Enhancing antimicrobial properties of dyed and finished cotton fabrics

Carbohydrate Polymers 78 (2009) 502–510

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Carbohydrate Polymers

journal homepage: www.elsevier .com/locate /carbpol

Enhancing antimicrobial properties of dyed and finished cotton fabrics

Mohamed Hashem a, Nabil A. Ibrahim a,*, Wfaa A. El-Sayed b, Shereef El-Husseiny b, Elham El-Enany b

a Textile Division, National Research Centre, Dokki, Cairo, Egyptb Faculty of Girls, Ain-Shams University, Cairo, Egypt

a r t i c l e i n f o

Article history:Received 6 April 2009Received in revised form 8 May 2009Accepted 11 May 2009Available online 18 May 2009

Keywords:1,2,3-Benzothiazole-7-thiocarboxylic acid-S-methylesterAntimicrobialBiocidesCotton fabricFinishing

0144-8617/$ - see front matter � 2009 Elsevier Ltd. Adoi:10.1016/j.carbpol.2009.05.007

* Corresponding author.E-mail address: [email protected] (N.A. Ibrah

a b s t r a c t

1,2,3-Benzothiazole-7-thiocarboxylic acid-S-methylester (commercially known as Actigard� AM-87) wasutilized to impart cotton fabric durable antimicrobial properties. Finishing treatment was carried outunder a variety of conditions. The latter were included, effect of pH, concentration of antibacterial agents,curing temperature and curing time. The effect of fabric construction, mercerization, and dyeing with dif-ferent dyestuff were also investigated. The study was also extended to investigate the technical feasibilityof combining antimicrobial finishing treatment in question with other finishing treatment generally car-ried out on cotton fabric, like soft finishing and crease recovery finishing. The treated fabrics were mon-itored for antimicrobial properties before and after washing. The treated fabrics were also evaluated forthe physio-mechanical properties like fabric tensile strength, elongation at break (or bursting strength forknitted fabric), wettability, crease recovery angle, whiteness index and roughness. Results obtained showthat, the most appropriate conditions for treatment cotton fabric with Actigard� are: padding the cottonfabric in aqueous solution containing 6% Actigard� at pH 5 (adjusted using formic acid) then squeezed towet pick up of 100%, dried at 80 �C for 5 min then cured at 100 �C for 150 s. The untreated cotton fabricdid not show any antimicrobial activity towards Staphylococcus aureus or Escherichia coli. Treatment ofcotton fabric with Actigard� improves its antimicrobial properties towards S. aureus or E. coli. It is alsoobserved that, treatment of cotton fabric with Actigard� marginally decreases fabric tensile strength,elongation at break, roughness and WI, whereas; both wettability and crease recovery angle remain prac-tically intact. This was observed whether the fabric was pre-mercerized or not.

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1. Introduction The purpose of an antimicrobial finish is to (Böhringer et al.,

In industrial practices, each decade brings into focus new tech-nologies as a marketing strategy to boost the sale both in domesticand export markets. Textile industry is no exception to this. One ofthe themes which are dominating the present decade in the textileindustry is the ‘‘medical textile”.

Microbial damage to raw cotton is a common problem, becausecotton fabrics have poor resistance to microorganisms and thus thepossibility of harming the human body due to the close contact be-tween skin and textile after only short wearing times they arecrowded by microorganisms. Additionally, the environmental con-ditions on textiles are similarly favorable as on the skin and thussupport the bacteria growth (Allen, Auer, & Pailthorpe, 2005; Böh-ringer, Rupp, & Yonenaga, 2000).

Antimicrobial finishes prevent the growth of microorganismson fabrics used in wide variety of apparel, home furnishing, com-mercial and industrial products. Fabrics for tents, tarpaulins, andauto fabrics will have a longer life when treated with some typeof antimicrobial finish that reduces or prevents damage from rotand mildew (Joseph & Marjory, 1998).

ll rights reserved.

im).

2000; Rouette, 2001):

– Prevent the transmission and spreading of pathogenic (diseasecausing) microbes.

– Inhibit odor development resulting from microbial degradation.– Avoid losses of textile performance properties.

Antimicrobial finishes should have the following requirements(Holme, 2007; Payne, 1997; Schatz, 2001; Sun & Xu, 1998, 1999).

