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Project Report on

Production of Cinnamic Aldehyde

Submitted in partial fulfilment of the requirements of the degree of

Bachelor of Technology

In

Chemical Engineering

By

Neetish Kumar (146245)

Anshul Choubey (146204)

Jahnawi Priya (146143)

Shubham Manhar(146236)

Under the Guidance of

Dr. Shirish Hari Sonawane

Department Of Chemical Engineering

NATIONAL INSTITUTE OF TECHNOLOGY WARANGAL

2017

I
APPROVAL SHEET

This Project Work entitled “Production of Cinnamic Aldehyde” by Neetish Kumar (146245),
Anshul Choubey (146204) , Jahnawi Priya (146143) and Shubham Manhar (146236) is approved
for the degree of BACHELOR OF TECHNOLOGY in CHEMICAL ENGINEERING.
Examiners

________________________

________________________

________________________

Supervisor (s)

________________________

________________________

________________________

Chairman

________________________

Date :____________

Place :____________

II
Department of Chemical Engineering

National Institute Of Technology

Warangal-506004

DECLARATION
We declare that this written submission represents our ideas in our own words and where others ideas
or words have been included. We have adequately cited and referenced the original sources. We also
declare that we have adhered to all principles of academic honesty and integrity and have not
misrepresented or fabricated or falsified any idea/ data/ fact/ source in my submission. We understand
that any violation of the above will be cause for disciplinary action by the Institute and can also evoke
penal action from the sources which have thus not been properly cited or from whom proper
permission has not been taken when needed.

Neetish Kumar (146245)

Anshul Choubey (146204)

Jahnawi Priya (146143)

Shubham Manhar(146236)

Date: __________

III
CERTIFICATE

This is to certify that the project work entitled “Production Of Cinnamic Aldehyde” is a bonafide
record of work carried out by “Mr Neetish Kumar (146245), Ms. Jahnawi priya (146143) and Mr.
Anshul Choubey(146204) and Mr. Shubham Manhar(146236)”, submitted to the faculty of
“Department Of Chemical Engineering”, in partial fulfillment of the requirements for the award of the
degree of Bachelor of Technology in “Chemical Engineering” at National Institute of Technology,
Warangal during the academic year 2017-18.

Dr. A Sarath Babu Dr. Shrish Sonawane


Head of the Department Assistant Professor
Department of Chemical Engineering Department of Chemical Engineering
NIT Warangal NIT Warangal

IV
ACKNOWLEDGEMENT

Foremost, we would like to express our sincere gratitude to our advisor Dr. Shirish Hari S. for the
continuous support of our project work, for his patience, motivation, enthusiasm, and immense
knowledge. His guidance helped us in all the time of research and drafting of this work. We could
not have imagined having a better advisor and mentor for our project.

We take this opportunity to express gratitude to all of the Department faculty members and our
Head of the Department, Dr. Sarath Babu Anne for their help and support. We thank our parents for
the unceasing encouragement, support and attention.

We also place on record, our sense of gratitude to one and all who directly or indirectly, have lent
their hand in this venture.

V
CONTENTS

S.No. Title Page No.

Approval sheet ii
Declaration iii
Certificate iv
Contents vi
List of tables vii
List of figures viii

1. Introduction 9

2. Market Analysis 10

3. Properties & Applications of Cinnamic aldehyde 14

4. Literature review 17

5. Methods of production 20

6. Flow sheet 21

7. Process Description 22

8. Material Balance 24

9. Energy Balance

10. Design of equipment

11. Cost estimation

12. Profitability analysis

13 Plant location and layout

14 Safety and environmental issues

15 References

VI
LIST OF TABLES

Table 1 Physical properties of Cinnamic aldehyde 14


Table 2 Molecular weights and boiling points of the compounds 24
Table 3 Material balance around the reactor 26
Table 4 Material balance around the screening 27
Table 5 Material balance around the separator 28
Table 6 Material balance around the membrane separator 29
Table 7 Material balance around the distillation column 1 31
Table 8 Material balance around the distillation column 2 32
Table 9 Heat capacity constant of compounds
Table 10 Enthalpy of feed to the reactor
Table 11 Enthalpy of product from reactor
Table 12 Overall energy balance around reactor
Table 13 Enthalpy of feed to the separator
Table 14 Enthalpy of product stream to screening
Table 15 Overall energy balance around separator
Table 16 Enthalpy of top product from distillation column 1
Table 17 Enthalpy of bottom product from distillation column 1
Table 18 Overall energy balance around distillation column 1
Table 19 Enthalpy of top product from distillation column 2
Table 20 Enthalpy of bottom product from distillation column 2
Table 21 Overall energy balance around distillation column 2
Table 22 Antoine constants data of compounds in distillation column 1
Table 23 Equilibrium data of compounds in distillation column 1
Table 24 Composition of feed, top and bottom streams in distillation column 1
Table 25 Relative volatility of compounds in distillation column 1
Table 26 Composition of heavy and light key in distillation column 1
Table 27 Calculation for minimum reflux in distillation column 1
Table 28 Antoine constants data of compounds in distillation column 2
Table 29 Composition of feed, top and bottom streams in distillation column 2
Table 30 Equilibrium data of compounds in distillation column 2
Table 31 Relative volatility of compounds in distillation column 2
Table 32 Composition of heavy and light key in distillation column 2
Table 33 Calculation for minimum reflux in distillation column 2
Table 34 Equipment cost estimation parameters
Table 35 Total capital investment evaluation
Table 36 Total product cost evaluation
Table 37 Profitability analysis summary

VII
LIST OF FIGURES

Figure 1 Cinnamic aldehyde structure 9


Figure 2 Global share of perfume and flavouring industry 10
Figure 3 Comparative study of cinnamic aldehyde market 11
Figure 4 Trade during the month of September 2014 11
Figure 5 Different countries to which cinnamic aldehyde is exported 12
Figure 6 Production of benzaldehyde in India and market value in rupees/kg 13
Figure 7 Oxidation reaction of cinnamyl alcohol 18
Figure 8 Material balance around the reactor 25
Figure 9 Material balance around the screening 26
Figure 10 Material balance around the seperator 27
Figure 11 Material balance around the membrane seperator 28
Figure 12 Material balance around the distillation column 1 30
Figure 13 Material balance around the distillation column 2 32
Figure 14 Energy balance around the reactor
Figure 15 Energy balance around distillation column 1
Figure 16 Energy balance around distillation column 2
Figure 17 Screening design setup
Figure 18 Flash separator design parameter
Figure 19 Plant layout

0
1.Introduction

Perfumes and scented oils have been used since the beginning of human history and its use has been
recorded as far back as the ancient Egyptians and ancient China.

The manufacture of the fragrances has undergone drastic changes in the past quarter century.
Advances in chemistry at this point in time allowed for larger distribution and larger amounts to be
made. Prior to this, perfumes were made in small personal batches at home. The odorous substances
are mainly organic compounds occurring in natural substances. Cinnamic aldehyde is one of such
compound which is used in the perfume industry.

Fig. 1. Cinnamic Aldehyde, C9H8O

The flavour and aroma of cinnamon is due to an essential oil which makes up between 1 and 4% of the
bark of the Cinnamomum zeylanicum tree. This oil contains many different compounds but the most
abundant (65 to 75% of the oil) is cinnamic aldehyde. Cinnamic aldehyde, or phenylprop-2-enal to use
its IUPAC name, is an oily yellow liquid at room temperature.

Cinnamic aldehyde can be made from the steam distillation of the oil of cinnamon bark or through
synthetically which is a much more efficient process. It is mainly used as a flavouring agent or as a
scent for candles. It is non-toxic but can irritate skin if in contact for too long. As with many
components of essential oils cinnamic aldehyde displays antiviral, antibacterial and antifungal
properties. It is also reported to be a good pesticide. These properties support the medicinal and
soothing properties of cinnamon bark. This compound makes up about 10% of the oil and displays
antiseptic and analgesic properties which may also contribute to cinnamon's soothing effect.

Cinnamic aldehyde was isolated from cinnamon essential oil in 1834 by Dumas and Peligot and
synthesized in the laboratory by Chiozza in 1854.

This project deals with the feasibility of industrial production of cinnamic aldehyde from acetaldehyde
and benzaldehyde.

1
2. Market Analysis

The perfume industry in India has come of age. From a cottage industry it has become a full-fledged
industry in the last two decades. The industry is growing at 125 per cent annually. The growth is
attributed to an increase in disposable incomes.

With globalisation, liberalisation and the IT revolution, living standards of the Indians have increased
manifold. The illegal flow of lifestyle products confirms the great demand for these products in India.
The affinity of the Indians for foreign goods also compels the indigenous manufacturers to tie-up with
international brands to tap this segment of people.

The domestic perfume market is estimated to be worth Rs 300 crores and is growing at around 125 per
cent annually. The forecast is that it may grow at a rate of 200 per cent in the coming years, with fast
changing consumer behaviour and habits. Geneva-based International Fragrance Association has
estimated that the global perfume market is worth $ 10 billion, out of which the mass market has a 70
per cent share.

Fig.2. Global share of perfume industry

Cinnamic Aldehyde is one such compound which is exported to the European nations from India. The
cinnamon flavour or perfume is of high demand in the other parts of the world and India and China are
the only places where is found in abundant.

The figure shows the export quantity in the years 2011 to 2017. It can be observed that the amount is
double folded in the year 2010-2017. So its production if optimized through a different method can be
profitable to the GDP as well.

The cost of perfume grade (purity > 99.9%) cinnamic aldehyde per kg has increased from around
Rs. 130 in 2001 to Rs. 400 in 2017.

2
Cinnamic Aldehyde

quantity value(million
(tonnes) rupees)
2106.927

1029.89
757.722
300.63
108.69 143.27

2014-2015 2015-2016 2016-2017

Fig.3. Production of Cinnamic Aldehyde in India and value in Rs/kg

With this amount of export data available it can be inferred that There is a lot of scope of increase in
the production of the final perfume in India itself. The production costs if minimized will result in
boosting the profit margins for the exports.

Recent Studies (2015 & 2016)

From the data available from Jawaharlal Nehru Port Trust, Mumbai, cinnamic aldehyde is exported to
cities like Hamburg, New York, Barcelona, Hong Kong, Singapore and Houston. Among these places
Barcelona has the highest stake and takes up 70% of the quantity.
In the first quarter of 2015 itself, 72.03 tonnes of cinnamic aldehyde was exported from this port
having a worth of 11.5 million rupees.

Fig.4. Total quantity of exports by loading port in India (USD)

3
Export data showing the places from where the compound is exported. Nhava Sheva Sea is the
port in Mumbai.

Fig.5. Pie chart showing the different countries to which cinnamic aldehyde is exported
from India

Raw Materials

The general method of production is from the cassia and cinnamon barks which requires these plants.
Since India has an abundant of these it is able to export the cinnamic aldehyde to other countries.
For synthetic production acetaldehyde and benzaldehyde are required. India produces enough amounts
of these compounds. Benzaldehyde is also exported in large amounts from India. So implementing
this method would be feasible as both the raw material compounds are availbale at low costs.

Benzaldehyde

Quantity(tonnes) Valve (Million rupees)


5755.346
5227.78 5202.638

978.7 609.42 554.98

2014-2015 2015-2016 2016-2017

Fig.6. Chart shows the production of benzaldehyde in India and the value in Rs/kg

4
3. Properties & Applications of Cinnamaldehyde
Cinnamaldehyde is a yellow oily liquid only a little stickier than water. It strongly smells like
cinnamon. This compound is the main source of cinnamon oil that can be produced from distillation.
Concentrated cinnamaldehyde can be harmful to skin. The chemical is irritant when is in large doses.

Both aromatic and an aldehyde, cinnamaldehyde has a mono-substituted benzene ring. A conjugated
double bond (alkene) makes geometry of the compound planar. The molecule is in a phenyl group that
is tied to an unsaturated aldehyde. The molecule can also be shown as a derivative of acrolein.

3.1.Physical properties
Table 1. Properties of Cinammic Aldehyde

Properties

Molar mass 132.16 g/mol

Appearance Yellow oil

Odour pungent, cinnamon-like

Density 1.0497 g/mL

Melting point −7.5 °C (18.5 °F; 265.6 K)

Boiling point 248 °C (478 °F; 521 K)

Solubility in water Slightly Soluble

Solubility soluble in ether, chloroform


insoluble in petroleum ether
miscible with alcohol, oils

Refractive index(ND) 1.6195

Vapour pressure 0.0289 mm Hg at 25 deg C

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3.2.Chemical properties

The natural product is trans-cinnamaldehyde. The molecule consists of a phenyl group attached to an
unsaturated aldehyde. Its colour is due to the π → π× transition. It is chemically stable, but
incompatible with strong oxidizing agents and bases.

