DEMOCRATIC AND POPULAR ALGERIAN REPUBLIC

MINISTRY OF HIGHER EDUCATION AND RESEARCH

SCIENTIFIC

Yahia Fares University of Medea

Faculty of Technology

Bachelor's Thesis
Field: Process Engineering

THE EXTRACTION METHODS OF

ESSENTIAL OILS

Presented by:
HAZEDJE Noudjoud

MOUZAOUI Kouather

Proposed and Directed by:

Mr. LETTREUCH H

Promotion 2023

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 Acknowledgments

We thank above all, "God" the Almighty, for having

permission to present this modest work.
We would like to express our heartfelt thanks and our deep
Thanks to our promoter Mr. LETTREUCH HICHEM for his
availability, assistance throughout the entire course of this project. Thanks to his/her

devotion, scientific advice and monitoring, we were able to carry out

term our work.

Our sincere thanks go to all the teachers.

from the Department of Process Engineering who offered us all this
to know.

Finally, we thank all those who contributed directly or indirectly to

the completion of this thesis.

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 We thank them with all our heart
JK

Dedication
I dedicate this work:
To my very dear Mother
Affable, honorable, amiable: You represent for me the
symbol of excellence in kindness, the source of tenderness and the example
the devotion that has constantly encouraged me and prayed for me
I love you, mom.
To my Father

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NOUDJOUD

KAOUTHER

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Resume

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 List of figures

Figure I.1: Structure of some arenas derived from phenylpropane.

Figure II.1: Diagram of the steam drive assembly.

Figure II.2: Schematic diagram of hydro-distillation setup.

Figure II.3: diagram of the CO extraction setup2supercritique.

Figure II.4: Mechanisms of heat and mass transfer in extraction

classic and microwave of natural products.

List of tables

Table I.1: Properties of some essential oils.

Table I.2: Localization of essential oils from some plants.

List of abbreviations

Essential oil.

°C : Celsius degree.

MHz: Megahertz.

GHZ: Giga hertz.

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CO2Carbon dioxide.

Mm: Millimeter.

Essential oils.

Summary

Thank you

Dedications

Resumes

List of figures

List of tables

List of abbreviations

GENERAL INTRODUCTION……………………………………..01

Chapter I: General information on essential oils.

I.1 Definition…………………………………………………………..03

I.2 The role of essential oils……………….…………………….03

I.3 Composition of essential oils...........................03

I.3.1 terpenic compounds..................................03

I.3.2 Aromatic Compounds.........................05

I.3.3 Compounds of diverse origin..............................07

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I.4 Properties of essential oils............................08

I.4.1 Physico-chemical properties……………………………...…08

I.4.2 Biological properties………………………………………..08

I.4.3 Pharmacological properties…………………………...……………….08

I.4.4 Properties of some essential oils…………………..09

I.5 Localization of essential oils……………………………….10

Chapter II: Methods of extracting essential oils.

II.1 The methods of extracting essential oils....................12

II .1.1 Water vapor training……………………………….12

II .1.2 Extraction by hydrodistillation……………………………...13

II .1.3 Extraction by CO2supercritique........................14

II .1.4 Microwave-assisted extraction………………………….15

General conclusion……………………………………………………...18

Bibliographic References......................................................19

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 Chapter I: Generalities on essential oils

General introduction

Under the influence of solar radiation, plants synthesize compounds

fragrant: essential oils.

Often extracted by a distillation process, they constitute the material.

premiere of aromatherapy.

Essential oils are most often the concentrated extracts from plants.
aromatic (plants that contain enough aromatic molecules in one or
several of its reproductive organs). [1]

The objective of this mini project is to explore some methods of oil extraction.
essential oils, steam extraction, hydro-distillation extraction, extraction with
CO2supercritique, microwave-assisted extraction.

The first chapter of this mini project presents general information on oils.
essentials.

And in the last chapter, we present the methods of oil extraction.

essential.

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Chapter I: Generalities on Essential Oils

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 Chapter I: Generalities on essential oils

I.1 Definition of essential oils:

Essential oils are viscous liquids that range in color from pale yellow to orange and
of an aromatic smell, spicy at the base with a rising aldehyde scent at the top.
These are 18 products of generally complex composition containing principles
volatile compounds found in plants that are more or less modified during the
preparation.
The French Association for Standardization (AFNOR) defines essential oils
as a "product" obtained from a plant raw material, either by
steam distillation training, either by hydro distillation. The essential oil is
separated from the aqueous phase by
Physical processes.
According to ISO 9235 standard, natural origin aromatic raw materials
vocabulary, an essential oil is defined as a 'product obtained from
a raw material of plant origin, after separation of the aqueous phase by
physical processes: either by steam training or by
mechanical processes from the epicarp of
Citrus, either by dry distillation.

