Application Of Microencapsulation Technique To Modern Textile Finishing.

1. Development of A Cotton Smart Textile
With Medicinal Properties Using Lime Oil
Microcapsules
NEW DEVELOPMENTS OF TEXTILES USING
MICROENCAPSULATION TECHNOLOGY

2. Applications of microencapsulation technique to the
development of textile industry
 The microencapsulation technique is used to
develop and modify textiles with new enhanced
properties such as
polychromic and thermochromics textiles
fire proofing textiles
fragrance releasing textiles
cosmetic textiles
therapeutic textiles
medical textiles

3. Development of smart cotton with
antioxidant & antibacterial properties

4. Why lime oil capsules?
• Lime essential oil is one of the most reasonably
priced and best therapeutic essential oil.
• The major components of lime essential oil proved
to be d-limonene (53.8%), β-pinene (12.6%), γ-
terpinene (16.5%), terpinolene (0.6%), α-terpineol
(0.4%), and citral (2.5%), which are very likely
responsible for the good antimicrobial &
antioxidant activity
• Lime oil is a powerful healing agent of
– acne, asthma, colds, dull skin, flu and sore
throats
Other beneficial properties such as
– antiseptic, antioxidant, antiviral, anti-
inflammatory, anti-nitrosamine, astringent,
aperitif, bactericide, antitumor and disinfectant
• Obtained by mechanically rupturing or cold
pressing the peel of the fruit of lime tree (Citrus
aurantifolia)

5. Lime oil microcapsule manufacturing process
Gum Arabic
solution
•While stirring, the prepared emulsion is added dropwise into the gum arabic solution kept in an ice bath.
•The mixture is stirred continuously for another hour.
Emulsion
•A mixture of 1.0 g of chitosan, 50 mL of distilled water and 4.0 mL of pure lime oil are stirred at 600 rpm for about 10 minutes at
room temperature until an emulsion is obtained.
Complex
coacervation
•2.5 g of gum arabic is mixed with 50 mL of distilled water and the mixture is stirred at 50 °C for about 20 minutes until all the gum
arabic are completely dissolved.
Obtain the
microcapsule
•Due to above reactions microcapsules are formed.
Final finishes
•Prepared lime oil microcapsules are well washed with a 70% ethanol solution to remove any remaining
unencapsulated lime oil.
•The washed capsules are gravity filtered and dried inside a desiccator.
Storing
•The microcapsules are kept in refrigerator until further use.
Verification
•UV-Visible and FTIR spectrometry verify the successful encapsulation of LO.

6. Verification of Lime Oil Microencapsulation
TEST
•0.08 g of washed microcapsules was transferred into a falcon tube containing 2.0 mL of 70% ethanol
•Another 0.08 g of washed microcapsules was transferred into another falcon tube containing 2.0 mL of
70% ethanol and it was well crushed using a glass rod
•Both samples were centrifuged at 4000 rpm for 10 minutes.
•The supernatants were collected separately
OBSERVATION
•UV-Visible spectra of the supernatants and pure lime oil were obtained, and the spectra were
compared
•The absorbance values of both intact (uncrushed) and crushed microcapsule samples at 243 nm
were recorded (the wavelength at which the maximum absorbance for pure lime oil was observed)
and compared
RESULT
•Mechanically crushed microcapsules recorded a significantly higher UV absorbance value at 243 nm
wavelength compared to the uncrushed microcapsules (the wavelength at which the maximum
absorbance for pure lime oil was observed).
•UV absorbance at 243 nm of test samples as mentioned below
• Uncrushed lime oil microcapsules: No absorbance
• Crushed lime oil microcapsules: 3.267 ± 0.1
CONCLUSION
•lime oil was successfully encapsulated in the prepared microcapsules and the encapsulated oil can be
released upon mechanical crushing of the microcapsule wall.

7. Properties
MORPHOLOGY
SIZE:
LOADING AND
LOADING EFFICIENCY%:
ANTIOXIDANT
ACTIVITY:
CYTOTOXICITY:
LO ATTACHMENT TO
THE COTTON
ANTIBACTERIAL
ACTIVITY
WALL
Irregular
15–160 μm
2943 ± 128 μL/g with a loading efficiency of 82 ± 4%
1336 ± 17 μg PGE/g (Folin-Ciocalteu assay)
Cytotoxicity of LO was masked by microencapsulation (has been
minimized)
The SEM images confirmed the steady attachment of LO
microcapsules to the cotton fibers prior to and after washing.
Mechanically crushed microcapsules displayed inhibition zones
against all the tested bacterial strains.
SEM images verified that Lo capsules have rough walls.