• Cinnamic aldehyde dissolves plentifully in aqueous bisulphite of ammonia, forming an oily liquid
which afterwards solidifies to a crystalline magma
• It oxidizes in air to form cinnamic acid.

• Cinnamic aldehyde dissolves in oil of vitriol with yellow colour; the addition of water renders the
solution milky, and precipitates cinnamic acid.
• It dissolves in hydrochloric acid, and water separates from the solution.

3.3.Toxicological data

ORAL (LD50):
Acute: 2220 mg/kg [Rat]
1160 mg/kg [Guinea pig].

Potential Health Effects:

• Very hazardous in case of ingestion. Hazardous in case of skin contact (irritant), of eye contact
(irritant), of inhalation.
• The substance is toxic to mucous membranes.
• Repeated or prolonged exposure to the substance can produce target organs damage.

3.4.Application

3.4.1 Flavourant/ perfume

The most obvious application for cinnamic aldehyde is as flavouring in chewing gum, ice cream,
candy, and beverages; use levels range from 9 to 4900 parts per million (ppm) (that is, less than 0.5%).
It is also used in some perfumes of natural, sweet, or fruity scents. Almond, apricot, butterscotch, and
other aromas may partially employ the compound for their pleasant smells. Cinnamic aldehyde can be
used as an adulterant; powdered beechnut husk aromatized with cinnamic aldehyde can be marketed as
powdered cinnamon. For perfume grade 98% purity of cinnamic aldehyde is prepared.

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3.4.2 Agrichemical

Cinnamic aldehyde is also used as a fungicide. Proven effective on over 40 different crops, cinnamic
aldehyde is typically applied to the root systems of plants. Its low toxicity and well-known properties
make it ideal for agriculture. Cinnamic aldehyde is an effective insecticide, and its scent is also known
to repel animals, such as cats and dogs. It has recently been recognized as a very effective insecticide
for mosquito larvae. As little as 29 ppm of cinnamic aldehyde kills half of Aedes aegypti mosquito
larvae in 24 hours.

3.4.3 As an antimicrobial

Another use for cinnamic aldehyde is as an antimicrobial. Researchers from the University of Illinois
at Chicago (who were funded by the Wm. Wrigley Jr. Company) have found that cinnamic aldehyde,
prevented oral bacterial growth by more than 50%. It is especially effective against bacteria living at
the back of the tongue, reducing anaerobic bacteria populations by about 43%.

3.4.4 As an anticancer agent

Recent research documents anticancer activity of cinnamic aldehyde observed in cell culture and
animal models of the disease. Proliferation, invasion, and tumour growth were inhibited in a model of
human melanoma, though only at high doses not achievable through dietary intake.

7
4. Literature Review

Cinnamic aldehyde was isolated from cinnamon essential oil in 1834 by Dumas and Péligot and
synthesized in the laboratory by Chiozza in 1854.Cinnamic aldehyde can be prepared using the
following methods:

4.1Cassia and cinnamon bark essential oils

Cinnamic aldehyde is isolated from the cassia or the cinnamon bark through the fractional distillation.
Commercial cinnamon contains about 2% cinnamaldehyde. The isolation will be accomplished by
steam distillation is employed for isolation. This means that the solid cinnamon is boiled in water, and
then steam condensed and collected. Since cinnamaldehyde is soluble in steam (but not in water), it
will be carried up with the distillate and form a finely distributed emulsion, which will appear milky
upon cooling.

The following conclusions can be made regarding this process:

• This process is a separation technique which cannot be employed on industrial scale. Small
amounts of the product may be derived.
• The purity of the raw materials may vary depending on the type of bark being used.
• Availability of raw materials depends on the cinnamon and cassia plants.
• The yield is relatively low (50 to 60%)

4.2 Acetaldehyde and benzaldehyde

Base catalyzed aldol condensation of benzaldehyde with acetaldehyde can be used to procure the
chemical synthetically. The reaction is as follows

ION EXCH RESIN+PEG


C6H5CHO + CH3CHO C6H5CHCHCHO + H20

The catalyst used is PEG 400 in ion exchange resin. This method has a defined flow sheet involving a
reactor and a distillation column. Fractional distillation is used in such a way that the purity of the
cinnamic aldehyde is above 98%.

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Comments regarding this method are:

• This is the only method which can be implemented on industrial scale.

• The product yield is high as the process is driven by condensation of two compounds to get
cinnamic aldehyde and water
• Aldol condensation is highly efficient as a base is used to catalyse the reaction

4.3 Cinnamyl alcohol

Fig 7. Oxidation reaction of cinnamyl alcohol

Cinnamic aldehyde can also be produced by partial oxidation of cinnamyl alcohol using an
oxidizing agent such as MnO2.

Cinnamyl aldehyde is not readily available, so this process is just a reaction ending up in the
formation of cinnamic aldehyde.
4.4. Industrial processes

4.4.1 Under alkaline conditions, benzaldehyde and acetaldehyde condensation reaction, the mixture
was distilled under reduced pressure to give cinnamic aldehyde. Since benzaldehyde is insoluble in
water, this method belongs to the two-phase reaction, the yield is too low, the yield of less than 60%,
low economic efficiency.

4.4.2 Benzaldehyde and acetaldehyde, KFAl2O3 as catalyst, PEG as phase transfer solution, cinnamic
aldehyde synthesis, yield over 80%.Cinnamaldehyde high yield synthesis of this method, the process
is relatively simple, but the more complex the preparation of the catalyst used, and expensive,
environmental pollution, cumbersome recovery step.

4.4.3 Benzaldehyde and acetaldehyde, in near-critical water cinnamic aldehyde synthesis. This
cinnamic aldehyde synthesis process is simple, relatively small environmental pollution, but the yield

9
is too low, below 50%, and at high temperature and pressure conditions, organic subcritical water
reaction more severe corrosion of equipment, while using this method. The investment is too large.

4.4 Selection of process

For our study, the aldol condensation method is chosen as it is the only one with the prospect of
industrial production. As the purity which can be obtained through this method is sufficient in making
the perfume grade cinnamic aldehyde, this is the best option we have. In summary, the method of the
present invention is easy and raw materials, catalyst separation and recovery is highly efficient, non-
polluting products, environmentally friendly, continuous operation, compared with the normal
process. The positive reaction speed reduces consumption of products and results in stable cinnamic
aldehyde product, high yield more than 80%, and high purity.

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5. Methods of Preparation

It has been found that a high yield (75-85%, based on the benzaldehyde) of cinnamaldehyde can-be
obtained by adding the acetaldehyde gradually to the benzaldehyde. A reversal in the order of addition
or the simultaneous mixing of the reagents results in low yields of the order of 18 and 49%
respectively.

The addition of the acetaldehyde to the benzaldehyde avoids having an excess of acetaldehyde and
thereby minimizes the self-condensation of the acetaldehyde as well as the further condensation of
cinnamaldehyde with acetaldehyde.

Preferably, the reaction is carried out at a room temperature such as 25 C although this reaction
temperature may be varied from 30-35 C. without a substantial loss in yield. Here Polyethylene glycol
in Ion resin is used as catalyst which gives yield upto 80%.

The first configuration solution: Take a PEG-400 2kg I t was added to the deionized water Stir and set
aside. 50kg of strongly basic anion exchange resin has been configured and PEG-400 in aqueous
solution by the addition vessel, used strongly basic anion exchange resin Rohm & Hass Co. (Rohm
and Haas) produced Amber jet 4400 0H, then added benzyl wake 400kg, was stirred for half an hour.
Then 400 kg of acetaldehyde was added dropwise to the reactor for 2 hours. After completion of the
reaction the reaction solution was washed with water, and then screening was done to remove the
resin. The separated resin was washed with Deionized water to charge it again for further use. The
product stream is passed through a separator to separate water and PEG from product. PEG is
separated from water through membrane process. The remaining product stream is sent for fractional
distillation to achieve 98% pure grade of cinnamaldehyde.

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6. FLOWSHEET

Process flow sheet of Cinnamaldehyde production

12
7. Process Description

7.1 REACTOR

REACTION:-
ION EXCH. RESIN+ PEG 400
CH5CHO + CH3CHO C6H5CHCHCHO + H20

CONDITIONS: The reaction is carried out at a room temperature (250C) although this reaction
temperature may be varied from 30-35 0C without too substantial loss in yield. The catalyst used is
PEG in strong anionic ion exchange resin.

RAW MATERIALS: It is not necessary that the benzaldehyde be highly purified. Technical grades
of benzaldehyde containing small amounts of chlorine may be used. The quality of the cinnamic
aldehyde obtained is very good, analysing as high as 99 pure and is suitable for the preparation of
perfumes. The addition of the acetaldehyde to the benzaldehyde minimizes the self-condensation of
the acetaldehyde as well as the further condensation of cinnamaldehyde with acetaldehyde. Thus all
the side reactions are eliminated.

7.2 SCREENING

Sieving is an essential process for any industry and application. Screening is the practice of
taking granulated material and separating it into multiple grades by particle size. This task is
particularly important in the industry where there is a high risk of solid contamination which cannot be
ignored. This contamination can consist of airborne particles, unmixed product or resins which have
formed, all of which can enter during any stage of production. In this process a screen is placed at the
output of the reactor, operating at atmospheric temperature and pressure conditions. Screening is
employed to separate resin from product stream. Product stream is separated from ion resin and sent
for further separation.

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7.3 SEPARATOR

A separation process is a method to achieve any phenomenon that converts a mixture of chemical
substance into two or more distinct product mixtures, which may be referred to as mixture, at least one
of which is enriched in one or more of the mixture's constituents. In some cases, a separation may fully
divide the mixture into its pure constituents. They are often classified according to the particular
differences they use to achieve separation. Usually there is only physical movement and no substantial
chemical modification. In the production process, the filtered stream is sent to a separator tank
operating at atmospheric conditions. A separation tank is used to separate PEG and water from product
stream. Thus the unreacted benzaldehyde, acetaldehyde and newly formed cinnamic aldehyde leave
the separation tank for further operations.

7.4 MEMBRANE SEPERATION

The separation process is purely physical and both fractions (permeate and retentate) can be used.
Membrane separation is employed to the product stream of separator at atmospheric temperature and
pressure conditions, and separate PEG from water. The PEG is separated and can be used in another
batch along with some quantity of fresh PEG.

7.5 DISTILLATION

The unreacted benzaldehyde, acetaldehyde and newly formed cinnamic aldehyde are fed into the
distillation column at atmospheric conditions. The acetaldehyde is removed in the first column as a top
product, and leaves at 350K while the unreacted benzaldehyde can be recovered by fractional
distillation and in the same fractionation cinnamaldehyde is obtained in a state of high purity leaving
behind high boiling by-products at 380K. The chlorine containing impurities are removed in the final
fractionation of the cinnamaldehyde, leaving the reactor from the bottom at 420K. The high boiling
by-product which is recovered after the removal of the unreacted benzaldehyde from the top at 310K.

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8. Material Balances

Basis:
As the annual demand of cinnamic aldehyde is about 3400 tons per year and there are a few
(around 6-10) manufacturing units in India. It was intended to design the process with a production
capacity of 340 tons per year.

Assuming that there are 300 working days in a year, production per day is 1.14 tons

The time required for one batch is around 7 hours.

No. of batches per day = 3

Amount of cinnamic aldehyde produced in one batch is 380 kg. Since this a batch process the units
of mass flow will be in kmol or mol.

The compounds are denoted by the alphabets A, B, C, W to denote acetaldehyde, benzaldehyde,


cinnamic aldehyde and water respectively.

