enzymatic modification of cotton/ wool and viscose/ wool blended fabrics
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Enzymatic Modification ofCotton/ Wool and Viscose/ WoolBlended FabricsN.A. Ibrahim a , E.A. Allam b , M.B. El-Hossamy b &W.M. El-Zairy ba National Research Center, Textile ResearchDivision , El-Bhouth Street, Dokki, Cairo, Egyptb Faculty of Applied Arts, Printing, Dyeing, andFinishing Department , Helwan University , Cairo,12311, EgyptPublished online: 11 Oct 2008.
To cite this article: N.A. Ibrahim , E.A. Allam , M.B. El-Hossamy & W.M. El-Zairy(2008) Enzymatic Modification of Cotton/ Wool and Viscose/ Wool Blended Fabrics,Journal of Natural Fibers, 5:2, 154-169, DOI: 10.1080/15440470801929648
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Journal of Natural Fibers, Vol. 5(2) 2008Available online at http://jnf.haworthpress.com
© 2008 by The Haworth Press. All rights reserved.154 doi:10.1080/15440470801929648
WJNF1544-04781544-046XJournal Of Natural Fibers, Vol. 5, No. 2, April 2008: pp. 1–23Journal of Natural Fibers
Enzymatic Modification of Cotton/ Wool and Viscose/ Wool Blended Fabrics
N.A. Ibrahim E.A. Allam
M.B. El-Hossamy W.M. El-Zairy
ABSTRACT. Con/wool and viscose/wool blended fabrics sampleswere biotreated with acid cellulases, neutral cellulase and/or proteaseenzymes for enhancing their performance properties. The experimentaldata indicate that: the extent of loss in weight is governed by the type ofenzyme, i.e. Acid cellulases > Neutral cellulase > Protease > none, aswell as nature of substrate, i.e., viscose/wool > cotton/wool; 2) incorpora-tion of H2O2 in enzymatic formulation results in an improvement infabric whiteness as well as its hydrophilicity; 3) bio-treatment of the usedblends results in an improvement in dyeability with anionic dyes, and theextent of improvement is governed by type of enzyme, nature of thesubstrate, as well as class of dyestuff; 4) two-steps enzymatic treatmentsgives better performance properties, and bio-treatment efficiency followsthe descending order: (Acid cellulases Proteases) > Acid cellulases >
N.A. Ibrahim is affiliated with the National Research Center, Textile ResearchDivision, El-Bhouth Street, Dokki, Cairo, Egypt.
E.A. Allam, M.B. El-Hossamy, and W.M. El-Zairy are affiliated with theFaculty of Applied Arts, Printing, Dyeing, and Finishing Department, HelwanUniversity, Cairo 12311, Egypt.
Address correspondence to: N.A. Ibrahim at the above address (E-mail:[email protected]).
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Protease > none; and 5) subsequent soft finish of enzymatic – treatedfabric samples gives rise to an improvement in fabrics resiliency andsoftness.
KEYWORDS. Cellulose/wool blend, enzymes, biotreatments, perfor-mance properties
INTRODUCTION
In the light of current move towards more eco-friendly processes andproducts, enzymatic treatments have been attempted, using different typeof enzymes, to replace harsh chemical treatments with gentler biotreat-ments; impart desirable properties, e.g., softness, drapabiliy, brightness,better dye absorption . . . etc.; minimize the environmental impacts ofindustrial processes and products; improve the economics of production;and to attain higher quality textile or apparel products (Ibrahim et al.,2005a,b; Karapinar & Sariisik, 2004; Das & Ramaswamy, 2006; Lanttoet al., 2005; Schroeder et al., 2005; Bishop, 1998; Cegarra, 1996).
With increasing demand for cotton or viscose with wool blends forproduction of trans-seasonal apparel, coolness/comfort/favorable marketshare of cellulosic component along with warmth/ resilience/hand full-ness of wool, there is a greatest need for enhancing the performance anddyeing properties of blended fabrics (Chikkodi et al., 1995; Chikkodi,1996; Sampaio, 2005).
The present work focuses on enhancing the performance properties ofcotton or viscose/wool blended fabrics by enzymatic treatment.
EXPERIMENTAL
Materials
Two mill scoured and bleached cotton/wool (70/30) and viscose/wool(70/30) blended fabrics, of 235 g/m2 weight each, were experimentallyused.
