Fragrance Finish- Aroma Microencapsulation

1. Introduction
Textile is an integral part of human life, a basic necessity for maintaining modesty, providing
protection and improving aesthetics. While the world today is progressing in all manifolds, the
increase in per capita consumption and improved standards of living has also been observed.
With upgrading lifestyles, a massive change has also been seen in the customers’ choice that is
looking for daily comfort wear. They are looking at apparels that move beyond the workspace
and home. This can be substantiated by increased usage of active wear, sportswear, season-
based clothing, aesthetic finish based textile materials, and so on. Finishing of textiles is a
segment in textile wet processing that has seen a variety of developments in terms of chemistry,
new products, processes and finishes. Finishes like UV protective, temperature regulating, odour
controlling finishes have been developed. Fragrance finishing of textiles with aroma
microcapsules has been explained further in this document.

2. Microencapsulation
Microencapsulation is a process by which very tiny droplets or particles of liquid or solid
material are surrounded or coated with a continuous film of polymeric material. It is one of the
latest technologies used to impart an array of unique characteristics to a fabric or garment.
Particles filled with active ingredients are applied to the fabric or garments for long lasting
effects. As the wearer moves, the capsules are activated producing a slow release of the active
ingredient. Active ingredients run the gamut including moisturizers, aloe Vera, vitamin E,
therapeutic smells and insect repellents. Microencapsulation is the solution for long term
durability of functional textiles. Microcapsules are small particles with sizes between 1 micron
and 7 mm that contain an active ingredient surrounded by a natural or synthetic polymer
membrane. The encapsulation is used to protect fragrances or other active agents from oxidation
caused by heat, light, humidity and exposure to other substances over their lifetime. It has also
been used to prevent the evaporation of volatile compounds and to control the rate of release.
The encapsulated agent can be released by many actions such as by mechanical pressure,
temperature change, diffusion, pH, biodegradation and dissolution means. Microencapsulation
techniques include coacervation, atomization, interfacial polymerization and in situ
polymerization. The selection of the technique and shell material depends on the final application
of the product, considering physical and chemical stability, concentration, desired particle size,
release mechanism and manufacturing costs. (Cheng et al. (2008))

2.1 Application of Microencapsulation in Textiles

 Phase Change Materials
Phase change materials are those which change the aggregation from solid to liquid within
certain range of temperature. In this way the thermoregulation of clothing is achieved and the
constant temperature is provided. They possess the ability to change their state within a certain
temperature change. These materials absorb energy during the heating process as phase change
takes place and release energy to the environment in the phase change range during a reverse
cooling process. (Jegat et al. (2001))
 Fragrance Finishes
Microencapsulation of the fragrance oil may be done and then applied to the fabric substrate.
This gives a controlled release of the fragrance and a long lasting aroma. Examples: pine oil,
lavender, rose and jasmine.
 Flame Retardants
Microencapsulation may also be done to impart flame retardant nature. In many cases where the
flame retardant finish is water soluble and hence not fast, microencapsulation may be one of the
possible solutions.
 Polychromic and Thermo-chromic Microcapsules
The application of polychromic and thermo-chromic microcapsules can be found in textiles like
product labeling, medical and security applications. One of the colour changing systems changes
colour in response to temperature, this is thermos-chromatic and the other changes colour in
response to UV light (photo chromatic). Today even microencapsulated thermos-chromatic dyes
are produced that change colour at specific temperature in response to human contact
 Antimicrobials
Demands of antimicrobial finishes continue to grow, especially for textiles for medical and
technical use. Antimicrobial finishes can be applied to textiles by microencapsulation. The
release of active substances of microcapsules with antimicrobial agent is slow and sustained.
 Counterfeiting
Microcapsules can be used to deal with the problem of illegal copying in high value added
textiles and in branded and designer goods with providing a hidden yet clear marketing system.
Microcapsules applied to label contain a colour former or an activator. By the use of UV light or
a solvent, microcapsules break open, the content is released, colour is developed and in this way
detection is achieved. In high value added textiles and also in designer or exclusive goods, there
is a great pressure to protect the goods from illegal copying within the marketplace.
Microencapsulation may be used here to give a covert, yet distinctive marking system of the
goods.
 Dyes and Pigments
Cotton, wool, polypropylene and other textiles may be dyed by using microencapsulated dyes
and pigments. (Skundric et al. (2006))