Table 2: Molecular weights and boiling points of the compounds

Compound Name Molecular Boiling


Weight point

C6H5CHO – Benzaldehyde (B) 106 178.1oC

CH3CHO – Acetaldehyde (A) 44 20.2oC

PEG 400-Polyethylene glycol (P) 414 294oC

C6H5CHCHCHO – Cinnamic Aldehyde(C) 132 248oC

H2O – water (W) 18 100oC

Deionised Water (D) 18 100oC

Ion Exchange Resin - -

15
1) Feed

Acetaldehyde (industrial grade GC purity 99.9%) = 9.09 kmol or

400 kg Benzaldehyde (purity 99.5% GC) = 3.77 kmol or 400 kg

Deionised Water = 0.056 kmol or 1 kg

PEG-400 = 4.82 kmol or 2 kg


Rohm & Hass Resin = 50 kg

2) Reactor

ION EXCH. RESIN


C6H5CHO + CH3CHO C6H5CHCHCHO + H2O
PEG 400

Product conversion = 0.80

In product

C = 3.77×0.80 = 3.016 kmol or 398.11 kg

A = 9.09 - 3.016 = 6.074 kmol or 267.26 kg

B = 3.77 - 3.016 = 0.754 kmol or 79.924 kg

W = 3.016×18 = 54.3 kg

Overall mass balance

Mass entering the reactor = 853 kg

Mass leaving the reactor = 852.589 kg

S1 S2

S3

S4 S

S5

Fig 8:- Material balance around the reactor

16
Table 3: Material balance around the reactor

Components S1 S2 S3 S4 S5 S

Acetaldehyde(A) 400 0 0 0 0 267.256

Benzaldehyde(B) 0 400 0 0 0 79.924

Cinnamic Aldehyde(C) 0 0 0 0 0 398.11

Water (W) 0 0 1 0 0 54.288

Rohm & Hass Resin 0 0 0 50 0 50

PEG 0 0 0 0 2 2

Total 400 400 1 50 2 852.589

3) SCREENING

S M

Fig 9:- Material balance around the screening

17
Table 4: Material balance around screening

Components S M N

Acetaldehyde(A) 267.256 267.256 0

Benzaldehyde(B) 79.924 79.924 0

Cinnamic Aldehyde(C) 398.11 398.11 0

0
Water (W) 54.288 54.288

Rohm & Hass Resin 50 0 50

PEG 2 2 0

Total 852.589 802.589 0

4) Separator

Stream X

A = 6.074×1 = 6.074 kmol or 267.256 kg

B = 0.754×1 = 0.754 kmol or 79.924 kg

C = 3.016×1 = 3.016 kmol or 398.11 kg

Stream Y

P = 2 kg

W = 55.28 kg
M X

Fig 10:- Material balance around the separator

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Overall mass balance

Mass entering the phase separator = 801.572 kg

Mass leaving = 267.26+79.924+398.11 = 801.57 kg

Table 5 : Material balance around the separator

Components M X Y

Acetaldehyde(A) 267.256 267.256 0

Benzaldehyde(B) 79.924 79.924 0

Cinnamic aldehyde(C) 398.11 398.11 0

Water (W) 54.280 0 54.280

PEG 400 2 0 2

Total 801.57 745.292 56.280

5) Membrane Separation

Fig 11:- Material balance around the membrane separator

19
Table 6 : Material balance around the membrane separator

Components Y W P

Acetaldehyde(A) 0 0 0

Benzaldehyde(B) 0 0 0

Cinnamic aldehyde(C) 0 0 0

Water (W) 54.28 54.28 0

PEG 400 2 0 2

Total 56.280 54.28 2

20
6) Batch Distillation Tower I

A recovery of 98% of Cinnamic Aldehyde in the lower cut of this distillation tower is assumed.
The purity of the product at this stage is 67%. The following composition is arrived at:

Lower cut W1

Cinnamic Aldehyde in W1 = 3.015×0.99 = 2.986 kmol or 394.14 kg

ThereforeW1= 2.986/0.67= 4.4578kmol

F = W1+ D1

D1 = F – W1 = 9.844-4.4578 = 5.3862kmol

B = 0.549 kmol or 58.2 kg

Upper cut D1

Acetaldehyde gets removed in the upper cut to 99.99%.

A in D1 = 6.002 kmol or 264.08 kg

B = 0.204 kmol or 21.6 kg


D1

FEED

W1

Fig 12: Material balance around the distillation column 1

21
C = 0.03 kmol or 3.98 kg

Overall mass balance

Mass entering = 745.292 kg

Mass leaving = D1 + W1 = 290.06 + 455.74 = 745.2 kg

Table 7: Material balance around the distillation column 1

Components FEED D1 W1

Acetaldehyde(A) 267.256 264.08 2.1

Benzaldehyde(B) 79.924 21.6 58.2

Cinnamic Aldehyde(C) 398.11 3.98 395.24

Water (W) 0 0 0

PEG 0 0 0

Total 745.292 289.66 455.54

7) Batch Distillation Tower 2

Stream W2

C = 2.994× 0.99 = 2.965 kmol or 391.28 kg

Total distillate D2 = 2.965/0.999 = 2.995 kmol or around 64.72 kg

Other compounds = 2.995-2.965= 0.0299 kmol

Stream D2

C = 2.994-2.965 = 0.029 kmol or 3.428 kg

Total residue W2 = W1-D2 = 4.4578-2.995 = 1.4628 kmol

Other compounds in the residue = 1.4628– 0.029 = 1.4338 kmol

22
D2

W2

Fig 13: Material balance around the distillation column 2

Final cinnamic aldehyde content is around 391.28 kg per batch. The required amount was 380kg.
Assuming some losses the value obtained from the mass balance will be sufficient for the desired
annual production.

Table 8: Material balance around the distillation column 2

Components W1 W2 D2

Cinnamic Aldehyde(C) 395.24 391.28 3.428

Benzaldehyde(B) 58.2 0.6 58.1

Acetaldehyde(A) 2.1 0.1 2

Total 455.54 391.98 63.528

Mass entering = 455.54 kg

Mass leaving = D2 + W2 = 391.98 + 63.528 = 455.508 kg

23
9. ENERGY BALANCE
Data
Liquid Heat capacities (in J/kmol.K)
Cp = A+BT+CT2+DT3

𝑇
𝑇 2 − 𝑇𝑜 2 𝑇 3 − 𝑇𝑜3 𝑇 4 − 𝑇𝑜4
∫ 𝐶𝑝 𝑑𝑡 = 𝐴(𝑇 − 𝑇𝑜 ) + 𝐵 +𝐶 +𝐷
𝑇𝑜 2 3 4

Table 9: Heat capacity constant of compounds

Compound A (J/Kmol.K) B(J/Kmol.K2) C(J/Kmol.K3) D(J/Kmol.K4)

Acetaldehyde -52371.79 959.7215 -2.1140 0.00156

Benzaldehyde 147218.4 -229.179 1.2327 -0.00114

Cinnamaldehyde 173059.2 24.46007 0.6498 -0.00055

Water 53996.92 281.6147 -1.1723 0.00150

The above data is taken from NIST database of AspenPlus software. The enthalpies of
the liquids are calculated by the integration formula and for gases the enthalpies are
calculated by numerical methods in the calculator.

Taking reference temperature to be 298K (T0), the energy balance on each unit is shown
below

I. Reactor

(i) Enthalpy of feed stream

HF = ∑(𝑛 ∫ 𝐶𝑝 𝑑𝑇)

Fresh feed at 30oC is entering the batch reactor.

Molar Enthalpy of Acetaldehyde =


-52371.79×(303-298) + 959.7215(3032-2982)/2 – 2.114(3033-2983)/3 + 0.00156(3034-2984)/4
= 4372.96 kJ/kmol

24
Molar Enthalpy of Benzaldehyde =
147218.4×(303-298) – 229.179(3032-2982)/2 + 1.2327(3033-2983)/3 – 0.00114(3034-
2984)/4 = 7936.48 kJ/kmol

Molar Enthalpy of Water =


53996.9(303-298) +281.615(3032-2982)/2 – 1.1723(3033-2983)/3 + 0.0015(3034-
2984)/4 =3673.28 kJ/kmol

Table 10: Enthalpy of feed to the reactor

Component Amount (kmol) Molar Enthalpy Enthalpy (kJ)


kJ/kmol

Acetaldehyde 9.09 4372.96 39750.21

Benzaldehyde 3.77 7936.48 29920.53

Water 0.056 3673.28 205.71

Total 17.736 69876.45

Enthalpy of feed = 6.98E04 KJ

2) Energy balance around reactor

Feed, Batch reactor Product,


303K liq 303 K 319.7 K liq

The reaction takes place at 300C. The feed is preheated to that temperature and fed to the
reactor. The reaction considered is aldol condensation, thus it is an exothermic reaction. Heat
is liberated from the reaction.

Heat of the reaction at 303K = -1.159E04 kJ/kmol

25
Heat liberated = 1.16E04 × 3.77 × 0.80 = 3.49E04

Total energy entering the system = 1.05E05 kJ

The exit stream will retain the above energy assuming that there are no losses to the
equipment. Through trial and error method the exit temperature of the product stream was
calculated to be 319.696 K in Microsoft Excel using the heat capacity equation for liquids.

3) Enthalpy of product stream

The temperature is taken as 319.69K from the energy balance of the reactor.

Molar Enthalpy of Acetaldehyde =


-52371.79×(319.69-298) + 959.7215×(319.692-2982)/2 – 2.114×(319.693-2983)/3 +
0.00156×(319.694-2984)/4 = 5519.78 kJ/kmol

Molar Enthalpy of Benzaldehyde =


147218.4×(319.69-298) – 229.179×(319.692-2982)/2 + 1.2327×(319.693-2983)/3 –
0.00114(319.694-2984)/4 = 9527.37 kJ/kmol

Molar Enthalpy of Cinnamic Aldehyde =


173059.2×(319.69-298) + 24.46×(319.692 -2982)/2 + 0.6498×(319.693 -2983 )/3 –
0.00055×(319.694-2984)/4 = 12106.0 kJ/kmol

Molar Enthalpy of Water =


53996.9×(319.69-298) +281.615×(319.692 -2982 )/2 – 1.1723×(319.693 -2983 )/3 +
0.0015×(319.694 -2984 )/4 = 4614.69 kJ/kmol

Table 11: Enthalpy of product from reactor

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Acetaldehyde 6.074 5519.78 33527.143

Benzaldehyde 0.754 9527.37 7183.63

Cinnamic Aldehyde 3.016 12106.00 36511.69

Water 3.016 4614.69 13917.91

Total 17.68 91141.36

26
4) Overall balance
For overall balance around the reactor, we know
that In + Generation – Accumulation = Out

Table 12: Overall energy balance around reactor

In Generation Accumulation Out

69876.45 kJ 34985.6 kJ 0 91141.36 kJ

In + generation = 69876.45+ 34985.6 =104862.05 kJ


There is a small difference due to approximations.

II. SEPERATOR

(i) Enthalpy of feed stream

Enthalpy of feed to the unit is 91141.36 kJ at 319.7 K (from the energy balance of the
reactor). The Separator operates at a temperature of 349 K. So both the products have exit
at that temperature.

(ii) Enthalpy of product stream to distillation column:--

Molar enthalpy of Acetaldehyde =


-52371.79×(349-298) + 959.7215×(3492-2982)/2 – 2.114×(3493-2983)/3 + 0.00156×(3494-
2984)/4 = 4571.48 kJ/kmol

Molar Enthalpy of Benzaldehyde =


147218.4×(349-298) – 229.179×(3492-2982)/2 + 1.2327×(3493-2983)/3 – 0.00114×(3494-
2984)/4 = 1003.27 kJ/kmol

Molar Enthalpy of Cinnamic Aldehyde =


173059.2×(349-298) + 24.46×(3492-2982)/2 + 0.6498×(3493-2983)/3 – 0.00055×(3494-
2984)/4
= 51749.37 kJ/kmol

27
Table 13: Enthalpy of feed to separator

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Acetaldehyde 6.074 4571.48 27767.17

Benzaldehyde 0.754 1003.27 756.47

Cinnamic Aldehyde 3.016 40807.69 123076.10

Total 9.844 164599.74

(iii) Enthalpy of product stream to screening :-

Molar Enthalpy of Water =


53996.9(349-298) +281.615(3492-2982)/2 – 1.1723(3493-2983)/3 + 0.0015(3494-2984)/4 =
8394.92 kJ/kmol

Table 14: Enthalpy of product stream to screening

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

WATER 3.016 8394.92 25319.1

(iv) Overall balance


For overall balance around the reactor, we know that
In + Generation – Accumulation = Out
Total enthalpy leaving = 63959.74 + 25319.1= 89278.84 kJ
Heat duty of the flash separator = 32.88 Watt (from Aspen simulation)
= 32.88×3600×0.7 = 82857.69 kJ

Table 15: Overall energy balance around seperator

In Generation Accumulation Out

91141.36kJ 82857.69 kJ 0 164599.74

In + generation = 91141.36+ 82857.69 =171599.74 kJ


There is a small difference due to approximations.