8. Determination of the Loading and Loading Efficiency of
Lime Oil Microcapsules
• The loading efficiency signifies the fraction of lime oil
incorporated into microcapsules compared to the
total volume of lime used to synthesize the
microcapsules.
• The loading of the lime oil microcapsules was found
to be 2940 ± 138 μL/g and the loading efficiency was
found to be 82 ± 4%.

9. Folin ciocalteu assay to assess antioxidant capacity of LOMC
Preparation of folin
ciacalteu reagent.
•10.0 g of sodium tunstate and 2.5 g of sodium molybdate were dissolved in 70.0 mL of distilled water in a round bottom flask.
•5.0 mL of 85% of H3PO4 acid and 10.0 mL of concentrated HCl were added into the round bottom flask.
•The mixture was refluxed for 10 hours inside a fume hood.
•15.0 g of lithium sulphate, 5.0 mL of distilled water and one drop of liquid bromine were added to the mixture.
•The mixture was refluxed for another 15 minutes & mixture cool at room temperature and finally the volume was adjusted to 100.0 mL
with distilled water.
Folin ciocalteu assay
procedure
•A standard series was prepared using pyrogallol in methanol.
•2.0 mL of 2% (w/v) sodium bicarbonate was mixed with 100 μL of each standard solution.
•The samples were incubated for 2 minutes.
•100 μL of Folin Ciocalteu reagent was added to each sample.
•The samples were incubated for 30 minutes in the dark.
•The absorbance of each sample was measured at 750 nm using the UV-Visible spectrophotometer.
•The standard curve was developed.
•The same procedure was carried out with 0.04 g/mL methanolic solutions of crushed and uncrushed microcapsules and pure lime oil (an
equivalent amount to that encapsulated in microcapsules).
•The antioxidant activity of the test samples was determined using the standard curve.
Test results
Conclusion
•The AOC (antioxidant capacity) of lime oil was retained after the encapsulation process.
•The AOC of crushed microcapsules was higher than that resulted from a similar amount of un-
encapsulated lime oil. Because chitosan is an anti-oxidant agent.(Dutta, P. K. Dutta, J. Tripathi,V. S. J Sci Ind
Res, 2004H. Espinosa-Andrews, J. G. Baez-Gonzalez, F. Cruz-Sosa, E. J. Vernon-Carter. Biomacromolecules, 2007). So extra AOC
could be due to the chitosan wall material used to synthesize the lime oil microcapsules.

10. Brine Shrimp Lethality Assay to Test the Cytotoxic Activity of Lime Oil
Microcapsules
Testing
•Brine shrimp eggs were hatched using 3.8% NaCl solution inside a glass container.
•Ten nauplii were transferred into a 5 mL solution of 3.8% NaCl.
•An aliquot of 50 μL of an ethanolic solution containing crushed or uncrushed microcapsules (prepared by mixing 0.08 g of crushed or uncrushed
microcapsules in 1.0 mL of 70% ethanol) or pure lime oil (an equivalent amount to the encapsulated amount in microcapsules) was added.
•A 50 μL aliquot of 70% of ethanol was used as the negative control.
Observations
•Each sample was observed for a period of 8 hours and the numbers of live and dead nauplii were recorded after each hour
•The percentage of mortality was calculated
Conclusion
• Cytotoxic activity of encapsulated lime oil is very low compared to un-encapsulated
lime oil. So, cytotoxicity was masked by encapsulation.

11. Investigation Of Antibacterial Activity of Lime Oil Microcapsules
DISK DIFFUSION
TEST.
• Antibacterial activity of crushed, uncrushed and unencapsulated lime oil (a similar
equivalent to the amount encapsulated in the crushed microcapsule sample) was
tested against Escherichia coli (ATCC 35218), Bacillus cereus (ATCC 11778),
Salmonella typhimurium (ATCC14028), and Staphylococcus aureus (ATCC 25923)
using the disk diffusion assay
CONCLUSION
• Un-encapsulated lime oil resulted in inhibition zones for all four tested bacterial strains.
• Similarly, the crushed microcapsules displayed inhibition zones against all the bacterial strains.
• intact microcapsules did not show inhibition zones against any of the four strains.
• Encapsulated lime oil was released upon mechanical crushing and displayed similar antibacterial
activity as the un-encapsulated lime oil.
RESULT

