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Study of Parameters Affecting Dry and Wet Ozone Bleaching of Denim Fabric
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To cite this article: Sarra Ben Hmida & Neji Ladhari (2015): Study of Parameters Affecting
Dry and Wet Ozone Bleaching of Denim Fabric, Ozone: Science & Engineering, DOI:
10.1080/01919512.2015.1113380
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Study of Parameters Affecting Dry and Wet Ozone Bleaching of Denim Fabric
Sarra Ben Hmidaa,b and Neji Ladharic
a
Textile Engineering Laboratory of the Higher Institute of Technological Studies of Ksar Hellal, National Engineering School of Monastir,
Monastir University, Monastir 5016, Tunisia; bDenim Laundry Department, Company of Textile Arts Sartex, Ksar Hellal 5016, Tunisia; cHigher
Institute of the Fashion Trades of Monastir, Textile Engineering Laboratory of the Higher Institute of Technological Studies of Ksar Hellal,
Monastir University, Monastir 5070, Tunisia
Yellowing
CONTACT Sarra Ben Hmida benhmida.sarra87@gmail.com Textile Engineering Laboratory of the Higher Institute of Technological Studies of Ksar
Hellal, National Engineering School of Monastir, Monastir University, Monastir 5016, Tunisia.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/BOSE.
© 2016 International Ozone Association
2 S. BEN HMIDA AND N. LADHARI
(Figure 1). The isatin molecule presents a yellowish The ozone machine
color. Thus, the material passes from blue (indigo) to
The bleach testing of denim was performed by means
the yellow (isatin) during the reaction.
of an ozone machine G2 Plus from Jeanologia
The process allows replacing carbon-carbon double
(Valencia, Spain) (Figure 2).
bonds by carbon-oxygen double bonds. Indeed, in an
This finishing machine is equipped with an ozone
anhydrous medium, ozonolysis of indigo results in two
generator using electric power to charge the oxygen
reaction products: isatin and isatoic anhydride
molecules in the incoming air and generate ozone for
(Ledakowicz, Solecka, and Zylla 2001).
denim. The oxygen is compressed and gathered in a
We chose to study various parameters influencing
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A Datacolor 400-Top spectrophotometer (USA) was The variation of the moisture content of the fabric
used to measure the lightness DL* and the yellowing enormously influences response DL*. The degradation
degree Db* of the ozonated samples compared to the of the color from the surface of the fabric becomes more
untreated ones. intense over the course of time. We observe, according to
The presence of isatin was confirmed by the wavelength these graphs, that the increase of lightness is not signifi-
value given by the photoLab® 6000 spectrophotometer cant for moisture values of 10 and 20%. However the
(Xylem-Germany) after its dissolution in toluene while decolorization of fabric for these values slightly increases
anthranilic acid was identified (using a Perkin Elmer with values of ozone concentration of 60 and 84 g/Nm3.
Spectrum Two ATR-FTIR in the science department of The value of DL* increases considerably for 40% and 60%
Monastir in Tunisia) by the measurement of the pH of of water pickup. In fact, high moisture gives place to a film
aqueous extracts of treated and untreated samples. of water on the surface of the fabric and generates a
swelling of the fiber, which ensures the diffusion of gas
and consequently increases the specific surface attacked
Mechanical characterization by ozone, where the decolorization of fabric is better.
Ultimate tensile strengths of the fabrics were measured When the fiber inflates after the absorption of
using a Sodimat dynamometer HJKS 1304 in Sartex, water, it becomes more receptive. The uncolored
Ksar Hellal, Tunisia. weft of the denim fabric is also bleached when
ozone gets access into the fiber; the hydration of
Downloaded by [Gazi University] at 02:32 11 January 2016
35
the indigo dye. It certainly cannot be the indigo dye in
its leuco form because ozone breaks the -C = C- double
30 bond entirely. We estimated that this yellowing might
25
be due to a derivative of isatin. The yellowing becomes
more significant when moisture increases as shown in
20 Figure 4. The yellowing as it is directly related to the
DL*
output of the ozone generator and promotes the rever- ozonation, the pH of the aqueous extract of treated samples
sibility of the ozone generation reaction. The effect of has been measured as shown in Figure 5. The different
the moisture content is higher than that of the ozone values of measured pH showed that after ozonation the
concentration, but the treatment time remains the most more the fabric becomes yellow, the more the pH becomes,
effective parameter. According to these results, having acidic which can be explained by the formation of anthra-
better bleaching of the denim fabric would always be nilic acid (Reidies, Jensen, and Guisti 1992). FTIR spectrum
better with the increase of the treatment time at mod- shown in Figure 6, proves the formation of C = O groups at
erated ozone concentrations to keep the efficiency of 1730 cm−1 in the treated sample, which does not appear in
the ozone generator and guarantee an even fading. the untreated one (Spinelle 2012). This might confirm the
formation of anthranilic acid (Mock and Rucker 1991).
The elimination of the yellowing was studied through
Study of the yellowing observed on the surface of
the fabric after ozonation
Table 3. Spectrophotometric analysis of yellowish residue.
We noticed after ozonation that the fabric has a yellow- Solvent λmax (nm) Absorbance
ish aspect, sometimes greenish. This yellowing is due to Sample Toluene 403 0.475
Isatin 405 0.473
the formation of new products from ozone oxidation of
7
10
6 6
8
5
Db*
4 6
Db*
4
pH
3
4
2
1 2
2
0
10 20 30 40 50 60
0
0 12 24 36 48 60 72 84 96 108
Moisture content (%)
Ozone concentration (g/Nm3)
Figure 4. Effect of moisture on yellowness index of samples
treated for 23 min. Figure 5. Variation of aqueous extract pH of ozonated samples.