Three commercial grade enzymes namely: Denimax®992L (acid cellu-lases – strength 750 unit/g), Denimax® 362S (neutral cellulase – strength2000 unit/g), and Savinase® 16 LEX (protease enzyme for wool finishing−4 unit/g) were kindly supplied by Novo Nordisk.
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Three commercial grade anionic dyestuff namely: Telon® Red 2B(acid), Realan® Yellow 3G (reactive), and Sirius® Blue S-BRR (direct)were kindly supplied by Dystar.
Siligen® WW (nonionic softener, based on amino-functional polysi-loxne-BASF), Leomin® NI-ET (nonionic softener with hydrophilic prop-erties, based on fatty acid condensates, Clariant), as well as Hostapal®
CVL-ET (nonionic wetting agent based on alkylaryl polyglycol ether,Clariant) were of commercial grade. All other chemicals used in thisstudy were reagent grade.
Methods
Enzymatic Treatments
Enzymatic treatments of blended fabrics are given in Table 1.Nonionic wetting agent (2 g/l); goods to liquor ratio, LR, of 1:20, agita-
tion rate (40 rpm) in the absence or presence of H2O2 (10 ml/l, 35%).After treatment the enzyme was deactivated by raising the bath temper-
ature up to 80°C for dwell time of 10 min. The samples were rinsed,squeezed, and then dried and conditioned at 20°C ± 1°C and 65 ± 2% r.h.for 48 h before testing.
Soft Finishing
Soft finishing of enzymatic treated fabric samples was conducted at50°C for 30 min in presence of the softening agent (2% owf), at pH 5(using acetic acid) and LR of 1:20, followed by squeezing and drying at100°C for 5 min.
Anionic Dyeing
Portions of biotreated fabric samples, in presence of H2O2, along withuntreated controls were post-dyed with the aforementioned anionic dyes,
TABLE 1. Enzymatic treatments of blended fabrics
Enzyme Enzyme dose (%owf)
pH Temp. (°C)
Time (min)
Acid cellulases 0–1 4.5 50 30Neutral cellulase 0–2 6.5 50 30Protease 0–2.5 8.5 50 30
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Ibrahim et al. 157
3% owf, at pH 4.5 and LR of 1:20 in Launder Ometer according to themanufacturer instructions, followed by thoroughly rinsing, washing at50°C for 15 min in the presence of the nonionic wetting agent (1g/l).After being washed, the fabric samples were rinsed thoroughly with waterand then air dried.
Fabric Evaluation
Weight loss, WL, was determined as a percentage of the original, con-ditioned weight by weighting before and after enzymatic treatment.
Drop absorbency time, AT, of the treated fabric samples was deter-mined according to AATCC test method 79–1992.
Color strength, K/S, of the dyed fabric samples was measured usingColor Eye® 3100 Spectrophotometer and automatically calculated fromthe reflectance data by use of Kubelka-Munk Equation (Garland, 1983):
where K is the absorption coefficient; S is the scattering coefficient; andR is the reflectance at the wavelength of maximum absorption.
Whiteness was expressed as reflectance at 460nm measured using anreflectance spectrophotometer (Sampaio, 2005). Dry wrinkle recoveryangles, WRA (w + f)°, were evaluated according to AATCC test method66–1996. Stiffness of experimental fabrics was evaluated with the Drape-Flex stiffness tester for flexural rigidity according to ASTM test method D1388–75. Tensile strength of experimental fabrics, warp direction, wasdetermined by the strip method according to ASTM Procedure D2256–66T.
RESULTS AND DISCUSSION
Since the main task of this study is to examine the technical feasibilityof enhancing the performance properties of cotton/wool and viscose/woolblended fabrics using cellulase and protease enzymes, enzymatic treat-ments were carried out under different parameters. Results obtained alongwith appropriate discussion follow.
Type and Concentration of Enzyme
For a given set of enzymatic treatment formulations and conditions,Figure 1. shows that increasing the enzyme concentration up to 1% owf
K/S R R,= −( ) /1 22 (1)
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for acid cellulases; or up to 2% owf for neutral cellulase; or up to 2.5%owf for protease enzymes results in a gradual increase in the %WL,regardless of the used enzyme and blend components. The increase in% WL of cellulosic component is a direct consequence of increasing theextent of enzymatic action of cellulase enzymes on the accessible cellu-lose chains in amorphous area and on crystallite surfaces thereby breakingthe long cellulose chains into smaller ones and/or to glucose (Ibrahimet al., 2005a). On the other hand, the increase in % WL of wool componentcould be discussed in terms of the specific action of protease enzymes onthe peptide bonds of protein thereby enhancing the extent of their hydrol-ysis and reducing the protein chain length (Chikkodi et al., 1995). Theextent of hydrolysis is determined by the type of enzyme, e.g., molecular
FIGURE 1. Effect of enzyme type and dose on the % weight loss oftreated substrates.
