5 m3
Bulk Density = Mass of Solid/Total Volume
= 2500/ 2.95 = 847.45
V Methanol = 1500/792 = 1.894 m3

30
V Solid = Mass/ Bulk Density of Solid = 2500/847.45 = 2.95 m3
Volume of Tank = V Methanol + V Solid = 1.894+ 2.95= 4.844 m3
V = 1.3 V T = 6.3 m3
Also we know, V=∏/4*D2
*H
6.3 = ∏/4*D2
*1.2 D
D3
= 6.68
DT = 1.9 m
And Height H = 1.2 DT
H = 1.2*1.9 = 2.28 m
1. AGITATOR DESIGN:
DT = 1.9 m
Diameter of Impeller Da= 1/3 DT = 0.63 m
Length L = Da/4 =0.801/4 = 0.159 m
Width W = Da/5 =0.801/5 = 0.127 m
Impeller Distance above vessel = Da=0.63 m
Distance between to Impeller = Da = 0.63 m
Number of Impeller = 2
Number of Blades = 4
Velocity of Agitator ω = v/r
ω = 120 rpm =2 rps, ra = 0.63/2 = 0.315 m
v = ω*r = 0.63 m/s

31
Similarly, calculations for other can be done and summed up as:
PARAMETER AZ EXTRACTOR OIL EXTRACTOR
Type of Impeller Flat Blade Propeller Flat Blade Propeller
Agitator diameter (Da) 0.63m 0.773
Angular Velocity (ω) 120 rpm 120 rpm
Impeller Height above vessel
floor (E)
0.63 m 0.773 m
Length of Impeller (L) 0.16 m 0.193 m
Width of Impeller (W) 0.13m 0.155 m
Distance Between Impeller 0.63 m 0.773 m
2. SHELL DESIGN:
Operating Pressure (Po) = (ρmix × g × h) + 101325
Density of mixture (ρmix ) = 1177.5 kg/m3
Height (h) = 2.28 m
Po = 2.28 x 1177.5 x 9.81 + 101325 = 127661.907 Pa
And Design Pressure = 1.3 P
= 165960.5 Pa
Thickness = (Pdi /2 fj- P) + C
Permissible Stress of Stainless Steel (f) = 25 × 106
Pa
Corrosion Allowance (Cc) = 2 × 10-3
m
Diameter of reactor (di) = 1.85 m
Joint Efficiency (Ej) = 0.85
ts = [(165960.5 × 1.91)/[(2 x 25 × 106
× 0.85) - 165960.5)]
= 7.44 × 10-3
m ≈ 8.00 mm
Baffle Spacing = 1/5 Ds = [1.91+(8 × 10-3
)]/5 = 0.402 m

32
3. HEAD DESIGN
 Crown Radius Rc = Di = 1.9m
Knuckle Radius Rl = 0.06*Di = 0.06*1.9m
= 0.115 m
th = P* Rc *W/(2fJ)
W = ¼*(3+√(Rc/R))
= 1.77 m
P = 2.28 x 1177.5 x 9.81 + 101325 = 127661.907 Pa
= 127 KPa
Considering Torispherical Head,
Design Pressure = 1.1 P
= 140 KPa
 So, th = 140*1.9*1.77/(2*68947.57 *0.85)
= 4.73 mm ≈ 6 mm
 Diameter of Top Head (DTH) = 1.25 D
=1.25 × 1.9 = 2.375 m
 Diameter of Bottom Head (DBH) = 1.1 DTH
= 1.1 × 2.375 = 2.6125 m
Outer Diameter (D0) = Di + 2t = 1.922 m.
Thus, we can design an extractor with cross sectional view as given below:

33
Thus, we can similarly design an oil extractor and the design can be summarized as:.
PARAMETER AZ EXTRACTOR OIL EXTRACTOR
Total Volume(V) 6 m3
9 m3
Inside diameter (Di) 2 m 2.3 m
Height(H) 2.3m 2.8 m
Diameter of top head (DTH ) 2.3 m 3 m
Diameter of bottom head (DBH) 2.55 m 3.2 m
Operating Pressure (Po) 142216.51 Pa 126159.24 Pa
Shell Thickness(ts) 8 mm 8 mm
Thickness of top head(Th) 6 mm 8 mm
Outside diameter (Do) 2 m 2.5 m
Baffle Spacing 0.402 m 0.462 m

