Extraction of Valuable Products from Rose and Marigold

Project report submitted to

Visvesvaraya National Institute of Technology, Nagpur

Bachelor of Technology
In Chemical Engineering

by

Eashan Bhat (BT17CME025) Atharva Sarode (BT17CME017)

Suzana John (BT17CME074) Ujwal Pimpalkar (BT17CME081)
Sahil Jikar (BT17CME064) Rebecca D’Souza (BT17CME057)

under the guidance of

Dr. Sachin Mandavgane

Department of Chemical Engineering

Visvesvaraya National Institute of Technology
Nagpur 440 010 (India)

2020

© Visvesvaraya National Institute of Technology (VNIT) 2020

 Department of Chemical Engineering
Visvesvaraya National Institute of Technology, Nagpur

Declaration
We, hereby declare that this project work titled “Extraction of Valuable Products from Rose
and Marigold” is carried out by us in the Department of Chemical Engineering of Visvesvaraya
National Institute of Technology, Nagpur. The work is original and has not been submitted
earlier whole or in part for the award of any degree/diploma at this or any other Institution /
University.
Date: 20-06-2020

Sr. No. Enrolment No. Names Signature

1 BT17CME025 Eashan A. Bhat

2 BT17CME017 Atharva D. Sarode

3 BT17CME074 Suzana M. John

4 BT17CME081 Ujwal V. Pimpalkar

5 BT17CME064 Sahil A. Jikar

6 BT17CME057 Rebecca M. D’Souza

Acknowledgment
We would like to express our heartfelt gratitude to our respected professor Dr. Sachin
Mandavgane who helped us a lot in understanding and analysing the project helped us with
utter generosity in every possible way and put us on a unique journey in learning and thinking
differently.
THANK YOU, SIR!
 Certificate
This is to certify that the project titled “Extraction of Valuable Products from Rose and
Marigold”, submitted by Eashan Bhat, Atharva Sarode, Suzana John, Ujwal Pimpalkar,
Sahil Jikar and Rebecca D’Souza is in the fulfilment of the requirements for the evaluation
of Innovative Design Course at the Department of Chemical Engineering, VNIT Nagpur. The
work is comprehensive, complete and fit for final evaluation.

Dr. Sachin Mandavgane

Associate Professor, Department of Chemical Engineering,
VNIT, Nagpur.

Head, Department of Chemical Engineering,

VNIT, Nagpur.
Date: 20-06-2020
ABSTRACT
This project is aimed to understand how one can effectively utilise flower waste which is
usually generated from temples, flower markets, and other sources. Two commonly found
flowers are taken into consideration in this project: Rose and Marigold. The primary focus is
on the extraction of different products that are of use from these flowers. Particularly, lutein
and flavonoids from Marigold and rose water and rose oil from Rose. Lutein is used in cataract
treatments and is known as an ‘eye vitamin’. An extensive study was conducted in the most
effective way to extract lutein from Marigold with minimal by-products. A process flow
diagram was formulated which includes the addition of different chemicals and mixing in
reactors along with the processes of filtration, and crystallisation. The by-product of this whole
process is flavonoids which can also be converted into a separate product. The recovery of the
chemicals used is also mentioned along with the process flow diagram. When it comes to rose,
the two products can be extracted by different methods. Conveniently, when it comes to steam
distillation, rose oil is the main product while rose water is the by-product. Rose oil can also
be generated through the process of Solvent extraction or CO2 Extraction. However, rose water
cannot be obtained from these particular processes. Other than these products, these flowers
are also ardently used in various ayurvedic treatments.