– Durability of activity to laundering dry cleaning.– Selective activity towards undesirable micro organisms.– Acceptable moisture transport properties.– Compatibility with other finishing agents and easy to apply.– Absence of toxic effects for both the manufacturer and consumer.– Applicable with no adverse effect on the fabric properties

including wear comfort.– Should be low cost.– Resistant to body fluids and to disinfections (sterilization).

Graft polymerization of cellulosic textiles with poly(2-methyl-5-vinylpyridine) followed by treatment with potassium iodidesolution imparts antibacterial and antifungal activity (Holme,

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Table 2Name, color index and the manufacture of the dyes used in our study.

Commercial name of dye CI Company

Sunfix� Supra REd S3B SPE 150% Reactive red 195 Alwan Misr Co., Egypt

Cibanon Navy Blue-01 Vat Blue 20 Ciba Specialty ChemicalsCibanon Scarlet BNIE 200% Vat 89Cibacron Red FNR 0.05% Reactive Mix

Remazol Brilliant Blue R. Specplus

Reactive blue 19 Dyestar

Remazol Brilliant Red 3BS Reactive red 195Remazol Brilliant Yellow 4GL

PlusReactive yellow160

M. Hashem et al. / Carbohydrate P

2007; Payne, 1997; Schatz, 2001; Sun & Xu, 1998, 1999). One of themost durable type of antimicrobial products is based on a diphenylether (bis-phenyl) derivative like 2,4,40-trichloro0-2-hydroxy diphe-nyl ether or 5-chloro-2-(2-dichloro-phenoxyl) phenol (Chung, Lee, &Kim, 1998; Sekar, 2001; Washino, 1993; Wenming, Peixin, Wei, &Oing, 2002).

Quaternary ammonium compounds, biguanide, amines and glu-coprotamine show polycationic, porous and absorbent properties.Fibres finished with these substances bind microorganisms to theircell membrane resulting in the breakdown of the cell (Ha, Jung,Lee, Kim, & Kim, 1998; Lee & Jeong, 2005; Schindler & Hauser, 2004).

Complexing metallic compounds based on metals like cad-mium, silver, copper and mercury cause inhibition of the active en-zyme center (inhibition of metabolism). Amongst these, the silvercompounds are very popular and already been used in the prepa-ration of antimicrobial drinking water (Ha et al., 1998; Lee & Jeong,2005; Schindler & Hauser, 2004; Seo, Mitsuhashi, & Tanibe, 1992).

Chitosan is an effective natural antimicrobial agent derived fromchitin, a major component in crustacean shells. Coatings of chitosanon conventional fibres appear to be the more realistic prospect since;they do not provoke an immunological response. A fibre made fromchitosan is also available in the market place (Ha et al., 1998; Lee &Jeong, 2005; Schindler & Hauser, 2004; Seo et al., 1992).

The work presented in this paper aimed essentially at impartingcotton fabric an antimicrobial properties using 1,2,3-benzothiadi-azole-7-thiocarboxylic acid-S-methyl ester (commercially knownas Actigard� 87). The study was also extended to investigate thetechnical feasibility of combination between the antimicrobialtreatment with other finishing treatment of cotton fabrics like easycare finishing, softener finishing and dyeing.

2. Experimental

2.1. Materials and chemicals

Fabrics used and its specification are set out in Table 1. The fab-rics were pre washed using an aqueous solution containingNa2CO3, (10 g/L), wetting agent (2 g/L) at 95 �C for 30 min, followedby washed several times with hot water then with cold water anddried at ambient conditions.

Actigard� AM-87 was kindly supplied by Clariant internationalLtd. (It is based on 1,2,3-benzothiadiazole-7-thiocarboxylic acid-S-methyl ester – shown by structure I):

Remazol Brilliant Red B.B. Reactive red 21Remazol Turquoise Blue G plus Reactive blue 220

Reactive black B plus Reactive black 5 Dyes and IntermediatesLtd.Reactive black HFGR plus Reactive Mix

Reactive red ME 4 BL Reactive red 195

Table 3Dyeing recipes and conditions.

1,2,3-benzothiazole-7-thiocarboxylic acid-s-methylester (Actigard®87)

SC

SCH3O

N

Table 1Specification of the used substrates.