Viscose / wool (ـــ) (-------) Cotton/ wool
0
0.5
1
1.5
2
0 0.5 1 1.5 2 2.5Enzyme dose (%owf)
WL(
%)
ProteaseProteaseNeutral CellulaseNeutral CellulaseAcid CellulaseAcid Cellulase
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Ibrahim et al. 159
weight, specific action, activity, mode, and extent of attack, compatibilitywith other ingredients (Ibrahim et al., 2005a; Cegarra, 1996) and followsthe descending order:
It is also evident from Figure 1, that the % WL value is governed bythe blend component, irrespective of the used enzyme and follows thedecreasing order viscose/wool > cotton/wool, reflecting the differencesbetween the two blends in surface morphology, availability, and accessi-bility of amorphous and less ordered crystalline regions in the treatedsubstrate, amount and surface fibers, chemical composition, as well as thepresence or absence of other contaminants (Ibrahim et al., 2005a; Cegarra,1996).
Combined Enzymatic Treatment/ H2O2-Bleaching
To check the feasibility of combined enzymatic treatment along withhalf-bleaching, untreated blended fabric samples were treated with theaforementioned enzymes under their proper formulation and conditions inpresence of H2O2 (10 ml/l, 35%) as a bleaching agent (Figure 2). It is clearthat incorporation of H2O2 in the enzymatic treatment formulations resultsin an improvement in the whiteness of treated samples for a given range ofpH’s which is a direct consequence of improving the extent of removal anddecolorization of colored impurities, i.e., –C=C–, from treated substratesby formation of both (•OH) and (•OOH) radicals and their subsequentaddition across sites of instauration as follow: •OH or •OOH + C = C– →−OH (Vigo, 1994). On the other hand, the positive impacts of enzymaticattack on both the blend components, via enhancing their extent of absorp-tion, as well as modifying the fabric structure, along with presence– NH2groups or – +NH3 active sites at lower pH’s, in addition to the activatingaction of the enzyme on the decomposition of H2O2 can not be ruled out(Cegarra, 1996; Levene, 1997; Ibrahim et al., 2004).
Current data, Figure 2, also show that the extent of improvement in thewhiteness of treated fabric samples is governed by both the type ofenzyme and substrate components and can be ranked as follow:
Acid cellulases Neutral cellulase Protease None.> > >
Acid cellulases Protease Neutral cellulase None and
Viscos
> > >ee/Wool Cotton/Wool respectively.>
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Fabric Wettability
As far as the changes in wettability of biotreated fabric samples as afunction of type of enzyme, Figure 3 shows that 1) enzymatic treatmentof untreated fabric samples is accompanied by a significant enhancementin fabric wettabiltiy; 2) the extent of improvement is determined byenzyme nature, i.e., Acid cellulases > Neutral cellulase > Protease >None; 3) wettability of bio-treated viscose/wool is much better than thatof cotton/wool blend which reflects the positive impact of viscose com-ponent; 4) the positive impact of cellulase enzymes is a direct conse-quence of modifying fiber surface and fabric structure, along with theremoval of hydrophobic non-cellulosic substance; and 5) the improvement
FIGURE 2. Effect of combined enzymatic treatment and H2O2-bleachingon the whiteness of treated substrates.
20
25
30
35
40
Untreated Protease(2.5% ow f)
Acid cellulases(1% ow f)
C/WV/W
Neutral cellulase(2% ow f)
Whi
tene
ss (R
efle
ctio
n at
460
nm
)
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Ibrahim et al. 161
in wettability of blended fabrics treated with protease enzyme reflectsits ability to remove the impurities and scales from the wool componentthereby improving the surface morphology, as well as modifying thewool structure and availability and accessibility of its hydrophilic sites(Chikkodi et al., 1995; Chikkodi, 1996; Sampaio et al., 2005; Garland,1983; Vigo, 1994; Levene, 1997; Ibrahim et al., 2004; Kim et al.,2006).