I
List of Figures
Sr. No. Title Page No.
1. Flow chart of products available from rose 3
Process Flow Diagram for Extraction of Rose oil
2. 3
and Rose water using Steam distillation
3. Flow chart of products available from marigold 7
Process Flow Diagram for Extraction of Lutein
4. 7
using Saponification
5. Flow chart of Ayurvedic uses 11

List of Figures
Sr. No. Title Page No.
1. Rose Oil Extraction Calculations 4
2. Lutein Extraction Calculations 8

II
INDEX
Sr. No. Title Page No.
A. Field Visit 1
B. Stakeholders 1
C. Extraction of Rose Oil 2
1. Introduction 2
2. Uses and Significance 2
3. Method of Extraction 2
4. Calculations 3
D. Extraction of Lutein 6
1. Introduction 6
2. Uses and Significance 6
3. Method of Extraction 7
4. Calculations 8
E. Flowers in Ayurveda 11
1. Importance of Rose 11
2. Importance of Marigold 12
F. Conclusion 13
G. References 13
H. Details of Meeting 14

III
FIELD VISIT
On Wednesday 11/03/2020, we paid a visit to the flower market in Sitabuldi, Nagpur and
spoke to a few flower vendors regarding their sales and the waste generated.
We noted down the following observations
i.) The most common flowers sold are roses and marigolds.
ii.) The vendors procure them in huge quantities, i.e., in the range of 100-200 kgs.
iii.) On a daily basis, roses sell out almost completely.
iv.) Of the total quantity, 60% of the flowers get sold and the remaining 40% goes to
waste which is then picked up from the dump the following day.

STAKEHOLDERS
We identified the following Major stakeholders while solving this issue.
i.) Farmer
ii.) Vendor
iii.) Consumer
iv.) Transporter
v.) Garbage Collector
vi.) Oil Producers/ Manufacturers

1
EXTRACTION OF ROSE OIL
Introduction
Rose oil (rose otto, attar of rose, attar of roses or rose essence) is the essential oil extracted
from the petals of various types of rose. Rose ottos are extracted through steam distillation,
while rose absolutes are obtained through solvent extraction, the absolute being used more
commonly in perfumery. Even with their high price and the advent of organic synthesis, rose
oils are still perhaps the most widely used essential oil in perfumery.
The most common chemical compounds present in rose oil are: citronellol, geraniol,
nerol, linalool, phenyl ethyl alcohol, farnesol, stearoptene, α-pinene, β-pinene, α-terpinene,
limonene, p-cymene, camphene, β-caryophyllene, neral, citronellyl acetate, geranyl acetate,
neryl acetate, eugenol, methyl eugenol, rose oxide, α-damascenone, β-damascenone,
benzaldehyde, benzyl alcohol, rhodinyl acetate and phenyl ethyl formate.
Uses and Significance
When applied directly to the skin, skin care products containing rose essential oil are
purported to hydrate dry skin, clear acne, reduce signs of aging, minimize the appearance of
scars, and help with conditions such as eczema and rosacea.
Rose essential oil is typically touted as an aromatherapy remedy for the following health
concerns:
• Anxiety
• Depression
• Headaches
• Menopausal symptoms
• Menstrual cramps
• Migraines
In addition, rose essential oil is said to enhance libido, reduce stress, stimulate circulation,
sharpen memory, and boost mood.
Method of Extraction
Steam distillation is used for extraction of rose oil and it gives rose water as by-product.
The setup consists of three major equipment, viz., i) Steam distillation column, ii) Heat
Exchanger (Condenser) and iii) Decanter (Separator).

2
 Fig. 1 - Flow chart of products available from rose

Rose petals are cleaned with water and put in the distillation column. Saturated steam is
passed through the column and the oil is evaporated and it escapes from the petals and is carried
along with the steam. The steam is passed through a shell and tube heat exchanger to condense
the vapours. These vapours are fed to a decanter to separate the organic and aqueous phases,
the organic phase is concentrated rose oil and the aqueous phase is rose water.
Rose oil content is about 0.0033% w/w in the petals. Extraction rates of up to 80-90%
can be easily achieved using steam distillation.