I.2 Role of essential oils:

Essential oils have four main roles:

Attraction of pollinating insects

Inhibits the germination of the seed of species that share the same space
Protection of the plant against predators (insects)

Heat exchanges in capillary phenomena

I.3 Composition of essential oils:

To date, more than 3000 constituents have been isolated from essential oils.
the latter are complex and highly variable mixtures of constituents that
belong to two groups characterized by distinct biogenetic origins:
Terpenic compounds.
Aromatic compounds derived from propylene phenyl

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 Chapter I: Generalities on essential oils

I.3.1 Terpenic compounds:

Terpenes are present in plants, of which they are often the constituents.
fragrance substances, which have been known for a long time to be extracted in the form of oils

essentials
Many terpenic compounds are used in perfumery or in various
other industries. Terpene hydrocarbons have the empirical formulas C10H16(mono
terpenes), C20H32(di terpenes), C30H48(three terpenes), or C40H64(tetra terpenes)[6].
Oxygenated terpenic compounds have carbon chains similar to those of
hydrocarbons, acyclic or cyclic, but are sometimes less unsaturated than the
corresponding hydrocarbons. Mono terpenes are particularly found as
odorant constituents of plant essences

Myrrh cen (laurel)

Limonene (lemon, pine, mint)

I.3.2 Aromatic compounds:

The aromatic compounds deriving from phenylpropane (C6-C3) are frequent that the
terpenes in essential oils and they can also contain different functions. They are very
often allyles and propylphenols, we have gathered in figure 3 some
examples of them encountered in essential oils. This class includes compounds
odorants such as vanillin, anethole, eugenol... and methylchavicol or estragole. They

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 Chapter I: General Information on Essential Oils
are frequently found in the essential oils of Apiaceae (anise, fennel, parsley, etc...) and are
characteristics of those of vanilla, tarragon, basil....and clove.
They stand out from each other by:
The number and position of hydroxyl and methoxy groups.
The position of the double bond in the side chain, allylic or propenylic.
The oxidation degree of the aliphatic chain (alcohol, aldehyde, ketone, or acid...)
[7].

E-Anethole

Eugenol

Anisaldehyde

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 Chapter I: Generalities on Essential Oils

I.3.3 compounds of various origins:

These are products resulting from the transformation of non-volatile molecules. These
compounds contribute to the fruit aromas. Considering their preparation method, the
concrete and absolute can contain them. The same is true for the oils
essential, when trainable by water vapor (Bruneton, 1999). Figure: 3

Estragole Methyl cinnamate

Figure 3: Structure of some arenas derived from phenylpropane

I.4 Properties of essential oils:

I.4.1 Physico-chemical properties:
Essential oils have a number of physicochemical properties.
known are the following:
. At ambient temperatures, they are generally liquid; whereas they are
Volatiles at high temperatures, it is their volatility that distinguishes them from fixed oils.
such as olive oil and sweet almond oil.
. Intense diffusion and penetration power.
. They are colorless to pale yellow, but there are exceptions.
. They usually have a density lower than that of water (d<1), but there are
exceptions (clove essential oils).
. They are endowed with a rotational power justified by the presence of molecules.
asymmetric.
. They generally have a high refractive index.
. They are poorly soluble in water (can be carried by water vapor).

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 Chapter I: Generalities on essential oils

. They are soluble in common organic solvents, in fats.

(liposoluble), and in alcohols.
. Sensitive to oxidation; they also tend to polymerize to form
resinous products; this limits their preservation.

I.4.2 Biological Properties:

Only a few biological properties are recognized and come from use.
traditional validated: It concerns the antiseptic and digestive stimulating properties.
the inside and outside, as well as healing and analgesic properties. Others
properties are claimed and are subject to prescriptions under the full responsibility of the
prescribing physician.

I.4.3 Pharmacological properties:

Essential oils are complex mixtures of constituents in proportion

often variable, hence the difficulty of conducting rigorous pharmacological studies.
However, some main properties can be identified, A large number
essential oils have "digestive" properties or properties
antispasmodics, sedatives, irritants

I.4.4 Properties of some essential oils:

Essential oils The plants Properties

Mandarin Antiseptic, digestive,
tonic, sedative
antispasmodic
refreshing, soothes and
drain

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 Chapter I: Generalities on essential oils

Rosemary Toning, against the

rheumatism
respiratory problems
wrinkles and baldness.