FIGURE 3. Effect of combined enzymatic treatment and H2O2-bleachingon wettability of the treated substrates.
0
5
10
15
20
25
30
35
Untreated Protease(2.5% ow f)
Acid cellulases(1% ow f)
C/WV/W
Neutral cellulase(2% ow f)
Wet
tabi
lity
(sec
.)
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Fabric Stiffness
For a given set of enzymatic treatment conditions, Figure 4 shows that1) enzymatic treatment results in a decrease in fabric stiffness as a directconsequence of considerable reduction in protruding loose fibers, as incase of cellulosic fabrics, or softening and/ or removing of surface scalesto a limited extent, as in case of wool component (Cegarra, 1996; Ibrahim
FIGURE 4. Effect of combined enzymatic treatment and H2O2-bleachingon treated fabrics stiffness.
60
80
100
120
140
160
180
200
C/WV/W
Untreated Protease(2.5% ow f)
Acid cellulases(1% ow f)
Neutral cellulase(2% ow f)
Fabr
ic S
tiffn
ess
(mg/
cm2 )
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Ibrahim et al. 163
et al., 2004; Cortez et al., 2004); 2) the extent of decrease in fabric stiffnessis governed by the type, of enzyme, i.e., Acid cellulases > Neutral cellu-lase > Protease > None, as well as nature of blend, i.e., Viscose/ Wool >Cotton/ Wool; and 3) the net effect of aforementioned enzymatic-treatmentsis improving handle properties.
Dyeability with Anionic Dyes
As far the changes in dyeability of biotreated fabrics, expressed as K/S values, as a function of type and dose of enzyme, and for a given setof treatment and dyeing conditions, Figures 5 and 6 show that 1) bio-treatment of cotton/wool, Figure 5, and viscose/ wool Figure 6, blendedfabrics improves post-dyeing with the used anionic dyes; 2) the extentof dyeing is governed by the type of enzyme, Acid cellulases > Neutral
FIGURE 5. Effect of enzyme type and dose on the dyeability ofbio-treated cotton/wool blended fabrics samples with anionic dyes.
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cellulase > Protease > None, as well as blend components, Viscose/Wool > Cotton/ Wool; 3) the enhancement in dye uptake after enzy-matic treatment could be discussed in terms of better hydrophilicity,availability and accessibility of dye-binding sites, smoother fabricsurface along with less light scattering, i.e. to more dye uptake andbrilliant colors (Kim S.J. et al. 2006; Ibrahim N.A. et al. 1999); and 4)the change in K/S values by using different anionic dyes may be attributedto the difference among these dyestuffs in molecular weight, chemicalstructure, substantivity, extent of exhaustion, adsorption, and penetra-tion within the fabric structure, availability and accessibility of dyemolecules in the vicinity of cellulose/ wool active sites, affinity for theblend components, mode of interaction, and extent of fixation (Ibrahimet al., 2005a; Ibrahim et al., 1999).
FIGURE 6. Effect of enzyme type and dose on the dyeability ofbio-treated viscose/wool blended fabrics samples with anionic dyes.
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Enzymatic Treatment Sequence
The change in performance properties of treated fabric samples as afunction of enzymatic treatment steps are given in Table 2. The data soobtained indicate that 1) the enhancement in the evaluated fabric prop-erties depends on the enzymatic treatment sequence and follows thedecreasing order: Acid cellulases treatment followed by proteaseenzyme treatment > Acid cellulases > Protease > None; 2) the oppositeholds true for the retained strength value; 3) the improvement in theaforementioned properties by using the two-enzymatic step treatmentreflects its positive impacts on enhancing and modifying the fabricstructure to be more hydrophilic, softer, whiter, as well as to be moredyeable with the used anionic dyes; 4) the strength loss of the treatedsubstrates is mainly due to the enzymatic attack and partial hydrolysisof the cellulose chains and/or the polypeptide chains by acid cellulasesand/or protease enzymes respectively; and 5) proper enzymatic treat-ments prove to be an eco-friendly tool for desirable and favorablechanges in both the physical and aesthetic properties of cellulose/ woolblended fabrics.