Fig. 2 - Process Flow Diagram for Extraction of Rose oil and Rose water using Steam
distillation
Calculations
A TK Solver model was prepared for the process by assuming several parameters and
ideal conditions. The model can calculate the approximate amount of rose oil which can be
produced from the amount of waste flowers. It can also calculate the tentative size of equipment

3
required as per the input provided. The model is designed to calculate the steam required in the
distillation column as well as the amount of cooling water required in the shell and tube heat
exchanger. It can also calculate the time required for the separation of oil from water.
A sample calculation is shown below:
Table 1 - Rose Oil Extraction Calculations
Variable Symbol Input Output Unit
General information
Average temperature of cooling fluid T 37.5 oC
Atmospheric Pressure Patm 1 atm
Petal and steam details
Mass of petals mpetal 100 kg/h
Percent of product oil extracted mext 1
Mass flow rate of product mp .037 kg/h
Mass flow rate of steam mw .001 kg/s
Density of product oil ρp 700 kg/m^3
Steam properties
Heat Duty Q .154 kW
Latent heat of evaporated mixture Δh 15000 kJ/kg
Mass flow rate of cooling water m 5.311 kg/h
Specific heat of cooling fluid Cp 4.184 kJ/(kg*K)
Outlet temperature of cooling fluid T1 50 oC
Inlet temperature of cooling fluid T2 25 oC
Condensing temperature of product oil Tc 80 oC
Density of cooling fluid ρ 993.147 kg/m^3
Viscosity of cooling fluid μ .00068 Pa*s
Thermal conductivity of cooling fluid k .627 W/(m*K)
Basic heat exchanger data-1
Assumed overall heat transfer Uass 400 W/(m^2*K)
Heat transfer surface area
coefficient Ah .0074 m^2
Logarithmic Mean Temperature LMTD 52.460 oC
Difference Heat exchanger design parameters-1
Outer diameter of tubes Do 16 mm
Inner diameter of tubes Di 12 mm
Length of tubes L 5 m
Number of tubes (to be considered) n 0.03
No. of tubes N 1
Basic heat exchanger data-2
Total cross-sectional area of tubes Ac .00008 m^2
Heat transfer coefficient of condensing hc 10000 W/(m^2*K)
fluid in shell

4
Heat transfer coefficient in tube h 861.78 W/(m^2*K)
Fouling coefficient of tube fluid hf 5000 W/(m^2*K)
Heat exchanger design parameters-2
Velocity of tube fluid v .098 m/s
Reynolds number in tube Re 1859.902
Prandtl number in tube Pr 5.759
Nusselt number in tube Nu 16.914
Thermal conductivity of material km 50 W/(m*K)
Overall heat transfer coefficient U 649.457 W/(m^2*K)
Decanter details
Total volume of mixture vtotal .1004 m^3
Length of decanter Ls .1597 m
Viscosity of continuous phase μm .0068 Pa*s
Height of denser phase Z1 .5 m
Outlet of denser phase Z2 .711 m
Outlet of less dense phase Zt .8 m
Time of separation t 8.318 s

5
EXTRACTION OF LUTEIN
Introduction
Lutein is one such important member of carotenoid (xanthophyll) family widely present
in marigold flower, spinach; kale3,4 used as functional food as it has vivid applications from
poultry to opthalmo-pharmacy industry. Lutein and its isomer zeaxanthin are the oxidation
products of carotenoids in plants. Both lutein and its stereoisomer zeaxanthin are distinguished
from other carotenoid compounds based on the chemical composition of hydroxyl group
attachments to their structures.
Many people think of lutein as "the eye vitamin." It is commonly taken by mouth to
prevent eye diseases such as an eye disease that leads to vision loss in older adults (age-related
macular degeneration or AMD), and cataracts. There is no good scientific evidence to support
the use of lutein for other conditions.
Uses and Significance
Lutein is likely effective for:
• Lutein deficiency. Taking lutein by mouth is effective for preventing lutein
deficiency.
And possibly effective for:
• An eye disease that leads to vision loss in older adults (age-related macular
degeneration or AMD). People who eat higher amounts of lutein in their diet seem
to have a lower risk of developing AMD. But people who already eat high amounts
of lutein might not benefit from increasing their intake even more. Taking lutein
supplements for up to 36 months can improve some symptoms of AMD. Greater
improvement in symptoms might be seen when lutein is taken for at least 1 year at
doses above 10 mg, and when it is combined with other carotenoid vitamins. Lutein
does not seem to keep AMD from becoming worse over time.
• Cataracts. Eating higher amounts of lutein is linked with a lower risk of developing
cataracts. Taking supplements containing lutein and zeaxanthin reduces the risk of
developing cataracts that require surgical removal in people who eat low amounts
of lutein and zeaxanthin as part of their diet. Also, taking lutein supplements seems
to improve vision in older people who already have cataracts and do not already
consume a lot of lutein and zeaxanthin.