Subs. No. Fabrics specification

Subs (1) 100% woven cotton fabric (Gabardine), bleached, not mercerized(229 g/m2), weave construction 1/3 carded yarn

Subs. (2) 100% woven cotton fabric (Popline), bleached, not mercerized (189 g/m2), weave construction 1/1 carded yarn

Subs (3) 100% woven cotton fabric (Gabardine), bleached, mercerized (229 g/m2), weave construction 1/3 carded yarn

Subs. (4) 100% woven cotton fabric (Popline), bleached, mercerized (189 g/m2),weave construction 1/1 carded yarn

Subs. (5) 100% cotton, simple weave, (73/m2), weave construction 1/1 cardedyarn

Subs. (6) 100% knitted cotton fabric, Single jersey (58 g/m2)

Silicon softener under commercial name of Siligen� SIA, cationicsoftener under commercial name of Leomine� NI and Fixapret�

Eco, were of technical grade chemicals kindly supplied by BASFInternational Ltd. MgCl2�6H2O, citric acid, sodium hypophosphite,gluteraldehyde, zinc sulphate, formic acid, sodium carbonate, so-dium sulphate, sodium hydrosulphite, peptone, beef extract, agar,and sodium chloride, were of laboratory grade chemicals.

2.2. Microorganisms used

Both Staphylococcus aureus (S. aureus) (gram positive) and Esch-erichia coli (E. coli) (gram negative) were used for determinationthe antimicrobial properties of the treated samples according toAATCC standard test method (Rowe, 1978).

2.3. Dyes

Table 2 summarizes the commercial name and colour index aswell as the manufacture of dyes used.

2.4. Treatment of 100% cotton fabric with Actigard�

100% cotton fabric were padded to a wet pick up of 100% usinglaboratory padding machine in an aqueous solution containingActigard� (0–9%), at pH (2.5–9). Acidic pH was adjusted using 1%formic acid whereas alkaline pH was adjusted using 1% aqueousNaOH. The fabric was then dried at 80 �C for 5 min then cured at(100–150 �C) for (60–210 s) in laboratory oven. The treated sam-ples were then evaluated to antimicrobial activity before and afterwashing.

olymers 78 (2009) 502–510 503

Dye Shade (%) [Salt] (g/L) [Na2CO3] (g/L) Temp. (�C)

Reactive black B plus 3.90 40 20 60Reactive black HFGR plus 3.36Reactive Red ME4BL 0.65

Remazol Turquoise Blue Gplus

2.60 40 20 60

Remazol Brilliant Yellow 4GL plus

0.25

Remazol Brilliant Red BB 0.014

Remazol Brilliant Blue RSpec. plus

2.40 40 20 60

Remazol Brilliant Red 3BS 0.23Cibacron Red FNR 0.05% 0.05 40 20 60

0

5

10

15

20

25

2.5 5 7 9

E. coli Before E. coli After Staph. Before Staph. After

Inhi

bitio

n zo

ne (m

m)

pH

Fig. 2. Effect of pH on the antimicrobial properties of treated cotton fabric.Conditions used: bleached cotton fabric padded in aqueous solution containing 6%Actigard�, acidic pH was adjusted using 1% formic acid solution whereas alkalinepH was adjusted using 1% NaOH aqueous solution, wet pick up 100%, drying at 80 �Cfor 5 min, fixation at 120 �C for 90 s. (For interpretation of color mentioned in thisfigure legend the reader is referred to the web version of the article.)

0

5

10

15

20

25

30

0 1 2 3 6 9Actigard Concentration (% owb)

E. coli Before E. coli After Staph. Before Staph. AfterIn

hibi

tion

zone

(mm

)

Fig. 3. Effect of Actigard� concentration on the antimicrobial properties of thetreated cotton fabric. Conditions used: bleached cotton fabric padded in aqueoussolution containing Actigard�, pH was adjusted at 5 using 1% diluted formic acid,wet pick up, 100%, drying at 80 �C for 5 min, fixation at 120 �C for 90 s. (Forinterpretation of color mentioned in this figure legend the reader is referred to theweb version of the article.)

504 M. Hashem et al. / Carbohydrate Polymers 78 (2009) 502–510

2.5. Pilot-scale experiment

Ten meters from each kind of cotton fabric (plain weave mer-cerized, twill weave and knitted cotton fabric) were dyed in winchmachine (Barazoly). Dyeing recipes and conditions are set out inTable 3.