OZONE: SCIENCE & ENGINEERING 5
108
12 g/Nm3 of ozone
106
Untreated sample 48 g/Nm3 of ozone
1120 96 g/Nm3 of ozone
104
1100
102
96
1020
1000
94
980
92
4000 3500 3000 2500 2000 1500 1000 500 0
960
Wave number, cm–1 940
920
Figure 6. ATR-FTIR spectrum of treated and untreated sample. 900
0 5 10 15 20 25
Treatment time (min)
Table 4. Evaluation of the efficiency of different neutralizing
agents. Figure 7. Variation of ultimate tensile strength of treated sam-
Hydroxylammonium Sodium ples in the warp direction.
sulfate metabisulfite Oxalic acid
Downloaded by [Gazi University] at 02:32 11 January 2016
490
Ultimate tensile strength (%)
480
several rinses at high temperature (50 °C to 70 °C) and a
470
neutralization step.
The efficiency of different neutralizing agents was 460
Table 5. Color fastness to rubbing. in water may offer better results by maintaining the
Wet ozone (Treatment time = 23 min; Moisture content = 40 %) same wetting conditions and an even bleaching.
Ozone concentration (g/Nm3) Dry rubbing Wet rubbing
12 5 3/4
60 4/5 2/3 Funding
84 4/5 2/3
96 4/5 2/3 This project is carried out within the framework of a
108 4/5 2/3
Dry ozone (Treatment time = 23 min; Moisture content = 10 %)
thesis of doctorate MOBIDOC of PASRI program
Ozone concentration (g/Nm3) Dry rubbing Wet rubbing financed by the UE and managed by the ANPR.
12 5 4/5
60 5 4/5
84 4/5 2/3 References
96 4/5 2/3
108 4/5 2/3 Crookes, W. 1874. A Practical Handbook of Dyeing and
Calico-Printing. London, UK: Longmans, Green & Co.
Hegglin, M. I., D. W. Fahey, M. McFarland, and E. R. Hash.
2014. “Twenty Questions and Answers About the Ozone
Evaluation of rubbing fastness of the treated Layer: 2014 Update,” Scientific Assessment of Ozone
samples Depletion: 2014. World Meteorological Organization,
Geneva, Switzerland
Denim is a twill cotton fabric in which the dye is Katai, A. A., and C. Schuerch. 1966. “Mechanism of Ozone
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oxidized on the surface of the fabric, which is why Attack on Α-Methyl Glucoside and Cellulosic Materials.”
after evaluation of the results using the gray scale as Journal of Polymer Science Part A-1: Polymer Chemistry 4
(10):2683–703. doi:10.1002/pol.1966.150041030.
shown in Table 5, a certain amount of color rubs off the Khalil, M. M. H., and F. A. Al-Seif. 2008. “Molybdenum and
fabric, especially at wet test. Such a result does not Tungsten Tricarbonyl Complexes of Isatin with
mean the rejection of the process, as it is still acceptable Triphenylphosphine.” Research Letters in Inorganic
compared to the results given by the conventional Chemistry 2008 (4):1–4. Article ID 746058. doi:10.1155/
denim washing process. The cotton test cloth does not 2008/746058
Ledakowicz, S., M. Solecka, and R. Zylla. 2001.
show any yellowing stains in the wet or dry rubbing,
“Biodegradation, Decolourisation and Detoxification of
which confirms the efficiency of the neutralization Textile Wastewater Enhanced by Advanced Oxidation
done after ozonation. Processes.” Journal of Biotechnology 89:175–84.
doi:10.1016/S0168-1656(01)00296-6.
Lemeune, S., H. Jameel, H.-M. Chang, and J. F. Kadla.
2004. “Effects of Ozone and Chlorine Dioxide on the
Conclusion Chemical Properties of Cellulose Fibers.” Journal of
Applied Polymer Science 93:1219–23. doi:10.1002/
The process of ozone bleaching is integrated in the (ISSN)1097-4628.
portfolio of clean technologies used in the industry to Mock, G. N., and J. W. Rucker. 1991. “Yellowing of Indigo-
allow the significant reduction of the level of environ- Dyed Acid Washed Denim.” American Dyestuff Reporter
mental impact. Such a treatment makes it possible to 80 (5):15–16,61.
minimize the consumption of hot water and the harm- Perincek, S., K. Duran, A. Korlu, and I. Bahtiyari. 2007. “An
Investigation in the Use of Ozone Gas in the Bleaching of
ful products of denim wash to the environment. It also Cotton Fabrics.” Ozone: Science & Engineering 29
allows us to get rid of the problem of redeposition of (5):325–33. doi:10.1080/01919510701509578.
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of treatment. This technology proves to be interesting Denim with Indigo.” Text Chemical Colorist 24 (2):24–6.
not only in economic dimensions but also because it Sacco, A. 2009. “Ozone Water Treatment Application and
Design.” Paper presented at the American Society of
offers a better image of the textile industries. Wet ozone
Plumbing Engineers Seminar, Indianapolis, IN. p. 35.
treatment is more profitable and gives a richer range of February 19.
washed jeans than dry ozone; however, the moisture Spinelle, L., 2012. “Microsystems selective gas sensor to
content of the fabric remains a difficult factor to con- nitrogen dioxide combining chemical filters and semi-
trol at the textile industry work conditions and depends conductor structures (indigo and/or carbon nanomater-
on the spin and the time where the jeans remain in ials) for the quality control of air“. Research Thesis,
Blaise Pascal University, Clermont-Ferrand, France.
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