6
 • Cancer that starts in white blood cells (non-Hodgkin lymphoma). People who eat
higher amounts of lutein in their diet or take lutein supplements might have a lower
chance of developing non-Hodgkin lymphoma.
Method of Extraction
Saponification reaction is used for extraction of Lutein. The setup consists of four major
equipment, viz., i) Stirred Tank Reactor, ii) Leaf Filter, iii) Decanter (Separator) and
iv) Crystallizer. Stirred Tank Reactor in the process can also be used as crystallizer.

Fig. 3 - Flow chart of products available from marigold

Marigold petals are cleaned, dried and crushed. These crushed petals are put in the reactor
vessel along with solvents (any strong alkali and lower alcohol). The saponification reaction is
allowed to take place for sometime and the mixture is put through a leaf filter to separate out
the petals. The liquid which is mixture of solvent with Lutein dissolved in it is passed through
a decanter to separate the alkali and alcohol which contains Lutein. The alcohol is put in a
crystallizer to remove the alcohol and obtain pure Lutein.

Fig. 4 - Process Flow Diagram for Extraction of Lutein using Saponification

7
 Lutein content is approximately 0.001% w/w in the petals. More than 90% extraction rate
can be easily achieved using the saponification reaction.
Calculations
A TK Solver model was prepared for the process by assuming several parameters and
ideal conditions. The model can calculate the approximate amount of Lutein which can be
produced from the amount of waste flowers. It can also calculate the tentative size of equipment
required as per the input provided. The model is designed to calculate the amount of solvents
required in the reactor. It can also calculate the time required for filtration as well as the
separation of alcohol from alkali.
A sample calculation is shown below:
Table 2 - Lutein Extraction Calculations
Variable Symbol Input Output Unit
Impeller Shape
Type of Impeller Impeller 6-blade turbine
Power constant kt 5.75
Heat transfer constant a .74
Heat transfer constant b .67
Heat transfer constant c .33
Vessel Fluid Properties and Details
Density of vessel fluid ρ 850 kg/m^3
Viscosity of vessel fluid μ 80 mPa*s
Specific Heat of vessel fluid Cp 2.65 kJ/(kg*K)
Thermal Conductivity of k .4 W/(m*K)
Inlet
vesseltemperature
fluid of tank fluid Tin 20 oC
Outlet temperature of tank Tout 50 oC
Average
fluid temperature of tank T 35 oC
fluid Petal and mixture details
Density of petals ρpetal 200 kg/m^3
Density of mixture in vessel ρmix 741.667 kg/m^3
Volume of solvents vsolvent 5 m^3
Volume of crushed petals vpetal 1 m^3
Total volume of mixture vtotal 6 m^3
Viscosity of mixture μmix 139.140 mPa*s
Volume fraction of solids Φ .167
Vessel Design Parameters
Volume of reactor vreactor 7.5 m^3
Diameter of tank Dt 2.121 m