12. Investigation of Antibacterial Activity of
Microcapsule Incorporated Cotton Fabric
Antibacteria
l activity
test
•The fabric incorporated with lime oil microcapsules and normal cotton fabric disks were tested using disk
diffusion test against four bacterial species.
Result
•Cotton fabric containing lime oil microcapsules showed clear inhibition zones against all
four bacterial strains compared to the cotton fabric disks without the lime oil
microcapsules.
•The antibacterial activity of cotton fabric significantly increased when the microcapsules
on the fabric were subjected to crushing.
Conclusion
• Lime oil microcapsule incorporated cotton fabric displays significant
antibacterial activity against E. coli, B. cereus, S. typhimurium and S. aureus
bacterial species upon breakage of the wall of the microcapsules.
Wash
fastness
test
•Lime oil microcapsule incorporated cotton fabric was subjected to washing under 500 rpm rotational speed
for 30 min to confer the tolerable washing conditions of the microcapsule treated cotton fabric.
Results for
washed
fabric
•Inhibition zones were recorded for all four bacterial strains when the microcapsule containing fabric was
washed and then subjected to crushing.
Conclusion
•The lime oil microcapsules that were attached to the fabric were washed out up to a certain extent
under the specified wash conditions with a rotational speed of 500 rpm.
•Hence need to improve the retention of microcapsules on the cotton fabric upon washing, a
stronger fabric binder can be used during the incorporation of lime oil microcapsules to the fabric.

13. Before wash
After wash

14. Antibacterial activity of L.O.M.E cotton fabric test results

15. Incorporation of Lime Oil Microcapsules
Into Cotton Fabric
Sample
preparation
• 0.3 g of microcapsules was mixed with 3.0 mL saturated succinic acid.
• The sample was stirred overnight.
• Microcapsules were filtered and re-suspended in 1 mL of distilled water.
Application process
•A piece of 5 × 5 cm2 cotton cloth was dipped in the aqueous solution of microcapsules.
•The cloth was air dried and ironed.
Binding process
• Hydroxyl group in the cellulose enables the esterification with succinic acid which helps in the attachment of microcapsules to
the cotton fabric upon ironing. It is possible as cellulose esters are formed upon heating (Patent Number 2682454A1,2014)
Conclusion.
•According to the SEM images of microcapsules incorporated cotton fabric, adhesion of lime oil microcapsules to the cotton fiber surface confirmed (Figure 8).
• It was confirmed that the lime oil microcapsules retained on the cotton fabric even after being subjected mechanical washing under a rotational speed of 500
rpm 30 min(Figure 9) by SEM images.

16. Future developments
Since this textile has antioxidant property this can function as a reservoir system steadily
delivering antioxidants to the skin When in contact with skin, such textiles have the ability to
scavenge free radicals caused by skin degeneration and protect skin tissues from oxidative
stress and damage.
 Skin protective and durable 100% cotton face masks
 Skin protective inner garments.
Since these smart cotton textile could provide antibacterial property, these textiles can be
use as antibacterial protective textile.
 Patient clothes (for patients who are suffer from diabetic and leg ulcers )
 Daily clothes for who have skin diseases.
 Bandage for medical sector to increase the healing rate of wounds while masking
the odour.
 Inner garments next to the skin which can protect skin from microbials

17. References
• https://www.researchgate.net/publication/323887737_Development_of_a_Cotto
n_Smart_Textile_with_Medicinal_Properties_Using_Lime_Oil_Microcapsules
• https://pubs.rsc.org/en/content/articlehtml/2021/ra/d0ra09314a
• https://www.sciencedirect.com/science/article/abs/pii/S0927775715000618
• https://www.sciencedirect.com/science/article/abs/pii/S0141813017317579
• https://www.sciencedirect.com/topics/immunology-and-
microbiology/microencapsulation
• https://bibliotecadigital.ipb.pt/bitstream/10198/14448/1/Asma%20I%26EC%2020
17.pdf
• https://pubs.rsc.org/en/content/articlehtml/2021/ra/d0ra09314a
• https://www.sciencedirect.com/science/article/pii/S2214750019300447#fig0040
• https://oatao.univ-toulouse.fr/20871/1/ATGIE_Marina.pdf
• https://www.intechopen.com/books/potential-of-essential-oils/antibacterial-
properties-of-essential-oil-in-some-indonesian-herbs