28
II. BATCH DISTILLATION COLUMN 1

390 K
Vapour
425 K
Vapour

425 K
Condenser

Batch
349 K Distillation
Feed from 390 K, Liq
separator Column 1

425 K, liq

Fig 12:- Energy balance around the Distillation Column 1

In this column, the feed coming from the separator is fed and the overhead and bottom
streams are withdrawn at 390 K and 425 K respectively. The energy entering the column is
calculated by using the enthalpies of the feed. Therefore, energy entering is

𝟑𝟒𝟗
Ein = ∑i∫𝟐𝟗𝟖 𝒏 ∗ 𝑪𝒑 ∗ 𝒅𝑻

= 164599.74 kJ

Energy exits the column in two streams, through overhead and bottom. It is given by
390 425
𝐸𝑜𝑢𝑡 = ∑ ∫ 𝑛𝑖 × 𝐶𝑝𝑖 × 𝑑𝑇 + ∑ ∫ 𝑛𝑖 × 𝐶𝑝𝑖 × 𝑑𝑇
𝑖 298 298
𝑖

The first summation is for the overhead stream whilst the second summation is for bottom
one.

1) Overhead stream (D1):-

Using Aly Lee equation for gaseous compound enthalpies it is found that:

29
Molar enthalpy of Acetaldehyde at 390 K = 11653.67 kJ/kmol
Molar enthalpy of Benzaldehyde at 390 K = 15480.487 kJ/kmol
Molar enthalpy of Cinnamic Aldehyde at 390 K = 20315.140 kJ/kmol

Table 16: Enthalpy of top product from distillation column 1

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Acetaldehyde 6.002 11653.67 69945.33

Benzaldehyde 0.204 15480.487 3158.02

Cinnamic Aldehyde 0.03 20315.140 609.45

Total 73712.81

2) Bottom stream

Bottom stream contains all the compounds in liquid form, so the molar enthalpies are
calculated as per the integral method shown in Data section. The molar enthalpies are
calculated at 425 K

Molar Enthalpy of Benzaldehyde = 21793.436 kJ/kmol


Molar Enthalpy of Cinnamic Aldehyde = 30595.267 kJ/kmol
Molar Enthalpy of Acetaldehyde = 10170.23 kJ/kmol
Table 17: Enthalpy of bottom product from distillation column 1

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Acetaldehyde 0.048 10170.23 488.17

Benzaldehyde 0.549 21793.436 11964.6

Cinnamic Aldehyde 2.986 30595.267 91357.48

Total 103810.25

30
3) Condenser energy balance

The vapours are entering at the temperature of 425 K and leaving at a temperature of 390 K
in liquid and gaseous form. This reduction in temperature and phase change is brought about
by the condenser. Assuming that the reflux ratio to be 1.35.

L/D = 1.35

L = 1.35D therefore total vapours entering the condenser = D + 1.35D = 2.35D ( V= L+D)

Enthalpy of vapours at 425 K = 2.35×[0.03×13422.6 + 0.204×17241.49 +


6.002×22128.38] = 321326.03 kJ

Enthalpy of liquid stream from the condenser at 390 K = 1.35×[0.03×8349.771 +


0.204×15445.568 + 6.002×21715.404] = 180545.28 kJ

Heat extracted by the condenser = 321326.03 – 180545.28 = 140780.75 kJ

4) Overall energy balance on the column


Enthalpy entering = 164599.74 kJ (from the separator)
Enthalpy leaving = 103810.25 kJ
Energy removed from the condenser = 140780.75 kJ

Energy provided by the reboiler/pot = 103810.25 - 164599.74 +140780.75 =


79991.26 kJ

Table 18: Overall energy balance for distillation column 1

In Reboiler/pot Condenser Out

164599.74 kJ 79991.26 kJ 140780.75 kJ 103810.25 kJ

31
II. BATCH DISTILLATION COLUMN 2

357 K
Vapour
484 K
Vapour

Condenser
425 K Liq Batch
Distillation
Column 2 357 K, Liq
Feed from distillation 1

484 K, liq

Fig 13:- Energy balance around the Distillation Column 2

In this column, the feed coming from the distillation column 1 is fed and the overhead and
bottom streams are withdrawn at 357 K and 484 K respectively. The energy entering the
column is calculated by using the enthalpies of the feed. Therefore, energy entering is

𝟒𝟐𝟓
Ein =∑i∫𝟐𝟗𝟖 𝒏 ∗ 𝑪𝒑 ∗ 𝒅𝑻
= 103810.25 kJ

Energy exits the column in two streams, through overhead and bottom. It is given by

357 484
𝐸𝑜𝑢𝑡 = ∑ ∫ 𝑛𝑖 × 𝐶𝑝𝑖 × 𝑑𝑇 + ∑ ∫ 𝑛𝑖 × 𝐶𝑝𝑖 × 𝑑𝑇
𝑖 298 298
𝑖

The first summation is for the overhead stream whilst the second summation is for bottom
one.
1) Overhead stream

Using Aly Lee equation for gaseous compound enthalpies it is found that:

Molar enthalpy of Benzaldehyde at 357 K = 9927.487 kJ/kmol

Molar enthalpy of Cinnamic Aldehyde at 357 K = 13028.187 kJ/kmol

Molar enthalpy of Acetaldehyde at 357 K=5299.73 kJ/kmol

32
Table 19: Enthalpy of top product from distillation column 2

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Benzaldehyde 0.547 9927.487 5430.33

Cinnamic Aldehyde 0.029 13028.187 377.73

Acetaldehyde 0.045 5299.73 238.49

Total 6076.55

2) Bottom stream
Bottom stream contains all the compounds in liquid form, so the molar enthalpies are
calculated as per the integral method shown in Data section. The molar enthalpies are
calculated at 484 K :-

Molar Enthalpy of Benzaldehyde = 21793.436 kJ/kmol


Molar Enthalpy of Cinnamic Aldehyde = 30595.267kJ/kmol
Molar Enthalpy of Acetaldehyde =17134.52 kJ/kmol

Table 20: Enthalpy of bottom product from distillation column

Component Amount (kmol) Enthalpy per kmol Enthalpy (kJ)

Cinnamic Aldehyde 2.96 30595.267 90561.99

Benzaldehyde 0.0056 21739.436 121.74

Acetaldehyde 0.0023 17134.52 34.41

Total 90723.14

33
3) Condenser energy balance

The vapours are entering at the temperature of 425 K and leaving at a temperature of 357 K
in liquid and gaseous form. This reduction in temperature and phase change is brought about
by the condenser. Assuming that the reflux ratio to be 1.35,

L/D = 1.35

L = 1.35D therefore total vapours entering the condenser = D + 1.35D = 2.35D


Enthalpy of vapours at 484 K = 2.35×[0.547×25251.32 + 0.029×32408.49 +
0.045×29074.33] = 37742.56 kJ

Enthalpy of liquid stream from the condenser at 357 K = 1.35×[0.547×9697.57 +


0.029×13657.154 + 0.045×18195.63] = 8801.24 kJ

Heat extracted by the condenser = 37742.56-8801.24 = 28941.32 kJ

4) Overall energy balance on the column


Enthalpy entering = 103810.25kJ (from the distillation column 1)
Enthalpy leaving = 90723.14 kJ
Energy removed from the condenser = 28941.32 kJ
Energy provided by the reboiler/pot = 103810.25- 90723.14 + 28941.32 = 42028.43
kJ

Table 21: Overall energy balance for distillation column 2

In Reboiler/pot Condenser Out

103810.25 kJ 42028.43 kJ 28941.32 kJ 90723.14 kJ

34
11. DESIGN OF EQUIPMENT
11.1 Design of Batch reactor
11.1.1 Data:
Reactor conversion = 80%
Temperature of the reactor = 30C (303.15 K)
Pressure of the reactor = 1 bar
Catalyst used is Ion exchange resin in basic medium along with PEG 400
Reaction –

Rate expression = -rA = k CA.CB (aldol condensation reactions are of second order)
Where, k is rate constant
At temperature of 303.15K
Activation energy E = 262000 kJ/kmol (without catalyst)
Around 110000kJ/kmol (while using PEG catalyst)
Frequency factor A = 1.27×1015L mol-1s-1
= 1.27×1018 L kmol-1s-1
Rate constant k = A×e-E/RT = 0.1404 L kmol-1 s-1 = 505.6L kmol-1 h-1

11.1.2 Volume and dimensions of the reactor


Governing equation:
𝑑𝐶
− = −𝑟 … … . (𝑖)
𝑑𝑡

For a second order reaction with same initial inlet concentrations and constant volume
Process, the above reaction can be written as,
𝑑𝐶
= −𝑘𝐶 2 … … . (𝑖𝑖)
𝑑𝑡
In terms of conversion x,
𝑥
= 𝑘 × 𝐶° × 𝑡 … … . (𝑖𝑖𝑖)
1−𝑥

35
Time of operation, t = 2.2 h
No = 13 kmol (13 kmol of acetaldehyde and benzaldehyde is initially fed to the reactor),
Co = No/V = 13/V
x = 0.8
V = k×No×t×(1-x)/x
= 505.6 L kmol-1 h-1 × 13 kmol × 3.2 h × (1-0.8)/0.8
= 3615.2 L = 3.615 m3
From the kinetics of the reaction the volume should be 3.615 m3 for 0.8 conversion and
residence time of 2.2 hours.
Taking into consideration that some vapours may be formed and process instruments occupy
some of the reactor volume,
Allowance = 30% of volume of liquid
Volume of the reactor VT = 1.3 × 3.615 = 4.71 m3
Let the ratio of height to diameter of the reactor is 1.5
H/D = 1.5
VT = Π × (D2/4) × H
= Π × (D2/4) × (1.5D)
= (3/8) × Π × D3 = 4.71
Therefore, D = 1.59 m
H = 2.38 m
Height of dished bottom = 1 m
Total height, H= 3.38 m

11.1.3 Mechanical Design of reactor


A) Wall thickness
For the calculation of wall thickness, the total pressure which is the sum of static and
Operating pressure of the reactor
Density of the contents ρ = Mass/ Volume = 853/ 4.71 = 181.1 kg/m3
Static pressure (Ps) = ρ × g × H
= 181.1 × 9.81 × 2.38
= 4228.28 Pa
Operating pressure = 100000 Pa
Total pressure at base = Ps + Po = 104.228 kPa
Maximum allowable pressure, P = 1.33 × 104.23 = 138.624 kPa

36
Wall thickness = (P × Ri)/(S×Ej-0.6P) + CC
Material = Carbon steel
Working stress of Carbon steel, S = 94408 kN/m2
Internal radius, Ri = 0.795 m
Joint efficiency, Ej = 0.85
Corrosion allowance, CC = 2 mm = 0.002 m
Therefore wall thickness = (138.624×0.795)/(94408×0.85-0.6×138.624) + 0.002
= 0.00337 m =3.37 mm
Therefore outside diameter = Di + 2×t = 1.59 + 2×0.00337 = 1.60 m
B) Reactor head
Ellipsoidal head is used for pressure greater than 1034.214 KPa and for less than that
pressure at spherical head is used. As the pressure is around 165.474 KPa a torispherical head
is selected.
th = 1.104PD/(2ES – 0.2P) + tc
= 0.027 + 0.002
= 0.029 m
Thickness of the torispherical head = 29 mm
C) Agitator design
Agitators dimensions are
Impeller Diameter Da = Dt/3 = 0.53m
Impeller Height above the vessel floor E = Da= 0.53m
Length of Impeller Blade L = Da/4 = 0.132m
Width of Impeller Blade W = Da/5 = 0.106m
Width of Baffle J = Dt/10 = 0.159m
No. Of Impellers = 1
No. Of Impeller blades = 2
Shape Factors are
S1 = Da/Dt = 1/3 S2 = E/Dt = 1/3
S3 = L/Da = 0.25 S4 = W/Da = 1/5
S5 = J/Dt = 1/10 S6 = H/Dt = 1.5
Tip Velocity is generally in between 3 to 6 m/s
Assuming the velocity to be 3 m/s,
Tip velocity = Π × Da × N
Therefore, speed of impeller = [3/( Π×0.53)] × 60 = 108 RPM