Soft Finish
For a given set of bio and soft-finish treatments, Figure 7 shows that1) the fabric resiliency, expressed as WRA values, improves by enzymatictreatment alone or followed by soft finish; 2) the extent of improvementfollows the descending order: (Acid cellulases → Protease → Siligin®
WW) > (Acid cellulases → Protease → Lemoin ® NI) > (Acid cellulases→Protease) > None; 3) the improvement in fabric resiliency can be dis-cussed in terms of considerable reduction in loose surface fibers, as wellas softening and/or degradation of the wool surface scales using cellulaseand protease enzymes, respectively. It also shows that along with thepositive impact of softening agent on reducing fabric stiffness, in additionto a reduction of interfibers and interyarns friction, thereby upgrading thetreated fabrics resiliency (Ibrahim et al. 2005a); and 4) the change inWRA values upon using different softening agents, i.e. Siligen® WW andLeomin® NI, reflects the difference between them in molecular weight,chemical composition, functionality, extent of location and distribution,along with mode of interaction with the blend components, and the soft-ening efficiency follows the order: Siligen® WW > Lemin ® NI > Withoutsoftener.
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166
TA
BLE
2. E
ffect
of e
nzym
atic
trea
tmen
t seq
uenc
e on
som
e pe
rfor
man
ce p
rope
rtie
s of
trea
ted
fabr
ic b
lend
s
Enz
ymat
ic tr
eatm
ent
WL%
Whi
tene
ssW
etta
bilit
y (s
ec.)
Stif
fnes
s (m
g/cm
2 )W
RA
(w
+ f)
°R
etai
ned
Str
engt
h%
war
p
K/S
Aci
dR
eact
ive
Dire
ct
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
C/W
V/W
Aci
d ce
llula
se (
1%ow
f)1.
751.
9531
.536
.56
112
2.5
110
230
215
93.8
91.0
23.1
24.0
13.8
16.0
7.1
9.8
Pro
teas
e (2
.5 %
ow
f)0.
490.
6130
3517
.54
170
132.
522
621
197
.695
.322
.022
.813
.013
.56.
68.
8A
cid
cellu
lase
s (1
%ow
f)
follo
wed
by
prot
ease
(2
.5%
)
2.15
2.38
38.6
48.2
4<
194
7723
522
091
.387
.524
.325
.014
.817
.67.
910
.6
Non
e—
—25
2832
.510
190
150
223
206
100
100
20.0
21.8
12.0
13.4
4.0
8.0
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Ibrahim et al. 167
FIGURE 7. Effect of enzymatic treatment followed by soft finish on fabricresiliency.
200
210
220
230
240
250
260
A B C D
(A) Untreated
(B) Acid cellulases Protease
(C) Acid Celulases Protease Siligen® WW
(D) Acid cellulases Protease Leomin® NI
C/WV/W
WRA
(w+
f)˚
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CONCLUSIONS
In this study, attempts have been carried out to enhance the perfor-mance properties of cotton/ wool and viscose/ wool blended fabrics.Enzymatic treatments were performed under a wide range of conditionssuch as type and concentration of enzyme, inclusion of H2O2 in theenzyme bath, sequence of enzymatic treatments, as well as subsequentsoft finish. Results obtained led to the following conclusions.
• For a given enzymatic treatment, increasing the enzyme dose up tocertain limits results in a weight less, and the extent of loss in weight isgoverned by the type of enzyme:
• Incorporation of H2O2 (10 ml/l, 35%) in the enzymatic formulationbrings about an improvement in the fabric whiteness, and the extent ofimprovement in fabric whiteness can be ranked as follow:
• Biotreatment in presence of H2O2 results in upgrading the treatedblends hydrophilicity and wettability.
• Biotreatment with the used cellulase and protease enzymes is accompa-nied by a noticeable decrease in fabric stiffness, regardless of the usedenzyme.
• Dyeability of bio-treated substrates with anionic dyes is governed bytype of enzyme: Acid cellulases > Neutral cellulase > Protease > None,as well as blend components: Viscose/ Wool > Cotton/ Wool.
• Two-steps enzymatic treatment gives better performance properties,and the treatment efficiency follows the decreasing order:
• Subsequent soft finishing of biotreated fabric blends results in animprovement in fabric resiliency along with softer feel.
Acid cellulases Neutral cellulase Protease
None, as well a
> > >ss nature of substrate: Viscose/wool Cotton/wool.>
Acid cellulases Neutral cellulase Protease
None, as well a
> > >ss nature of substrate: Viscose/wool Cotton/wool.>
(Acid cellulases Protease) Acid cellulases Protease None.→ > > >
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RECEIVED: February 21, 2006REVISED: March 27, 2007
ACCEPTED: October 2, 2007
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