8
Height of tank H 2.121 m
Speed of Rotation of impeller n 120 RPM
Diameter of impeller Da .707 m
Power required by impeller P 6.034 kW
Reynolds number in vessel Re 10627.489
Prandtl number in vessel Pr 921.805
Nusselt number in vessel Nu 3509.710
Heat transfer coefficient in h 1985.159 W/(m^2*K)
vessel Jacket Fluid Properties
Jacket fluid Fluid_J 'Water
Atmospheric Pressure Patm 1 atm
Average temperature Tj 35 oC
Inlet temperature of jacket Tjin 50 oC
Outlet
fluid temperature of jacket Tjout 20 oC
Density of jacket fluid
fluid ρj 994.032 kg/m^3
Viscosity of jacket fluid μj .719 mPa*s
Specific Heat of jacket fluid Cpj 4.179 kJ/(kg*K)
Thermal Conductivity of kj .623 W/(m*K)
Mass
jacketflow
fluidrate of jacket fluid mj 3233.821 kg/h
Jacket Design Parameters-1
Diameter of jacket half coil Dc 200 mm
Cross-sectional of jacket half- Aj .0157 m^2
Equivalent
coil diameter of jacket De 122.203 mm
Number
half coil of loops of half coil N 5
Length of jacket half coil L 3.142 m
Jacket Design Parameters-2
Velocity of jacket fluid vj 207.107 m/s
Reynolds number in jacket Rej 34975107
Prandtl number in jacket Prj 4.823
Nusselt number in jacket Nuj 41901.144
Heat transfer coefficient in hj 213726.087 W/(m^2*K)
jacket Overall Design Details
Material of construction Material Low_Carbon_Steel
Thermal
ovessel conductivity kv 55.383 W/(m*K)
Roughness factor ε .045 mm
Outer diameter of vessel Dov 1.51 m
Inner diameter of vessel Div 1.5 m
Overall heat transfer Uj 1660.151 W/(m^2*K)
coefficient Jacket Details
Friction factor in jacket fj .0039
Pressure drop in jacket ΔPj 1713.67 Pa

9
 Filter Details-1
Time of filtration tf 1285.467 s
Resistance due to cake Kp 63.848
Resistance due to filter media β 22.701
Filter Details-2
Area of filter Afilter 1 m^2
Concentration of solid in feed Cs 33.334 kg/m^3
Specific cake resistance α 1350000 m^3/kg
Resistance of filter media Rm 16000000 m^-1
Pressure drop in filter ΔPf 1 atm
Decanter details
Time of separation ts 333.937 s
Length of separator Ls 12.4725 m
Height of denser phase Z1 .5 m
Outlet of denser phase Z2 .668 m
Outlet of less dense phase) Zt .7 m
Density of organic phase ρo 800 kg/m^3
Density of aqueous phase ρa 950 kg/m^3

10
FLOWERS IN AYURVEDA
Importance of Rose
For thousands of years, Ayurvedic healers have been using the rose plant in herbal
remedies, teas, oils and skincare formulations. It can be used as dried, preserved, juiced,
distilled, or an as powder or tincture.
• Rose essential oil is great for aromatherapy and for use in beauty products.
• Rosewater is delicious in food and beverage recipes as well as to soothe the skin.
• Rose hydrosol is a cooling and hydrating skin toner.
• Rose petal jam is a sweet uplifting treat.
• Rose tea has wonderful benefits for soothing the mind, heart and throat.
• Rose powder is useful in herbal formulas, skin products and culinary recipes.