37
Power No (Np) = 6
Shaft RPM (N) = 108 RPM = 1.8 rev/s
Power = Np × N3 × Da5 × ρ/ gc = 1.21 HP
Taking 85% efficiency, power required = 1.42 HP
D) Baffle design
No. Of baffles = 4
Width of one baffle = Dt/10 = 0.157 m
Height of baffle = 2.38 m

38
11.2 Design of Screening

Fig 13:- Basic screening setup

11.2.1 Data:
1. Average flow = 3000 Litre/day
= 3.47 × 10-5 m3/Sec
Maximum Flow = 4000Litre/day
= 4.63 × 10-5 m3/Sec
Minimum flow = 2700 Litre/day
=3.12 × 10-5 m3/Sec
2. Assume manual cleaning and angle of inclination of bars with horizontal as 300
Assume size of bars 9 mm x 50 mm, 9 mm facing the flow. A clear spacing of 30 mm
between the bars is provided.
3. Assume velocity of flow normal to screen as 0.1 m/sec at average flow.
4. Net submerged area of the screen opening required
= 3.47 × 10-5 m3/sec
0.1 m/sec
= 3.47 cm2
Assume velocity of flow normal to the screen as 0.4 m/sec at maximum flow, hence net
submerged area of screen opening
= 4.63 × 10-5 m3/sec
0.4 m/sec
= 1.16 cm2
Provide net submerged area = 3.47 cm2

39
5. Gross submerged area of the screen
When ‘n’ numbers of bars are used the ratio of opening to the gross width will be
[(n+1)30] / [(n+1)30 + 9 x n] ≈ 0.77 (for 20 to 30 number of bars)

Therefore gross submerged area of the screen 3.47 / 0.77


= 4.51 cm2
6. The submerged vertical cross sectional area of the screen
= 4.51 x Sin 30 = 2.25 cm2
This is equal to cross-sectional area of screen chamber, therefore velocity of flow in screen
chamber
= 3.47 × 10-1cm3/sec / 0.5 cm2 = 0.694cm/sec
This velocity is greater than the self cleansing velocity of 0.42 cm/sec
7. Provide 30 numbers of bars. The gross width of the screen chamber will be:
= 30 x 0.009 + 31 x 0.03 = 1.2 m
Therefore, liquid depth at average flow = 0.5 / 1.2 = 1.875cm
Provide free board of 0.1 m
Hence, total depth of the screen = 1.875 + 10 = 11.875 ≈ 12cm
Thus, the size of the channel = 1.2 m (width) x 0.12 m (depth)
9. Head loss through the screen, h, when screen is not clogged.
h = β (W/b)4/3 hv Sin θ
= 2.42× (9/30)4/3 ×[(0.694)2/(2 x 9.81×104)]× Sin 30
= 2.65 x 10-3 m = 0.00265 m = 2.65 mm

40
11.2 Design of flash separator

11.2.1 Volume and dimensions of the separator

Fig 14:-- Basic Flash column setup

Variables to determine: Diameter of the flash column, D


Height of liquid in the column hL
Height of feed inlet, hV
Permissible vapour velocity, Vperm

(𝜌𝐿− 𝜌𝑉 )
𝑉𝑝𝑒𝑟𝑚 = 𝐾 × √ … … . (𝑖𝑣)
𝜌𝑉

K is an empirical constant that depends on the type of drum.


2
+𝐷𝑙𝑛𝐹𝑙𝑣 3 +𝐸𝑙𝑛𝐹𝑙𝑣 4
𝐾 = е𝐴+𝐵𝑙𝑛𝐹𝑙𝑣+𝐶𝑙𝑛𝐹𝑙𝑣 … … . (𝑣)

𝑊𝑙 𝜌𝑣
𝐹𝑙𝑣 = ×√ … … . (𝑣𝑖)
𝑊𝑣 𝜌𝑙

Flv = 56.28/745.292 × (0.5618/1492.5)0.5 = 1.4657×10-3

A = -1.877478

41
B = -0.814580

C = -0.187074

D = -0.014523

E = -0.001015

K = 0.107 ft/sec (from the expression)

Vperm = 0.1504 × [(1492.5-0.56181)/0.56181]0.5 = 5.514 ft/sec = 1.57 m/s


Volumetric flow rate of the vapour = (mass/density)/time
= (745.292/0.56181)/(0.67×3600) = 0.55 m3/sec
Cross sectional area = flow rate/velocity = 0.55/1.57 = 0.35m2
Diameter = (4×A/Π)0.5 = 0.668 m
Height of pool in the column, hL = Volume of liquid /A = 0.78/0.35 = 2.23 m Height of feed
line from head= 36’’ + (1/2) diameter of feed line Assuming the diameter of the feed line is 4
inches, hV = 38’’ = 0.9652 m Height of feed line from liquid level, hf = 12’’ + (1/2) diameter
of feed line = 14’’ = 0.3556m
Finally, Height of column = hL + hV + hf = 2.23 + 0.3556 + 0.9652 = 3.5508 m
If 3< (L/D) < 5, the column should be vertical
Otherwise, the column should be horizontal
L/D = 3.526/0.668 = 5.3156
The flash separation column orientation should be in vertical alignment.

11.2.2. Mechanical design


A) Thickness calculation
The design specifications:
Po =101.3 kPa
Temperature=349K
Di = 0.668 m
Height = 3.508 m
Density, ρ = 1492.5 kg/m3
Joint Efficiency, E = 0.85 (Joint efficiency for spot examined of shell and hemi. Head to
shell.

42
Corrosion Allowance, CA = 0.125 inch = 3.175 cm Top
Head: Hemisperical
H = D/2 =0.668/2 =0.334 m
Pd = Po + ρgh
=101300 + (1492.5 x 9.81 x 0.334) =104.711 kPa
Pj = Pd×Safety factor
=104.711×(1.1)
=115.18 kPa
t = (PR)/(2SE + 0.2P)
= (115.18 x 0.334)/(2 x 94408 x 0.85 + 0.2 x 115.18)
=2.4mm
Shell : Cylindrical
H = 3.508 – ((1/3)×0.334) –( (1/3)×0.167) + 0.334 = 3.675m
Pd= 101300 + (1492.5×9.81×3.675)
= 139.015 KPa
PJ= 139.015×1.1
= 152.916 KPa
t = (PR)/(SE – 0.6P)
= (152.916×0.334)/(94408 x 0.85 – 0.6 x 152.916) = 6.37 mm
Bottom head : Ellipsodal
h= 3.675 + 0.167
= 3.842 m
Pd = 101300 + 1041.04 x 9.81 x 3.842
= 140.72 kPa
PJ = 140.72 × 1.1
= 154.792 kPa
t = (PD)/(2SE – 0.2P)
= (154.792 x 0.668)/(2 x 94408 x 0.85 – 0.2 x 154.792)
= 6.4mm
Height = 3.508 m
Density,ρ = 1492.5 kg/m3
Joint Efficiency, E = 0.85 (Joint efficiency for spot examined of shell and hemi. Head to
shell.
Corrosion Allowance, CA = 0.125 inch = 3.175 cm

43
Top Head: Hemisperical
H= D/2 = 0.668/2 = 0.334 m
Pd = Po + ρgh
=101300+(1492.5x9.81x0.334)
=104.711 kPa
Pj = Pd×Safety factor
=104.711×(1.1)
=115.18 KPa
t = (PR)/(2SE + 0.2P)
= (115.18 x 0.334)/(2 x 94408 x 0.85 + 0.2 x 115.18)
=2.4mm
Shell : Cylindrical
h = 3.508 – ((1/3)×0.334) –( (1/3)×0.167) + 0.334 = 3.675 m
Pd = 101300 + (1492.5 ×9.81×3.675) = 139.015 KPa
PJ = 139.015 × 1.1
= 152.916 KPa
t = (PR)/(SE – 0.6P)
= (152.916×0.334)/(94408 x 0.85 – 0.6 x 152.916) = 6.37 mm
Bottom head : Ellipsodal
h = 3.675 + 0.167 = 3.842 m
Pd = 101300 + 1041.04 x 9.81 x 3.842
= 140.72 kPa
PJ = 140.72 × 1.1
= 154.792 kPa
t = (PD)/(2SE – 0.2P)
= (154.792 x 0.668)/(2 x 94408 x 0.85 – 0.2 x 154.792) = 6.4 mm
The thicker one is chosen, t = 6.4 mm
B) Maximum allowable working pressure
Hemispherical head:
L = 0.334 m
T = 0.0064 m
P = (2SEt)/(L + 0.2t)
= (2 x 94408 x 0.85 x 0.0064)/(0.334 + 0.2 x 0.0064)
= 3063.59 kPa

44
Shell : Cylinder
P = (2S×Et)/(R + 0.6t)
= (2 x 94408 x 0.85 x 0.0064)/(0.334 + 0.6 x 0.0064)
= 3040 kPa
Ellipsoidal:
P = (2S×Et)/(D + 0.2t)
= (2 x 94408 x 0.85 x 0.0064)/(0.668 + 0.2 x 0.0064)
= 1534.72 kPa
Maximum allowable working pressure = 3063.59 kPa
C) Analysis of stress
Longitudinal Stress
σL = PDi/4t
= (3063.59 x 0.668)/(4 x 0.0064)
= 79940 kN/m2
σh = PDi/(2t)
= (3063.59 x 0.668)/(2 x 0.0064)
= 159881 KN/m2
Direct stress
σ = W/(π(Di + t)t)
Pw = 1280 N/mm2
Deff = Do
= Di + 2t
= 0.668 + 2(0.0064)
= 0.680 m
Dm = Di + t
= 0.668 + 0.0064
= 0.6744 m
Wv = 240×Cv×Dm×(Hv + 0.8Dm)×t
=240(1.08)(0.6744)(0.9652 + 0.8 x 0.6744)(0.0064)
=1.67 kN
Dead weight of stress
σw = 1.67x103/(π(0.668 + 0.0064)0.0064)
= 123.159 kN/m2
Bending stress
σb = ± (M/Iv)(Di/2 + t)

45
Mx = Wx2/2
Wind load
W= PwDeff
=1280 × (0.68)
= 870.4 N/m
x = hv
= 0.9652m
Mx= (870.4 × 0.96522)/2
= 395 N/m
Iv = π/64(Do4 – Di4)
= π/64(0.68084 – 0.6684)
= 7.7×10-4 m4
σb = ± (395/7.7×10-4)(0.668/2 + 0.0064)
= 174.62 kN/m2
For total longitudinal stress
σz = σL + σw ± σb
upwind
σz = σL + σw + σb
= 79940– 123.159 + 174.64
= 79991 kN/m2
Downwind
σz = σL + σw – σb
=79940 + 123.159 - 174.64
=79888.5 kN/m2
Maximum stress intensity
(∆σ)max = σ1 + σ2
=σh + σz
=159881 + 79991
=239872 kN/m2

Elastic Stability:
𝐸 𝑡
𝜎𝑐 = ×( ) … … (𝑣𝑖𝑖)
√3(1 − 𝑣 2 ) 𝑅𝑝

For steel at the ambient T, E = 94408 kN/m2 and with safety factor

46
σc = 94408 ×(0.0064/0.680)
= 888.546 kN/mm2
Maximum value of resultant
Σσ = σb + σw
= 174.62 kN/m2 + 123.159 kN/m2
= 297.78 kN/mm2
So: Σσ < σc { 297.78 < 888.55 }
Since that the maximum value of resultant not exceed the critical stress, the design is safe.
Flanges
Several different types of flange are used for various application. The principal types used in
the process industries are:
1. welding-neck flanges
2. slip-on flanges, hub and plate types
3. lap-joint flanges
4. screwed flanges
5. blank, or blind flanges
In term of economical aspect; since in this pressure vessel design, the material construction is
stainless steel which is expensive alloy pipe, so lap-joint flanges is suitable because they are
cheap because can be made from inexpensive carbon steel.
The lap can be formed on the pipe itself in some schedule of pipe and will give a cheap
method of pipe assembly.