3. Fragrance Finishing
3.1 Aroma Therapy
Aroma therapy refers to therapeutic uses of fragrances which at least mere volatilize to cure and
to mitigate or cure diseases, infection and indisposition by means of inhalation alone.
Aromatherapy is increasingly being used in textiles, as it can interact with the consumer by
reducing stress, promoting comfort, and relaxation. Infusion of textiles with aromatic essential
oils makes them immense value enriched for the aesthetic dominated fashion consumers to attain
cosmetic, therapeutic and medicinal benefits. (Shelly et. al. 2015). It is the practice of using the
natural oils extracted from flowers, bark, stems, leaves, roots or other parts of a plant to enhance
psychological and physical well-being. The inhaled aroma from these "essential" oils is widely
believed to stimulate brain function. Essential oils can also be absorbed through the skin, where
they travel through the bloodstream and can promote whole-body healing. It is used for a variety
of applications, including pain relief, mood enhancement and increased cognitive function. (Goel
et al. (2010))

As other finishes, fragrance too can be applied by exhaustion and padding methods with the help
of a binder. However, as fragrances are volatile, the conventional methods might not be that
effective with repeated cycles of use and laundering. In such a case, microencapsulation of
aroma can ensure that fragrance stay on textiles for long periods, since capsules greatly reduce
the aroma evaporation rate.
 Table 1.1: Moods Associated with Different Fragrances
Mood Fragrance
Anxiety Lemon, Chamomile, Rose, Jasmine, Clove, Cardamom
Lament Rose
Stimulation Camphor, Balm Oil
Anger Chamomile, Balm Oil, Rose
Wretchedness Basil, Cypress, Mint, Patchouli
Tension Camphor, Cypress, Vanilla, Jasmine, Lavender, Sandalwood
Melancholy Basil, Lemon, Chamomile, Vanilla, Jasmine, Lavender, Mint
Hysteria Chamomile, Balm Oil, Lavender, Jasmine
Mania Basil, Jasmine, Pine
Irritability Chamomile, Camphor, Lavender

3.2 Microencapsulation of Fragrance

Microencapsulation of fragrance addresses the problem of prolonging longevity of otherwise
volatile natural oils onto the textile substrate. Household textiles such as curtains, sofas,
cushions, sheets, as well as apparel items such as gloves, socks and ties may be treated with
microencapsulated fragrance and deodorizing finishes. The carpets can be finished with
fragrances of different kinds and can be widely used in home textiles as well as automotive
textiles. Microcapsules are minute containers that are normally spherical if they enclose a liquid
or gas, and roughly of the shape of the enclosed particle if they contain a solid. Two important
things have to be kept in mind while handling fragrance microcapsules: a) no ingredient should
be omitted ensuring the proper medicinal/aesthetic value of the product b) a low temperature
binder can be used to fix the micro capsules to the textile fabric while taking care that the
durability, launderability and handle are taken care of.
Microcapsules have an active material shelled within the coat which may be natural or synthetic
depending on whether microcapsule coats are permeable or not. Microcapsules may contain
essential oil flavours like lavender, rosemary, pine and other for the effect of aromatherapy.
The encapsulation ensures that the liquid component i.e. the perfume or natural oil has converted
to a dry solid system which helps in separation of dissimilar phases. A controlled diffusion of
active components ensures long lasting or delayed fragrance release, a need for fragrance
finishes.

Figure 1.1 Fragrance release from microcapsule

3.3 Components of Microencapsulation

Essentially there are two components of microencapsulation- Core and shell.
The core is basically the material that is to be encapsulated. It may include any antimicrobial
agent, dye, finish or fragrance. The core material may be solid, liquid or gaseous in nature. It
may be volatile or non-volatile. The wall should first of all be capable of forming a film that has
a cohesive bonding with the core material to be encapsulated. In addition, it should be
chemically compatible with the core material. It should also be inert towards the active material.
It is preferred that the wall material may not be hygroscopic and also should be soluble in an
aqueous media or solvent or must be capable of melting. The coating should also be capable of
breaking when the microcapsules need to be broken.