Anti-inflammatory,
antidepressant, astringent
Rose slightly sedative,
aphrodisiac, healing
purifying, hemostatic,
antispasmodic
digestive, tonique, laxative,
hepatitic, antiseptic.
Pin

Disinfectant.

Stimulant, warming,
Ginger aphrodisiac, against the
fever, fatigue, cough,
the pains and the
rheumatism.

Properties of some essential oils.

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 Chapter I: Generalities on Essential Oils

I.5 Localization of essential oils:

Essential oils exist almost exclusively in higher plants, there would be

about 17,500 aromatic species, it's all the organs of the same species can
Containing an essential oil, its composition varies according to its location.
leaves, stem, root, seeds.

Example Localization Examples Localization

Garlic Bulb Cedar Wood

Ginger Rhizome Cinnamon Bark

Small seeds Stem Lemongrass Leaf

Orange Fruit Pin Budge

Rose,
Anise, nutmeg Seeds Flower
Yianyalang

Vetiver Root Incense, Myrrh Sap

Table: Localization of essential oils from some plants(Pibiri,2005)

I.6 Conservation of essential oils:

Each type of product, or even product, has a specific method of preservation.

Essential oils can be stored for about 4 years after opening in the packaging.
original (amber glass bottle) protected from light and air, essential oils
citrus being the most sensitive to oxidation.

Oil will retain its properties better if it does not come into contact with air.
Frequent and prolonged exposure to air can alter the consistency, smell, and properties.
essential oil. By sealing the lids tightly, you prevent the evaporation of the oil
essential

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Chapter I: General Information on Essential Oils

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 Chapter I: Generalities on Essential Oils

II.1 The methods of extracting essential oils:

Essential oils are obtained with very low yields (about 1%); which
makes them fragile, precious, and rare substances. There are different methods to
extract, the choice of the most suitable method is made according to the nature of the material
plant material to be processed, physicochemical characteristics of the essence to be extracted, and usage
from the extract and the aroma of the departure during the extraction (Samate Abdoul, 2001).

II .1.1 Training with steam:

Steam distillation, this technique does not come into contact

direct the water and the plant material to be treated. The principle of steam distillation
consists of passing water vapor through the plant at an adequate temperature for
destroy the plant cells, release the aromatic molecules and carry them into a
cooling serpentine. There, the cooled vapors return to a liquid state forming
a mixture "water + essential oil". Collected in an essence container, the essential oil and
Floral water separates by simple difference in density. The absence of direct contact between
the water and plant material, then between the water and aromatic molecules avoids certain
Hydrolysis or degradation phenomena that can harm the quality of the oil
(Neffati, 2010).

Figure II.1: Diagram of the steam drive assembly.

II.1.2 Extraction by Hydrodistillation:

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 Chapter I: Generalities on essential oils

This is the simplest and most commonly used method to extract the

essential oils. The process involves immersing the plant material in a container

filled with an adequate amount of water. The whole thing is then brought to a boil. The heat

allows the bursting of plant cells and the release of the fragrant molecules contained in them.

are contained. The HE forms an azeotropic mixture with water vapor. Then, the

vapors are condensed using a refrigerant. In another collecting vessel,

essential oil separates from water due to differences in density. The essential oil being lighter than

the water, it floats above the hydrolysate.

Figure II.2: Diagram of the assembly of hydro-distillation.

II .1.3 Extraction by CO2supercritique

The originality of this extraction technique lies in the type of solvent used: the
Supercritical CO2. Beyond the critical point (P = 73.8 bars and T = 31.1 °C), CO2
has intermediate properties between those of liquids and those of gases which allows it
gives a good extraction power, which moreover, is easily adjustable by playing on the
temperature and pressure conditions. This technique offers a lot
advantages. First of all, supercritical CO2 is an ideal solvent since it is natural,

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 Chapter I: Generalities on essential oils

chemically inert, non-flammable, non-toxic, selective, readily available and low

expensive. Furthermore, it easily removes from the extract without leaving residues. In addition to these

advantages, the main strength is the impeccable quality of the extract since none
rearrangement does not occur during the process. Its only weakness is the very high cost of
his installation[4].