47
11.3 Design of Distillation column 1 :-
11.3.1Procedure
Vapor -liquid equilibrium is calculated by Antoine equation:-
𝑜
𝐵
log(𝑃𝑣𝑎𝑝 )=𝐴− … … . (𝑣𝑖𝑖𝑖)
𝑇+𝐶

Where:
Pvap=Vapour pressure of the component
A,B,C= Antoine constants
T= Absolute temperaturein Kelvin
For saturation feed at 349 K and 1bar

Table 22: Antoine constant data of compounds [6]

Component name Symbol A B C

Benzaldehyde Bz 5.21 2337.6 -5.1

Acetaldehyde Ac 3.7 823 -70

Cinnamaldehyde Cn 5.45 2677 -27

III. RESULTS AND DISCUSSION


The following data are obtained:

Table 23: Equilibrium Data of different components [5]

Component Symbol Vapour Distribution Component


name pressure(pv) coefficient(Ki) feed rate
Kmol/h

Benzaldehyde Bz 0.2045 0.2045 0.375

Acetaldehyde Ac 2.12 2.12 3.035

Cinnamaldehyde Cn 0.06 0.06 1.51

48
Calculate from equilibrium relationship: Ki= Pvi/Pt
Where:
Pvi = vapour pressure of component i
Pt = total pressure
Minimum number of stages
Fenske Equation
xD 1−xW
log ( )
1−xD xW
Nm = … … . (ix)
log αavg

αavg = √αt αb … … (x)

Where:-
Nm = minimum number of stages, xD =composition of the top product
α = relative volatility, xw=composition of the bottom product

Table 24: Composition of different components in feed, top and bottom streams

Component name Feed mole D, Mole W, Mole fraction


fraction fraction

Benzaldehyde 0.08 0.032 0.13

Acetaldehyde 0.62 0.964 0.2

Cinnamaldehyde 0.30 0.005 0.67

Where: D= distillate product, W= bottom product

Table 25: Relative volatility of compounds

Component name 𝛼i=pi/pj

Benzaldehyde 3.41

Acetaldehyde 35.33

Cinnamaldehyde 1

Pvi = vapour pressure of component i


Pj = vapour pressure of heavy key j

49
αlk =35.33 ,where αlk is the relative volatility of light key

Table 26 :-Composition of heavy and light key

Lk Hk

xD,mole fraction 0.964 0.005

xW,mole 0.2 0.67


fraction

The mole fraction of XD and XB are experimental data.


Determination of minimum number of stages (Nm):
Nm = 5.2 = 6 stages
Minimum Reflux Ratio Rm
Using Underwood equation:
αi xif
1−q =∑ … … . (xi)
αi − θ

For saturation feed condition, q=1, θ = 1.3 by trial and error


Where: αi = relative volatility of component (i), XiF = composition of component ( i) in feed

Table 27:- Calculation Table for minimum reflux

Component name αi xif



αi − θ
Benzaldehyde 0.51

Acetaldehyde 1.27

Cinnamaldehyde -0.0013

Total=1.78

Rm = 0.9
R actual = 1.5 × Rm = 1.35
Where R actual = R
X = (R-Rm) /(R+ 1) = 0.2

50
Y = 1- X0.33 = 0.41
N = (Nmin + Y)/(1-Y) = 10.86 = 11 stages

Column Efficiency :
Eo= 51 – 32.1 log (αi× μi)
μi = average viscosity= ∑ μi xi,
αi = relative volatility of light key
Eo= 65.4 Na = 11/0.654= 17 stages

Height of the column


Ht = (Na – 1) ×C + (Na /10) × C + 0.1 Ht
Where: Ht = Height of the column.
C = tray Space = 0.6
Ht = 14 m

Flow Rates:
Feed = 0.373 Ton/h.
Top Product(F) = 0.145 T/h.
Bottom Product(W) = 0.223 T/h
Vapor rate = D (1+R) = 0.341 T/h
LT = DR = 0.2 T/h; LB = F + LT = 0.573 T/h
Vapor rate (Bottom) = LB-W = 0.35 T/h
L / V (top) = 0.58 L / V (bottom) = 1.64

Column diameter: The column diameter must be selected so that flooding does not occur,
however at the same time vapour velocities that are high for greater plate are needed. In these
calculations, operation at 85% of flooding velocity is taken, this velocity determined from
equation:-

ρl − ρv
uf = k l √ … … (xii)
ρv

Flow factor:-
Lw ρv
Flv = … … . (xiii)
Vw √ ρl

51
Where:
ρv = density of the vapor phase
ρl= density of the liquid phase

Densities at the top of the distillation column


ρv= 0.67 Kg/m3 ρl= 1.07 Kg/m3
Densities at the bottom of distillation column
ρv= 1.16 Kg/m3 ρl= 1.23 Kg/m3

Taking tray spacing = 0.6 m


Flow factor at the top = 0.03
Flow factor at the bottom = 0.02
KT = 0.18 KB = 0.16
Where: KT and KB are constants at the top and bottom respectively
Velocity at the top = 2.8 m/s
Velocity at the bottom = 2.3 m/s
Operation at 85% flooding rate
Velocity at the top = 0.38m/s
Velocity at the bottom = 0.9 m/s

Calculation of volumetric flow rates


At the top =341/0.67/3600 = 0.14 m3/s
At the bottom =341 /1.17 / 3600= 0.11 m3/s
Area of the column:-
Top = 0.14/ 0.38= 0.4 m2
Bottom = 0.11/0.9 = 0.122 m2
Column cross sectional area:-
Top = 0.4 / 0.88 = 0.5 m2
Bottom = 0.122/0.88 =0.15 m2
4𝐴
Diameter of column: 𝐷 = √ 𝜋

DT = 0.8m, DB = 0.44 m
Where: DT= column diameter at the top, DB = column diameter at the bottom

52
Column diameter = 0.8 m
Column area = 0.51 m2
Down comer area (12 % Ac) = 0.06 m2
Active area = Ac – 2Ad = 0.39 m2
Hole area (10% Aa) = 0.04 m2
Hole diameter = 5 mm Plate thickness = 5 mm
Area of one hole = 1.96×10-5
Number of holes = 7945 holes

53
11.4 Design of Distillation column 2 :-

The feed to the distillation tower 2 is the distillate from the residue still, which consists of
Benzaldehyde and Cinnamaldehyde, in the condensed form. This being a binary mixture, the
Mc.Cabe Thiele method is applied to the distillation column.
Here Benzaldehyde is the light key component, and Cinnamaldehyde is the heavy key
component. The column is operating at 484 K and 1atm pressure. The feed entering from the
residue still must be saturated liquid at its bubble point. The bubble point and dew point for
the Benzaldehyde- Cinnamaldehyde mixture are to be calculated.

Antoine equation parameters:


𝑩
log10(P) = 𝑨 − 𝑻+𝑪 … … . (𝑣𝑖𝑖𝑖) where T(temperature) in K , P(Vapor Pressure) in bar

Table 28 :- Antoine constants data of compounds


Component Temp A B C References
range
Benzaldehyde 300 K - 5.21 2337.6 -5.11 [6]
491.1 K
Cinnamaldehyde 344 K - 5.45 2677 -27 [7]
493 K

Table 29 :- Composition of feed, top and bottom streams in distillation column 2

Mole Fractions: Weights(Kg)


Feed Distillate Residue Feed Distillate Residue
Benzaldehyde 0.16 0.954 0.01 58.2 57.2 0.5
Cinnamaldehyde 0.846 0.046 0.99 395.24 3.428 391.28

Bubble Point Calculation:-


Here the values Xi and P are known
Assume T= 425 K
Ki = vapor pressure/total pressure = Yi/Xi

Table 30 :- Vapor pressure Calculation table

54
Component Symbol Vapour Distribution Component
name pressure(pv) coefficient(Ki) feed rate
Kmol/h

Benzaldehyde Bz 0.439 0.439 0.375

Cinnamaldehyde Cn 0.053 0.053 1.51

Calculate from equilibrium relationship: Ki= Pvi/Pt


Where:
Pvi = vapour pressure of component i
Pt = total pressure
Minimum number of stages
xD 1−xW
log ( )
1−xD xW
Nm = … … . (ix)
log αavg

αavg = √αt αb … … (x)

Where:-
Nm = minimum number of stages, xD =composition of the top product
α = relative volatility, xw=composition of the bottom product
Where: D= distillate product, W= bottom product

Table 31:- Relative volatility of compounds


Component name 𝛼 i=pi/pj

Benzaldehyde 8.28

Cinnamaldehyde 1

Pvi = vapour pressure of component i Pj = vapour pressure of heavy key j


αlk = ,where αlk is the relative volatility of light key
Assume T = 390.22 K
q = (heat to convert to saturated vapor)/(heat of vaporization) = 1.000
As the feed is saturated liquid, the slope of q-line=q/(q-1) is infinite.

Table 32:- Composition of light and heavy key

Light Key Heavy Key

55
XD,mole 0.954 0.046
fraction

XW,mole 0.01 0.99


fraction

The mole fraction of XD and XB are experimental data


Determination of minimum number of stages (Nm):
Nm = 7.21 = 8 stages
Minimum Reflux Ratio Rm
Using Underwood equation:
αi xif
1−q=∑ … … (xi)
αi − θ

For saturation feed condition, q=1, θ = 1.2 by trial and error


Where: αi = relative volatility of component (i), xif = composition of component i in feed

Table 33:- Calculation Table for Minimum reflux

Component name αi xif



αi − θ
Benzaldehyde 1.67

Cinnamaldehyde 0.05

Total=1.72

Rm = 0.72
R actual = 1.5 × Rm = 1.08 Where R actual = R
X = (R-Rm) /(R+ 1) = 0.17
Y = 1- X0.33 = 0.44
N = (Nmin + Y)/(1-Y) = 15.07 = 16 stages

Column Efficiency:-

56
Eo= 51 – 32.1 log (αi× μi)
μi = average viscosity= ∑ μi xi,
αi = relative volatility of light key
Eo= 65.4 Na = 16/0.654= 25 stages
Height of the column :-
Ht = (Na – 1) ×C + (Na /10) × C Where: Ht = Height of the column.
C = tray Space = 0.6 , Ht = 16 m
Flow Rates:- Feed = 0.455 Ton/h. , Top Product = 0.063 T/h.
Bottom Product = 0.391 T/h
Vapor rate (Top) = D (1+R) = 0.13 T/h
LT = DR = 0.2 T/h ; LT :- Liquid flow rate at Top
LB = F + LT = 0.655 T/h ; LB :- Liquid flow rate at Bottom
Vapor rate (Bottom) = LB-W = 0.264 T/h
L / V (top) = 1.54 L / V (bottom) = 2.48
Column diameter: The column diameter must be selected so that flooding does not occur,
however at the same time vapour velocities that are high for greater plate are needed. In these
calculations, operation at 85% of flooding velocity is taken, this velocity determined from
equation:-

ρl − ρv
uf = k l √ … … (xii)
ρv

Flow factor:-
Lw ρv
Flv = … … . (xiii)
Vw √ ρ l

Where:
ρv = density of the vapor phase
ρl= density of the liquid phase
Densities at the top of the distillation column
ρv= 0.64 Kg/m3 ρl= 1.03 Kg/m3
Densities at the bottom of distillation column
ρv= 1.06 Kg/m3 ρl= 1.13 Kg/m3
Taking tray spacing = 0.6 m
Flow factor at the top = 0.03
Flow factor at the bottom = 0.02

57
KT = 0.18, KB = 0.16
Where: KT and KB are constants at the top and bottom respectively
Velocity at the top = 2.8 m/s
Velocity at the bottom = 2.3 m/s
Operation at 85% flooding rate
Velocity at the top = 0.38m/s
Velocity at the bottom = 0.9 m/s
Calculation of volumetric flow rates
At the top =130/0.64/3600 = 0.10 m3/s
At the bottom 130 /1.06 / 3600= 0.07 m3/s
Area of the column
Top = 0.10/ 0.38= 0.3 m2
Bottom = 0.07/0.9 = 0.08 m2
Column cross sectional area
TOP = 0.3 / 0.88 = 0.34 m2
Bottom = 0.08/0.88 =0.10 m2
4𝐴
Diameter of column : √ 𝜋

DT = 0.8m, DB = 0.44 m
Where: DT= column diameter at the top, DB = column diameter at the bottom
Column diameter = 0.8 m
Column area = 0.50 m2
Down comer area (12 % Ac) = 0.06 m2
Active area = Ac – 2Ad = 0.38 m2
Hole area (10% Aa) = 0.04 m2
Hole diameter = 5 mm Plate thickness = 5 mm
Area of one hole = 1.96×10-5
Number of holes = 7945 holes

12. COST ESTIMATION

58
12.1 Estimation of total capital investment

Marshall and Swift equipment cost index for different equipment has been obtained from the
year 1985. Using the relative capacities, the total equipment cost can be determined for the
year 1985.