34
COST ESTIMATION:
AZ EXTRACTOR
FIXED CAPITAL COST:
A. Cost of Shell
Inner Diameter of the shell (Di) = 1.9 m
Thickness of the shell (t) = 8 mm
Outer Diameter of the shell (Do) = Di + 2t = 1.9 + (2×6*10⁻³) = 1.916 m
Height of the shell (H) = 2.28 m
Volume of the shell (V) = (π/4 × H) × (Do2
– Di2
) = (π/4 × 2.28) × (1.9162
– 1.92
)
= 0.1093 m3
Material of Construction – Stainless Steel.
Density of Stainless Steel (ρ) = 8000 kg / m3
Mass of shell = Volume of the shell × Density of Stainless Steel
= 0.1093 × 8000 = 874.668kg
Cost of shell = Mass of shell × Cost of Stainless Steel
= 874.668 × 280 = Rs. 244906.94
Cost of Fabrication of shell = Mass of shell × Fabrication Charge
= 874.668 × 80 = Rs. 69973.44
Total Cost of shell = Cost of shell + Cost of Fabrication of shell
= 244906.94 + 69973.44
= Rs. 314880.38
B. Cost of Agitator:
Volume of Agitator (V) = L × B × t
Length of Agitator (L) = 0.159m
Width of Agitator (B) = 0.127 m
Thickness of the Agitator (t) = 0.012 m
Volume of Agitator (V) = 0.159 × 0.127 × 0.012
= 0.000243 m3
Mass of Agitator = Volume of Agitator × Density of Stainless Steel

35
= 0.000243 × 8000 = 1.94kg
so total mass = 4×1.94 = 7.75 kg
Cost of Agitator = 7.75 × 280 = Rs. 2170
Cost of Fabrication = 7.75× 80 = Rs. 620
Total cost of Agitator = Cost of Agitator + Cost of Fabrication
= Rs. (2170+620) = Rs. 2790
C. Cost of Top Head
• Diameter of Top Head (DTH)= 1.25 D = 1.25 × 1.9 = 2.375 m
• Thickness of Top Head (t)= 6 mm = 0.006m
• Volume of Top Head = (π/4 × DTH
2
) × t = (π/4 × 2.3752
) × 0.006 = 0.0266m3
• Mass of Top Head = Volume of Top Head × Density of Stainless Steel
= 0.0266 × 8000 = 212.65 Kg
• Cost of Top Head = Mass of Top Head × Cost of Stainless Steel
= 212.65× 280 = Rs.59541.03
• Cost of Fabrication of Top Head = Mass of Top Head × Fabrication Charge
= 212.65 × 80 = Rs. 17012.03
• Total Cost of Top Head = Cost of Top Head + Cost of Fabrication of Top Head
= Rs.(59541.03+ 17012.03) =Rs. 76553.03
D. Cost of Bottom Head
• Diameter of Bottom Head (DBH)= 2.62m
• Thickness of Bottom Head (t)= 6 mm = 0.006 m
• Volume of Bottom Head = (π/4 × DBH
2
) × t
= (π/4 × 2.622
) × 0.006= 0.0323m3
• Mass of Bottom Head = Volume of Bottom Head × Density of Stainless Steel
= 0.0323 × 8000 = 258.78 Kg
• Cost of Bottom Head = Mass of Bottom Head × Cost of Stainless Steel
= 258.78 × 280 = Rs. 72458.4
• Cost of Fabrication of Bottom Head = Mass of Bottom Head × Fabrication Charge
= 258.78 × 80 = Rs. 20702.4
• Total Cost of Bottom Head = Cost of Bottom Head + Cost of Fabrication of Bottom Head
= Rs.(72458.4 + 20702.4) = Rs. 93160.8