Fig. 5 - Flow chart of Ayurvedic uses

11
Importance of Marigold
Applied externally marigold has long been an effective treatment for skin problems
such as cuts, itching, cracked skin, sunburn and insect bites, and is used in many skin
cosmetics. It is also recommended as a treatment for mouth infections. A number of
investigations into the healing powers of marigold flowers have highlighted not only their
anti-inflammatory and antibacterial properties, but also their ability to fight off infection
caused by viruses and parasites. Research in Italy in 1994 found that triterpenoids in the plant
are responsible for its anti-inflammatory powers, and trials have shown that these compounds
can help to ease swelling caused by fluid retention. Marigold is also reputed to be capable of
staunching bleeding and calming muscular spasms.
• Marigold tea: Dried flowers of the plant can be used to make tea. The best way to
use marigold is in the form of tea, by drying only the flowers and using them to
make tea.
• For making tea, boil water and add a tablespoon of flowers to the pot of tea and let
it steep. The tea purifies blood, and therefore should be had regularly. Marigold tea
is a good remedy for cases of diarrhoea, liver problems, herpes and glandular
swelling, hepatitis, in expelling worms, and intestinal inflammation.
• Marigold tea and horsetail could be used in equal proportions for cracked feet,
ulcerated legs, cancer and tumour growths, and non-healing wounds.
• Marigold ointment: To make an ointment, chop some fresh flowers, and add it to
coconut oil. Heat lightly and allow it to cool. The ointments are an excellent remedy
for Athletes feet, varicose veins, nose scabs, eczema, and skin infections.
• A cold infusion conducted by cooling marigold tea in a refrigerator, dipping cotton
pad into the resulting solution and placing it on the eye, and replacing the pad often
when required, is good for eyes.
• Marigold tincture is also excellent in healing burns, impetigo, and stings. It is
wonderful in the treatment of corns, warts and calluses, while the flowers are used
in the treatment of several skin conditions ranging from eczema to varicose ulcers.
• The distillate from the flower can be used to treat asthma. 4-5 drops is added with
a glass of hot water and consumed.

12
CONCLUSION
A simple user-friendly TK Solver model was prepared for calculating the approximate
amount of Rose Oil and Lutein which can be extracted from Rose and Marigold, respectively.
Both the models have the capability to design simple pilot plant for the purpose of extraction.
This project can be used to manage flower waste generated in the cities effectively and make
useful profitable products from them.

REFERENCES
Research Papers
1. “Combined process of reaction, extraction, and purification of lutein in marigold flower by
isopropanol–KOH aqueous two-phase system” by Tingting Wang, Juan Han, Yue Tian, Dan
Zhang, Yun Wang, Yingchun Wu and Liang Ni
2. “Recovery of water-soluble constituents of rose oil using simultaneous distillation–
extraction” by Mohammad H. Eikani, Fereshteh Golmohammad, Soosan Rowshanzamir
and Mehdi Mirza
Websites
1. https://en.wikipedia.org/wiki/Rose
2. https://en.wikipedia.org/wiki/Tagetes
3. https://en.wikipedia.org/wiki/Rose_oil
4. https://en.wikipedia.org/wiki/Lutein
5. https://www.newdirectionsaromatics.com/blog/articles/how-essential-oils-are-
made.html#steam-distillation
6. https://www.planetayurveda.com/library/marigold-tagetes-erecta-uses-and-health-
benefits/
7. http://www.drvikram.com/marigold.php
8. http://www.ayurvedictalk.com/the-wonders-of-marigold/1032/
9. https://www.bimbima.com/ayurveda/medicinal-use-of-gendamarigold/515/
10. https://www.webmd.com/vitamins/ai/ingredientmono-754/lutein
11. https://www.verywellhealth.com/the-benefits-of-rose-essential-oil-
88790#:~:text=When%20applied%20directly%20to%20the,such%20as%20eczema%
20and%20rosacea

13
DETAILS OF MEETING
1. First Meeting – 5th April 2020, for 40 minutes
Narrow down the list of raw materials and products and find more information
regarding the processes.
2. Second Meeting – 13th April 2020, for 40 minutes
Make a Flowsheet of the processes and get the details of Ayurvedic uses.
3. Third Meeting – 4th May 2020, for 50 minutes
Do energy balance and material balance for the processes and get information
regarding the design of Equipment.
4. Final Meeting – 8th June 2020, for 30 minutes
Refine the calculation model and start preparing the report.

14