Table 34: Equipment cost estimating parameters


Equipment Plant parameter Reference Range validity Cost(Cr) N
size $1000

Distillation 10 trays×2 5 trays 5-50 trays 3300 1.0


Column

Batch reactor 4.7 m3 or 18000 100 gallon 100-20000 93 0.59


gallon gallon

Flash separator 1.1 m3 or 4500 100 gallon 100-105 gallon 2.6 0.52
gallon
Pump 1kW ×2 10kW 0.2-16 kW 2 0.26

Screening 1.3 m3 or 4700 100 gallon 100-105 gallon 0.2 0.54


gallon

Cost of the equipment in the table = $ (3300000×2 + 1716800 + 1100×2 + 19200)


= $ 8338200
Cost of auxiliary equipment like generators, motors, electrical instruments
= 40% of $8338200 = $ 333530

Total cost of plant in 1985 = $ 8,338,200 + $ 333,530 = $ 11,673,480


In 1985, 1 dollar = $ 12.6
Cost of plant in rupees = Rs 14, 70, 85,848 or approximately Rs 15, 00, 00,000

Using this cost, the equipment cost in 2018 can be estimated using the chemical plant cost
index method.

59
12.1.1 Direct costs

Material and labour involved in actual installation of complete facility (70 – 85% of fixed
capital investment). Assume direct cost to be 75% of cost of equipment.

(A) Machinery
Equipment purchase cost + Installation cost + Instrumentation and controls cost +
Piping installation cost + Electrical installation cost.

(i) Purchased cost (cost of equipment)


Chemical Plant Cost Index:
• For 1985: 325.3
• For 2018: 614.79
Estimated equipment cost in 1985 = Rs 15,00,00,000
Cost of equipment in 2018 = Cost in 1989 × Index for 2018/Index for
1985 = Rs 15,00,00,000 × 614.79/325.3 = Rs 283487550 = Rs 28.3448×107

(ii) Installation cost, including insulation and painting (25-55% of purchased cost)
Assuming 40% of purchased cost = 0.40×28.3448×107= Rs 11.3395×107

(iii) Instrumentation and controls cost (6-30% of purchased cost)


Assuming 30% of purchase cost = 0.30×28.3448×107 = 8.50344×107

(iv) Piping installation cost(10-80% of purchased cost)


Assuming 30% of purchased cost = 0.30×28.3448×107 = Rs 8.504×107
(v) Electrical costs(10-40% of purchased cost)
Assuming 10% of purchased cost = 0.10×28.3448×107= Rs 2.83448×107

Machinery cost, A = i + ii + iii + iv + v = Rs 59.556×107

(B) Building, process and auxiliary (10-70% of purchased cost)


Assuming 10% of purchased cost, B = 0.10 × 28.3448×107= Rs 2.83448×107

(C) Service facilities and yard improvements (40-100% of purchased cost) Assuming
55% of purchased cost, C = 0.55 × 28.3448×107= Rs 15.5896×107

(D) Land (10-20% of purchased cost)


Assuming 15% of purchased cost, D = 0.15 × 28.3448×107= Rs 4.2517×107

Direct costs = A + B + C + D = Rs 82.2014×107

60
12.1.2 Indirect costs

(E) Engineering and supervision (5-30% of direct cost)

Assuming 30% of direct cost, E = 0.3 × 82.2014×107= Rs 24.6604×107

(F) Construction expenses and contractor’s fee (6-30% of direct cost)


Assuming 25% of direct cost, F = 0.25 × 82.2014×107=Rs
20.5503×107

Indirect costs = E + F = Rs 45.2107×107

12.1.3 Contingency costs

5-15% of (direct cost + indirect cost)


Direct cost + Indirect cost = Rs 127.4121×107
Assuming the ratio as 10%, contingency cost = 0.1 ×127.4121 ×107 = Rs 12.74121×107

12.1.4 Total capital investment

Fixed Capital investment = Direct cost + Indirect cost + Contingency cost


= 82.2014×107+ 45.2107×107+ 12.74121×107
= Rs 140.1533×107

Working Capital – 10-20% of Fixed Capital investment


Assuming 15% of Fixed capital, working capital = 0.15 × 140.1533×107= Rs 21.0229×107

Total capital investment = Fixed capital investment + Working capital


= 140.1533×107+ 21.0229×107
= Rs 161.1762×107
The proposed total capital investment for the cinnamaldehyde will be Rs 161.1762×107.

Table 35: Total capital investment evaluation

61
Rate Component Sub-total (Rs) Amount (Rs)
(Rs)
Old Cost (1985) 325.3 15,00,00,000
New Cost (2018) 614.79 28.3448×107
(i)Purchase Equipment 28.3448×107
(ii) Installation 40% 11.3395×107
(iii) Instrumentation 30% 8.50344×107
(iv) piping installation 30% 8.50344×107
(v) Electrical installation 10% 2.83448×107
(A) Machinery (i+ii+iii+iv+v) 59.5256×107

(B)Building process auxilary 10% 2.83448×107


(C)Service 55% 15.5896×107
(D)Land 15% 4.25172×107
Direct Cost DC(A+B+C+D) 82.2014×107
24.6604×107
(E) Engineering &
Supervision 30%
20.5503×107
(F) Construction &
contractor’s fee 25%
45.2107×107
Indirect cost IC (E+F)
10% 12.774121×107
Contingency CC(based on
DC + IC)
140.1533×107
Fixed capital investment
FC (DC+IC+CC )
15% 21.0229×107
Working capital WC
161.1762×107
Total capital investment
(TCI)

12.2 Estimation of Total Product Cost

62
12.2.1 Manufacturing Cost
(A) Fixed Cost
(i) Depreciation (depends on life period, salvage value and method of calculation about
10% of FCI for machinery and equipment and 3-5% of Building Value for buildings)

10% of FCI for machinery = 0.10×59.556×107= Rs 5.9556×107

5% of Building value for building = 0.05×2.83448×107= Rs 0.1417×107


Total Depreciation = Rs 6.0973×107

(ii) Local taxes (3-4% of Fixed Capital Investment) Assumed value, 3% of FCI
= Rs 4.2046×107

(iii) Insurances (0.4 – 1 % of Fixed Capital Investment)


Assumed value, 1% of FCI = Rs 1.4015×107

(iv) Rent (8-12% of the rented land and buildings)

Assuming 10% of building value = 0.10×2.83448×107 = 0.28344×107


Total Fixed Cost = i + ii + iii + iv = Rs 11.987×107

Now, Fixed Costs = 15% of Total Product Cost

Thus, Total Product Cost = Rs 11.987×107/0.15 = Rs 79.912×107

(B) Direct Production Cost

(i) Raw materials (10-50% of Total Product Cost)

Assumed value, 30% of Total Product Cost = 0.30×79.912×107 = Rs 23.974×107

(ii) Operating labour (10-20% of Total Product Cost)

Assumed value, 15% of Total Product Cost = 0.15×79.912×107 = Rs 11.987 ×107

(iii) Direct supervisory and clerical staff (10-25% of operating labour)


Assumed value, 15% of Operating labour = 0.15×11.987×107 = Rs 1.798 ×107

(iv) Utilities (10-20% of Total Product Cost)

Assumed value, 12% of Total Product Cost = 0.12×79.912×107 = Rs 9.5894×107

(v) Maintenance and repairs (2-10% of Fixed Capital Investment)


Assumed value, 8% of FCI = 0.08×140.1533×107 = Rs 11.212×107

(vi) Operating supplies (10-20% of cost of maintenance and repair)


Assuming 10% = 0.10×11.212×107 = $ 1.1212×107

(vii) Laboratory charges (0-20% of operating labour)

Assuming 10% of Operating labour = 0.10×11.987 ×107 = Rs 1.1987×107

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(viii) Patents and royalties (0-6% of Total Product Cost)

Assumed value, 5% of Total Product Cost = 0.05×79.912×107 =Rs 3.9956 ×107

Direct Production cost = Sum [(i), (ii), (iii), (iv), (v), (vi), (vii) & (viii)] = Rs 64.876 ×
107

(C) Plant Overhead costs (includes for the following: general plant upkeep and
overhead, payroll overhead, packaging, medical services, safety and protection,
restaurants, recreation, salvage, laboratories, and storage facilities)

10% of Total Product Cost = 0.10×79.912×107 = Rs 7.9912×107

Manufacturing Cost = A+B+ C = 79.912×107+64.876×107+7.9912 ×107


= Rs 152.78×107

12.2.2 General Expenses

Includes administration expenses, distribution prices and also R&D costs

(A) Administration (2-6% of total product cost)

Consider 5% of total product cost = 0.05×79.912×107 = Rs 3.9956 ×107

(B) Selling and Distribution (2-20% of total product cost)

Consider 10% of total product cost = 0.10×79.912×107 = Rs 7.9912 ×107

(C) R & D (about 5% of total product cost)

Consider 5% of total product cost = 0.05×79.912×107 = Rs 3.9956 ×107

(D) Interests on financing (0-10% of total capital investment) Consider 5% of TCI =


0.05×161.1762×107 = Rs 8.0588×107
General Expenses = A + B + C + D = Rs 24.041×107

Total Product Cost = Manufacturing Cost + General Expenses = 152.78×107 +


24.041×107 = Rs 176.82×107

Table 36 : Total product cost evaluation

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Rate Component(Rs) Sub-Total(Rs) Amount(Rs)

(i) Depreciation of 10% 5.9556×107


machine
(ii) Depreciation of 5% 0.1417×107
building
(iii) Local Tax 3% 4.2046×107
(iv) Insurance 1% 1.4015×107

(v) Rent 10% 0.2834×107

(A) Fixed cost FC 11.987×107


Total Product cost 15% 79.912×107
(i) Raw material 30% 23.974×107
15% 11.987×107
(ii) Operating labour
15% 1.798×107
(iii) Direct supervisory &
clerical staff
(iv) Utilities 12% 9.5894×107
(v) Maintenance & repair 8% 11.212×107
(vi)Operating supplies 10% 1.1212×107
(vii) Laboratory charges 10% 1.1987×107
(viii) Patents & royalties 5% 3.9956×107
(B) Direct Cost DC 64.876×107
(B) Overheads 10% 7.9912×107

Manufacturing Cost
MFC 152.780×107
7
(i) Administration 5% 3.9956×10
(ii) Selling & Distribution 10% 7.9912×107

(iii) R & D 5% 3.9956×107

(iv) Interests 5% 8.0588×107

General GE 24.0410×107

Total Product cost


(MFC + GE) 176.820×107

13. PROFITABILITY ANALYSIS

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13.2 Gross Profit
Current selling price of 99.9% cinnamic aldehyde = Rs 650.00 / kg
Production capacity = 3400 ton/year = 34,00,000 kg/year
Thus, annual revenue = S.P. × sales quantity = Rs 650× 3,40,000 = Rs 2210000000
Gross profit = annual revenue – total product cost = Rs 2210000000- Rs 1768200000
= Rs 44,18,00,000
Let’s say income tax rate averages at 34% (of gross profit).
Tax paid = 0.34 × 44,18,00,000= Rs 15,02,12,000

13.2 Net Profit

Net Profit is the final operational income made by the industry after taking into account
various expenses.
Hence Net Profit = gross profit – tax = Rs 44,18,00,000- Rs 15,02,12,000= Rs 29,15,88,000

13.3 Rate of Return

Rate of Return is the rate at which amount invested as total capital in the industry is returned
through net profit of the industry.
Rate of Return = (Net Profit / Total Capital Investment) ×
100% = (29,15,88,000/1,61,17,62,000) × 100% = 18.09%

13.4 Payback Period

Payback period is the duration of time in which the fixed capital investment made in the
industry at the beginning is recovered through annual net profits (and depreciation claims).
All revenue made after this time gives rise to a net positive cash flow in the industry.
Payback Period = Fixed Capital Investment / (Net Profit + Depreciation) =
1,61,17,62,000/ (29,15,88,000+5,95,56,000) = 4.59 years

13.5 Break-Even Analysis


Let plant operate at ‘x’ fraction of its capacity which is its Break-Even Point (BEP) of 0
profit.
Revenue at BEP = Rs 650× 34,00,000× x = Rs 221,00,00,000×x

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Total fixed costs = fixed cost + overhead + general expenses
= Rs 11.987×107+ Rs 7.9912×107+ Rs 24.041×107= Rs 44.0192×107
Total direct costs = Rs 64.876×107 (at full capacity)
Direct costs at BEP = Rs 64.876×107× x

At break-even point: Revenue at BEP = Total fixed costs + Direct costs at BEP
(221×107 × x) = (44.019×107) + (64.876×107 × x)

On solving, we get, x = 0.282 = 28.2%

In terms of quantity, BEP = 0.4959 × 3.4 KTA = 1.687 KTA

Plant must operate at a minimum of 28.2% of its capacity to break-even.