Table 2.1: Core and Shell Material of Fragrance Encapsulation

Core material Shell Material Reference

Perfume PU/Urea Rodrigues (2009)
lavender B-Cyclodextrin Singh (2017)
patchouli chitosan-gelatin Liu(2013)
citronella gelatin, arabic gum Specos(2010)
citronella polyurethane Ribeiro2010
limonene chitosan Souza2014
limonene, orange gelatin, chitosan, gum arabic Prata2015
Jasmine PMMA Teeka2014
thyme oil, cypress oil and grapefruit sodium alginate, Acacia arabica and Geethadevi (2015)
oils in combination of 2:1:1 Moringa oleifera gum
sodium alginate (SA), Song (2017)
tetradecylallydimethylammonium
apple aroma bromide (TADAB)
cedarwood essential oil sodium alginate Ferrandiz (2017)
Limonene and vanillin chitosan/gum Arabic Sharkawy (2017)
Lemon GelatinArabic gum Abdul Aziz (2015)
Rosemary Ethylcellulose (EC)
Lemon grass Sodium alginate
Annapoorani
Citronella and Marjoram Sodium alginate-Calcium chloride (2016)

3.4 Techniques of Microencapsulation

Numerous preparation technologies available for the encapsulation of core material have been
reported. The microencapsulation techniques that are more relevant for the encapsulation of
aromatic/ essential oils and disperse dyes are discussed below:

 Phase Separation/Coacervation
It is the approach of phase separation i.e., partial dissolution of a homogenous polymer solution
into a polymer rich phase (coacervate) and the poor polymer phase (coacervation medium). The
concept behind simple or complex coacervation microencapsulation is the phase separation of
one or many hydrocolloids from the initial solution and the subsequent deposition of the newly
formed coacervate phase around the active ingredient suspended in the same reaction media. The
hydrocolloid shell can then be cross-linked, using an appropriate chemical or enzymatic cross
linker.
 Spray Drying

Microencapsulation by spray drying is a low-cost commercial process which is mostly used for
the encapsulation of fragrances, oils and flavours. Core particles are dispersed in a polymer
solution and sprayed into a hot chamber. The shell material solidifies onto the core particles as
the solvent evaporates such that the microcapsules obtained are of polynuclear or matrix type.
Figure 2.2: Schematic Representation of Spray Drying

 Centrifugal Extrusion

Liquids are encapsulated using a rotating extrusion head containing concentric nozzles. In this
process, a jet of core liquid is surrounded by a sheath of wall solution or melt. As the jet moves
through the air, it breaks into droplets of core, each coated with the wall solution. While the
droplets are in flight, a molten wall may be hardened or a solvent may be evaporated from the
wall solution. Since the drops are formed by the breakup of a liquid jet, the process is only
suitable for liquid or slurry (Holme et al. (2004).

3.5 Methodology for application of commercial fragrance microcapsules

Microcapsules can be applied to textiles by padding, coating, spraying or immersion without
altering their feel or colour. For all these methods, a binder is required; it may be acrylic,
polyurethane, silicon or starch. Its role is to fix microcapsules into the fabric and hold them in
place during wash or mechanical agitation. The textile support may be cotton, silk, wool, nylon,
polyester, leather, woven, knits, yarns and fibres. Also it can be applied to all types of clothing as
well household linen (Marinkovic et al. (2006)). An example of application of commercial
fragrance microcapsules is explained further.
  Solution Preparation
Acetic acid is used to obtain a pH of 5-6 in the final product formulation. An acidic pH helps in
exhaustion of the micro capsules. Under acidic conditions, the amine group in melamine
formaldehyde gets protonated. Due to delta negative charge on cotton fibre and the protonated
amine group, a salt linkage is formed. This helps in better exhaustion as well as durability of the
finish. Solutions are of concentrations 10gpl, 15gpl, 20 gpl.

 Application
The substrates are given a pre-treatment with 2 gpl non-ionic soap. The fabrics are then dipped in
solutions of microcapsules and padded at 70% expression, dried at 80℃ for 2 mins and cured at
different temperatures of 130℃, 150℃, 170℃. The effect of concentration of fragrance
microcapsules and that of curing temperature can be assessed.