36
E. Cost of Baffles
• Diameter of the Baffle (d) = 0.25 Ds = .25 × 1.85 m = 0.46 m
• Thickness of the Baffle (t) = 10 mm = 0.01m
• Volume of the Shaft (V) = (π/4) × d2
× t = (π/4) × 0.462
× 0.01
= 0.0016 m3
• Mass of the 4 Baffle = Volume of the Baffle × Density of Stainless Steel × 4 =
0.015 × 8000 × 4 = 51.2 Kg
• Cost of the Baffle = Mass of the Baffle × Cost of Stainless Steel
= 51.2 × 280 = Rs.14336
• Cost of Fabrication of Shaft = Mass of Baffle × Fabrication Charge
= 51.2 × 80 = Rs. 4096
• Total Cost of Baffle = Cost of the Baffle + Cost of Fabrication of Baffle
• = Rs. 18432
TABLE FOR TOTAL EQUIPMENT COST OF AZ-EXTRACTOR
S.NO PARTICULARS COST (Rs)
1 Agitator 2790
2 Shell 314880.38
3 Top Head 76553.03
4 Bottom Head 93160.8
5 Shaft 27046.8
6 Baffles 18432
7 Pump 120000
Total 752863.01

37
TOTAL EQUIPMENT COSTS
S.NO EQUIPMENTS COST (Rs)
1 Pretreatment Equipments 400000
2 AZ- Extractor 800000
3 Oil- Extractor 1700000
4 Distillation Column-I 700000
5 Distillation Column-II 1200000
6 Filters 360000
7 Dryer and Precipitator 360000
Total 5520000
TOTAL FIXED CAPITAL COSTS
The cost of fixed capitals is taken as certain % of Total Equipment Cost (TEC) and the total fixed
capital cost can be calculated as below:
SR.NO FIXED CAPITAL % of TEC COST (Rs)
1 Total Equipment Costing 100 5520000
2 Purchased Equipment Installation cost 40 2760000
3 Building cost Land purchase and construction 58 3477600
4 Construction expenses 20 1104000
5 Piping cost (Installed) 8 441600
6 Instrumentation & Control cost (Installed) 15 828000
Total 14131200

38
WORKING CAPITAL
COST OF RAW MATERIAL:
It is taken as:
COMPONENTS PRICE
(Rs/Kg)
AMOUNT TOTAL PRICE (Rs)
NEEM SEEDS 5 2500 Kg 12500
METHANOL 22 200 Kg 4400
HEXANE 55 200 Kg 11000
Total Rs. 27900
ELECTRICITY COST
It can be calculated by multiplying standard cost (Rs.) for 1 unit to obtained units in KWh
EQUIPMENTS ELECTRICAL
ENERGY
REQUIREMENT
(KW)
TIME
REQUIRED
(hr)
RATE
(Rs.)
COST
(Rs.)
Grinder 122.01 1 8 976.08
Ball Mill 315 0.5 8 1260
AZ Extractor 6.2 2 8 99.2
Pump for AZ Extractor and
Distillation Column-1
7.5 0.5 8 30
Oil Extractor 7.4 4 8 236.8
Pump for Oil Extractor and
Distillation Column-2
10 1 8 80
Total Rs. 2388.88

39
TOTAL WORKING CAPITAL COSTS
The working capital costs are calculated as certain percentage of Raw Material costs and labour
costs as shown in table below:
WORKING CAPITAL % of RM COST (Rs)
Raw Materials 100 % RM 27900
Lab & Other Service Cost 1% RM 279
Utilities 20% RM 5580
Electricity - 2388.88
Operating Labor &
Supervision Cost
- 6666.67
Plant Overhead Cost 50% Labor Cost 3333.33
Total Rs. 41125.88
PAYBACK PERIOD
The payback period (PBP) is the amount of time that is expected before an investment will be
returned in the form of income. It is usually measured as the time from the start of production to
recovery of capital investment.
In this plant setup, the Total Fixed Cost = Rs. 14131200
Total Variable Cost for one month = 41125.88 × 30 = Rs. 1233776.4
Price of AZ = Rs 6000/Kg
 Payback Period = Total Fixed Cost / Net Sales
= 14131200 / 5662236
= 2.1 years
So, for this plant the payback period is 2.1 years i.e, it requires 2.1 years to recover the capital
investment that was invested at the time of plant setup.

40
TURNOVER RATIO
The fixed-asset turnover ratio is, in general, used by analysts to measure operating performance .It is
a ratio of net sales to fixed assets. This ratio specifically measures how a company is able to generate
net sales from fixed-asset investments
TURNOVER RATIO = Net Sales / Total Fixed Cost
= 19980000 / 14131200
= 1.42

41
UTILITY DIAGRAM
UITLITY DIAGRAM

42
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