(KTA: kilo tonnes per annum)

Table 37: Profitability Analysis Summary

Unit Selling Price Rs 650.00 per kg

Annual Production 34,00,000 kg/year


Annual Revenue (SPxProd) Rs 221,00,00,000
Annual Product Cost Rs 1,61,17,62,000
Gross Profit GP (Revenue-Cost) Rs 44,18,00,000

Income Tax (34%) Rs 15,02,12,000

Net Profit (GP-Tax) Rs 29,15,88,000


Rate of Return (ROR) 18.09%
Payback Period (PBP) 4.59 years
Break-Even Point 28.2% of full capacity

67
14. PLANT LOCATION AND LAYOUT

The location of the plant is a crucial parameter in the profitability of the project and in the
quest for future expansion. Various factors decide the location of a plant. For the production
of Cinnamic aldehyde, the plant location is selected as Haldia town in West Bengal. An
overview of some factors for selecting the location is given below.

1. Market availability:

An effort must be made to locate the plant quite close to the primary market, as this will
reduce transportation costs. Being near to Kolkata, where many food processing
industries are present, cinnamic aldehyde finds a market place.

2. Raw material availability:

Being a hub of process industries, obtaining the raw materials – benzaldehyde and
acetaldehyde will not be a problem.

3. Available transportation infrastructure:

Transport of materials and products is an important consideration in the selection of the


location. Haldia is well connected by railroads and highways. Along with that the
Kolkata sea port can also serve for transportation purpose.

4. Availability of labor:

A local pool of unskilled labourers, availability of skilled workers for plant maintenance
is a must for any chemical plant. Being excessively populated, there is an abundant
supply of labourers in this region.

5. Availability of utilities:

Water, power and fuel are extremely important raw material for the commissioning of a
plant. Water scarcity can adversely cripple the functioning of a plant, while power
shutdowns necessitate the use of generators, which add to the capital and running costs.
Hence these factors are of overriding importance. River Ganges flows close to Haldia.
Water and power from Damodar Valley Corporation can be used for production.

6. Effluent disposal:

68
Effluent disposal is an important parameter. Local regulations on the limits of toxic and
non- toxic wastes can be adhered to. Attempts must be made to recycle the wastewater;
else the treated effluent must be discharged into natural streams.
7. Local community considerations:

The proposed plant must fit into the general scheme of things of the community. The
community safety must not be compromised by the proximity of the plant site. Health
hazards can be kept to a low minimum and all safety precautions taken.

8. Political and strategic considerations:

Capital grants, tax considerations etc. are often given by the government to direct new
investments to preferred locations, such as areas of high employment. The availability of
such grants from the ruling party, Trinamool Congress is the overriding consideration in
site selection.

In view of the above considerations, Haldia, West Bengal is an apt choice for location of
plant. It is one of the top 25 global economic zones (20). Many chemical plants are located in
that region, which makes the source as well as the market very close and hence also saves on
transportation costs immensely.

The economic construction and efficient operations of a process unit will depend on how well
the plant and equipment specified on the process flow sheet is laid out. The chief factors to be
considered are enumerated below:

1. Economic considerations:
Adopting a layout that requires the least length of pipes and least amount of structural steel
work can minimize the cost of construction. This layout, however, may not be the best
arrangement for smooth operation.

2. Process requirements:
All the requirements should be fully considered to ensure that none of the requirements are
hampered.

3. Convenience of operation:
Equipment that needs frequent maintenance and monitoring like valves, sample points should
be located at convenient positions and height. Sufficient working space and headroom must
be provided to allow easy access of equipment.

i. Safety:
Blast walls may be providing to isolate potentially hazardous equipment and confine the
effects of an explosion. At least two escape routes for operators must be provided from each
level in the process building.

69
ii. Future Expansion needs:
Equipment must be suitably located so that it can be integrated into any future expansion
plan.

iii. General considerations:


Open structural steelwork buildings are normally used for process equipments. The
arrangement of major items of equipment will generally follow the sequence given on the
process flowsheet, with the columns and vessels arranged in rows and the ancillary
equipment, such as heat exchangers and pumps, positioned along the outer boundaries.

70
Fig 19 : Plant layout

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15. SAFETY & ENVIRONMENTAL ISSUES

15.1 Health and Safety Factors


Workers may be exposed to the organics like acetaldehyde, benzaldehyde and cinnamic
aldehyde. They should be monitored in a systematic program of medical surveillance that is
intended to prevent occupational injury and disease.
The program should include education of employers and workers about work-related hazards,
placement of workers in jobs that do not jeopardize their safety or health, early detection of
adverse health effects, and referral of workers for diagnosis and treatment. The occurrence of
disease or other work-related adverse health effects should prompt immediate evaluation of
primary preventive measures (e.g., industrial hygiene monitoring, engineering controls, and
personal protective equipment). A medical monitoring program is intended to supplement,
not replace, such measures. To place workers effectively and to detect and control work-
related health effects, medical evaluations should be performed: before job placement;
periodically during the period of employment; and at the time of job transfer or termination.

15.1.1 Exposure to cinnamic aldehyde

• Inhalation: Cinnamic aldehyde causes respiratory tract irritation and also harm the
nervous system. Symptoms may include headache, nausea, dizziness, drowsiness and
confusion. In case of contact, move victim to fresh air and call a doctor if victim feels
unwell.

• Skin Contact: Cinnamic aldehyde Causes skin irritation. May cause skin sensitization,
an allergic reaction, which becomes evident upon re-exposure to this material. The
highest non-irritating concentration of cinnamaldehyde was 0.5% in Vaseline and 1%
in acetone (guinea pig study by DSM Special Products). In humans, closed patch test
found 3% in petrolatum produced no irritation after 48 hours. 8% in petrolatum
produced severe irritation after 48 hours. A patch test in humans found a
concentration of 1% in petrolatum was sensitizing in 15 out of 16 persons. Another
human patch test found 68% positive reactions (50/73) when 5% cinnamaldehyde in
Vaseline was used. 21% positive reactions (15/71) when 2% cinnamaldehyde in
Vaseline was used.

72
• Eye Contact: Cinnamic aldehyde may cause mild irritation in eye on contact. Flush
contaminated eye with lukewarm gently flowing water for 5 minutes holding the
eyelid open. A doctor should be consulted if irritation persists.

• Ingestion: Cinnamic aldehyde causes gastrointestinal irritation with nausea, vomiting


and diarrhea. Low hazard for usual industrial handling. If swallowed, do not induce
vomiting unless directed to do so by medical personnel. Never give anything by
mouth to an unconscious person.
• Carcinogenicity: Not known to cause cancer.
▪ International Agency for Research on Cancer (IARC): Group 3 - Not
classifiable as to its carcinogenicity to humans. (22)
▪ American Conference for Governmental Industrial Hygienists
(ACGIH): A4 - Not classifiable as a human carcinogen (23)

15.1.2 Fire hazards


As in any fire, wear a self-contained breathing apparatus in pressure-demand, MSHA/NIOSH
(approved or equivalent), and full protective gear. During a fire, irritating and highly toxic
gases may be generated by thermal decomposition or combustion. Vapours are heavier than
air and may travel to a source of ignition and flash back. Vapours can spread along the
ground and collect in low or confined areas.

• Extinguishing Media: Use extinguishing media most appropriate for the surrounding
fire.
• Flash Point: 71 deg C ( 159.80 deg F)
• Auto ignition Temperature: Not applicable.
• Explosion Limits, Lower: Not available.

• NFPA Rating: (estimated) Health: 2; Flammability: 2; Instability: 1

15.1.3 Handling and storage

• Handling: Wash thoroughly after handling. Remove contaminated clothing and wash
before reuse. Use with adequate ventilation. Avoid contact with eyes, skin, and
clothing. Keep container tightly closed. Avoid ingestion and inhalation.

• Storage: Store in a tightly closed container. Keep refrigerated. (Store below


4°C/39°F.)
• Chemical Stability: Stable under normal temperatures and pressures. Thickens on
exposure to air.

73
• Conditions to Avoid: Excess heat, prolonged exposure to air, excess light.
• Incompatibilities with Other Materials: Strong oxidizing agents, strong bases.

• Hazardous Decomposition Products: Carbon monoxide, irritating and toxic fumes and
gases, carbon dioxide.
• Hazardous Polymerization: May occur.

15.2 Pollution Prevention

The sources of wastes are classified as follows:


• Losses of oil (and hydrocarbons in general)
Such losses are caused mainly by entrainment, emulsification and to lesser extent,
dissolution of hydrocarbons in an aqueous phase in all operations involving contact
between hydrocarbons and water and by inadvertent leakage from equipment and
piping.

• Irreducible wastes generated as a separation of unwanted impurities in the processing


The impurities which originally comes with crude oil are often created during refining
are converted to useful and commercially viable products such as ammonia, sulphur,
phenolics and metals.

• Oily sludges: Oily sludges are stable emulsions formed through emulsification of oil
with water usually in the presence of suspended fines. Raw watery sludges are filtered
using pressure belt filter press or are centrifuged to remove solids which destabilize
the emulsion, causing it to separate into three phases: oil, water and dewatered
sludges. The dewatered sludge can be further treated to recover the oil using either
solvent extraction technique or thermal processing.

• Spent caustics: Solutions of NaOH are used primarily as catalyst and to wash the
hydrocarbon products or intermediates. The phenolic and sulphide spent caustics
should be segregated in order to enable recycling.
• Waste water
Wastewater is generated due to mainly the following streams: Flash separation outlet
and process water.

74
10. REFERENCES

[1] Industrial preparation method of high-yield cinnamaldehyde , Google patents,


Application No- CN 201210140439, published on Oct 10, 2012

[2] Shreve’s Chemical Process Industries, Perfume & Fragrance Industry, Fifth edition-2012
Page – 262.

[3] Kenichi Mori, Shinji Fujita, Nao Funakoshi, Tadashi Takemoto -U.S. application Ser.
No. 10/295,997, filed Nov. 18, 2002, U.S. Pat. No. 6,965,055, Continuation of International
Application Ser. No. PCT/JP01/03545, filed on Apr. 24, 2001

[4] Mia T. Casale, Aviva R. Richman, Matthew J. Elrod, Rebecca M. Garland, Melinda R.
Beaver, Margaret A. Tolbert, Kinetics of base -catalyzed aldol condensation reactions of
aliphatic aldehydes, Atmospheric Environment 41 (2007) 6212–6224

[5] Rawia. S.Hassan , Gurashi.A. Gasmelseed, B. A. Karama, and A.E Musa, A short-Cut
Method for Designing Multi-Component Fractionation Column, Journal of Applied and
Industrial Sciences, 2013, 1 (3): 44-48, filed on June 11, 2013

[6] De Maré, G.R.; Lehman, T.; Termonia, M., The vapour pressure of benzaldehyde between
273 and 376 K, The Journal of Chemical Thermodynamics, 1973, 5, 6, 829-832.
[doi:10.1016/S0021-9614(73)80044-8]

[7] Stull, Daniel R., Vapor Pressure of Pure Substances. Organic and Inorganic Compounds,
Ind. Eng. Chem., 1947, 39, 4, 517-540. [doi:10.1021/ie50448a022]

[8] Martin Iggland, Marco Mazzotti, Introduction to Chemical Engineering for Lecture 7: Flash
Distillation, ETH Zurich, Institute of Process Engineering, Sonneggstrasse 3, CH-8092 Zurich,
Switzerland, published in 2015

[9] Cutler, C.R. & Finlayson, S.G. Design Considerations for a flash column multivariable
constraint controller. 23-30. 10.1016/b978-0-08-035735-5.50008-5. Published in 1989

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