4. Analysis and Testing

4.1 Microscopic analysis

The microcapsule solutions when checked under optical microscope help to determine the shape
and size of the formed Microcapsules. Images are taken at 100 X zoom.
 4.2 Particle size distribution
The particle size distribution of the microcapsules is as shown below.
Parameter Particle Size (micron)

Mean Particle Size 0.030

Standard Deviation 0.078

Median Particle Size 0.030

Modal Particle Size 0.032

The mean particle size is 0.030 micron with a standard deviation of 0.078 micron. As depicted in the
graph, majority of the microcapsules have particle diameter between 0.03 and 0.05 micron. A narrower
particle size distribution indicates consistent microcapsule slurry. The consistency of the slurry leads to a
uniform application on the textile substrate which is one of the primary objectives of textile processing

4.3 Thermogravimetric analysis

TGA analysis measured the amount of weight change of a material as a function of increasing
temperature. This helps to understand the processing parameters for the finish as well as give an
idea whether the formulation can be incorporated in other textile finishing which are performed
at elevated temperatures.
 TGA Thermal Analysis Result
%
100.00 commercial product 2018-05-03 13-09.tad

80.00
Start 0
30.34x10
C
End 0
500.00x10
C
60.00 0
0.00x10 0
% 0.11x10 0
min 29.62x10
C
Mid Point 0
267.33x10
C
Onset 0
264.33x10
C
0
-10.00x10 0
% 10.17x10 0
min 136.05x10
C
0 0 0 Endset 0
332.22x10
C
-20.00x10
% 14.68x10
min 181.62x10
C
0
-30.00x10 0
% 18.68x10 0
min 222.10x10
C 0
Weight Loss -102.475x10
%
40.00 0
-40.00x10 0
% 21.40x10 0
min 249.06x10
C
0
-50.00x10 0
% 23.60x10 0
min 270.51x10
C
0
-60.00x10 0
% 25.69x10 0
min 291.32x10
C
0
-70.00x10 0
% 27.71x10 0
min 312.01x10
C
20.00 0
-80.00x10 0
% 29.14x10 0
min 326.11x10
C
0
-90.00x10 0
% 30.18x10 0
min 337.01x10
C
0
-100.00x10 0
% 42.86x10 0
min 464.95x10
C

0.00
100.00 200.00 300.00 400.00 500.00
Temp [C]

4.4 Sensory Evaluation

 Hedonic scale

It is the first impression of perfumes. A measure of the degree of acceptance of a product may
be obtained by the use of hedonic scale. Panelists were asked to their degree of likeness or
dislikeness in terms which best describes their feelings about the product. The term was given in
numerical values to enable the results to be scored.

 Intensity scale

Intensity scale measures the odor strength of the product. Panelists were asked to rate the odour
strength of the perfume ingredients.
5. Production Cost
The cost of production includes variable and fixed costs. The variable costs include raw
materials and utilities. The fixed costs include repairs and maintenance, the local taxes,
plant overheads, administrative expenses and salary wages. The raw material cost
(considering application of chitosan microcapsules with lemon oil on cotton cloth) is as
follows:

Raw Materials Unit Cost (Rs/kg)

Acetic Acid (Glacial) 52

Chitosan 1100

TWEEN 20 2514

Oil 475

NaOH 90

Cotton Cloth 250

6. Application Areas:
Home Textiles: Home textiles is a major textile sector in Indian Markets and includes
home furnishings like bedsheets, pillow covers, sofa covers, carpets, curtains, mats and
so on. Home Textile being an arena that encourages incorporation of aesthetic properties,
fragrance will be an added advantage and start a niche market. Besides, applying
microcapsules with essence of rose, lavender and sandalwood would help the consumer
reduce fatigue and tiredness giving customer a new age home experience
Automotive Textiles: An upcoming sector in India, fragrant technical textiles could be
incorporated in seat coverings, carpets, linings of the car. These bear the potential to
replace car air fresheners.

Apparels: Aesthetic qualities are looked up to when it comes to apparels. Fragrant

Textiles can be used specially for kid garments and female Indian Traditional wear like
sarees, suits. Athleisure will be another segment in focus which would incorporate
refreshing scents for active body and rejuvenating minds

Sport Tech: While, microcapsules enriched socks and sportswear are commercially
available in international market, their presence in Indian Market is still not there.

Medical Textiles: Textiles enriched with microcapsules serving dual purpose of

functional antibacterial properties and providing calmness to patient is another area of
focus. Hospital bed linens, medical wipes, hand wipes, patients’ clothes can be given
fragrance finish to provide relaxation to patients
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