By playing with temperature and pressure conditions, it is possible to make

the more selective extraction of odor compounds and thus obtain extracts of
composition quite similar to essential oils, not loaded with non-molecules
volatile. Thus, the temperature and pressure not to be exceeded to extract only the
The boiling point is 60 °C and 60 bars.

Figure II.3: assembly diagram of extraction with CO2super critique

This technique is now considered the most promising because it provides
very high quality volatile extracts that would fully respect the essence
original of the plant.

II .1.4 Microwave-assisted extraction:

Microwave-assisted extraction is a new technique that combines the use of
microwaves and other traditional methods. In this process, the plant material
is heated by microwaves in a closed chamber in which the pressure is reduced

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 Chapter I: General Information on Essential Oils

sequentially. The volatile compounds are carried by the steam formed at

starting from the clean water for the plant. They are then collected using classical processes.
condensation, cooling, and decantation. Studies show that this technique
has several advantages such as time savings in extraction, using small
amounts of solvent, and a high extraction yield (Hemwimon et al, 2007).

Figure II.4: Microwave-assisted hydrodistillation (Lucchesi M. E, 2005)

The authors of this process attribute certain advantages to it such as extraction time.
(ten to thirty times faster), energy savings and reduced thermal degradation.
Principles of microwaves:

Microwave-assisted extraction offers several advantages over techniques

more traditional ones, such as a shorter extraction time, a reduced use of
solvents, higher extraction rates of compounds and a processing cost
generally inferior.

[Link] of use of essential oils:

In medicine:

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 Chapter I: Generalities on essential oils

Aromatherapy is a form of alternative medicine in which essential oils have a

of great importance as they introduce numerous healing effects. Thus, they are used
increasingly in various medical specialties such as: podiatry, acupuncture,
masso-kinesitherapy, osteopathy, rheumatology, as well as in aesthetics (Yes,
2015).

I.7.2. In cosmetology:

The cosmetics industry and the hygiene product sector are also
consumers, even though the often high cost of natural products sometimes leads to
favor synthetic products for widely disseminated formulations. Since the
the majority of cosmetics contain a certain amount of essential oil such as
fragrant element, it would be likely that these essences also serve to preserve these
cosmetics while ensuring them a pleasant smell. At the boundary of the pharmacy and the
hygiene products (Bekhechi, 2010).

I.7.3. In the agri-food industries:

Due to their antiseptic and aromatic properties, essential oils are used
daily in culinary preparations (garlic, bay leaf, thyme, ..). They are also
very prized in liqueur-making (aniseed drinks, kummel) and in confectionery. Their power
Antioxidant helps to preserve food by preventing mold (Ouis, 2015).

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 Chapter I: Generalities on essential oils

General conclusion

First of all, the use of essential oils through aromatherapy (care

by plants) is the oldest medicine in the world, dating back several

millennia. Throughout history, this use of plants has allowed a large number of

civilizations to heal themselves. That is why today no one can contradict or

question the benefits of plants and it is thanks to this uninterrupted

aromatherapy and therefore the use of essential oils has evolved over the years,

centuries more and more extraction processes have been developed. Among these processes

extraction, one stood out (hydrodistillation) due to its ease of execution, its

cost and the little equipment needed. It is through this process that we were able to

noting that obtaining essential oil was simple but let us remember that obtaining a

One liter of essential oil, for example, requires a very large amount of the plant.

corresponding; essential oils are therefore very concentrated and very rich products

in active ingredients).

For a long time, hydro distillation seemed to be the extraction technique the

more profitable in terms of price and quality. But it turned out that this technique

has a production duration that is too long. Furthermore, it cannot be carried out on

a large amount of plant and it is possible to find traces of solvent there. It is for

that new techniques have been found such as microwave extraction or

Good extraction with supercritical CO2.

With the emergence of new regulations such as REACH, which mandates manufacturers to

companies to create a safety data sheet for oils containing at least 1%

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 Chapter I: Generalities on essential oils

of danger to the environment or health, the alternative was to choose

supercritical CO2 extraction. This is a technique that contains 0% danger as well.

for health as well as for the environment and allows for the production of very good quality

essential oil. The only problem is the price which is very high.

The references

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 Chapter I: Generalities on essential oils

The methods of essential oil extraction: (master's thesis:Characterization

physicochemical and biological analyses of the essential oil from Cuminum cyminum seeds
L. and Foeniculum vulgare Mill. extracted by hydrodistillation and supercritical CO2: Study
comparative.)

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