2.6. Testing and analysis

� The antimicrobial activity of the treated samples against S. aur-eus and E. coli were determined using agar diffusion method. Theexperimental technique was adopted as follows: known diame-ter of a swatch treated fabric put in the center of an agar plate.The plates were incubated at 37 �C for 24 h, a growth free ‘‘zoneof inhibition” around the fabric appears as the antibacterialagent migrates from the fabric onto the agar, and diffuses out-ward. Diameters of inhibition zones were determined accordingto AATCC test method 100–1999 (Fig. 1).

� Tensile strength and elongation at break of woven fabrics weredetermined according to ASTM standard test method D-1682-94 (1994).

� Bursting strength of the knitted fabrics was determined accord-ing to ASTM standard test method D-3786-01 (2002).

� Crease recovery angle of the fabric was determined according toAATCC test method 66-1972.

� Surface Roughness was measured according to JIS 94 Standardusing measuring instrument SE 1700a made in Japan.

� Wettability was assessed in terms of drop disappearance, AATCCstandard test method, D-79-1968.

� The degree of whiteness of the fabric sample expressed aswhiteness index was measured using Colour Eye� 3100 spectro-photometer supplied with SDL international according toreported method (Rowe, 1978).

� The colour strength (K/S) of dyed fabric was assessed usingKubeka-Munk equation (Convert, Schacher, & Viallier, 1999):

K=S ¼ ð1� RÞ2=2R

where K, S, and R are the absorption coefficient, scattering coeffi-cient, and reflectance, respectively.

3. Results and discussion

3.1. Effect of pH

100% cotton fabric was treated with an aqueous solution con-taining 1,2,3-benzothiazol-7-thiocarboxylic acid-S-methyl-ester(commercially known Actigard� AM-87) at different pH’s as ex-

Fig. 1. Photograph showing in

plained in the experimental part. The treated fabric samples wereevaluated for antimicrobial properties against S. aureus and E. colibefore and after washing. Results obtained are set out in Fig. 2. Itis seen from Fig. 2 that the inhibition zone observed with treated

hibition zone technique.

0

5

10

15

20

25

30

100 110 120 130 140 150

Curing Temperature ( °C)


Fig. 4. Effect of curing temperature on the antimicrobial properties of the treatedcotton fabric. Conditions used: bleached cotton fabric was padded in aqueoussolution containing 6% Actigard�, pH was adjusted at 5 using formic acid, wet pickup 100%, drying at 80 �C for 5 min, fixation time 90 s. (For interpretation of colormentioned in this figure legend the reader is referred to the web version of thearticle.)

M. Hashem et al. / Carbohydrate Polymers 78 (2009) 502–510 505

samples before washing increases as pH of the treated bath in-creases from 2.5 to 5. Further increase in pH to 9 decreases theinhibition zone. The observed inhibition zone is higher with S. aur-eus than that with E. coli at the same pH. After washing the inhibi-tion zone remain practically intact with E. coli whereas marginallydecrease with S. aureus. Result of Fig. 2 show that optimum pH fortreated 100% cotton fabric with Actigard� is 5.

3.2. Effect of Actigard� concentration

Fig. 3 shows the effect of Actigard� concentration on the antimi-crobial properties of treated cotton fabric before and after washing.Zero Actigard� concentration represents the untreated samples. Itis seen from Fig. 3 that the inhibition zone increases as the concen-tration of Actigard� increased from 1% to 9%. This is observed be-fore and after washing.

Results of Fig. 3 show also that, the inhibition zone observedwith S. aureus is higher than that observed with E. coli.

0

5

10

15

20

25

60 90 120 150 180 210


Inhi

bitio

n zo

ne (m

m)

Fixationtime (sec.)

Fig. 5. Effect of fixation time on the antimicrobial properties of the treated cottonfabric. Conditions used: bleached cotton fabric was padded in aqueous solutioncontaining 6% Actigard�, pH was adjusted at 5 using formic acid, wet pick up 100%,drying at 80 �C for 5 min, fixation at 100 �C. (For interpretation of color mentionedin this figure legend the reader is referred to the web version of the article.)

3.3. Effect of curing temperature

Fig. 4 shows the effect of curing temperature on antimicrobialproperties of Actigard� treated cotton fabric before and after wash-ing. It is seen from Fig. 4 that increasing curing temperature from100 to 150 �C exerts no effect on the antimicrobial properties of thetreated fabric. Therefore, curing at 100 �C was selected as optimumcuring temperature.

3.4. Fixation time

Fig. 5 shows the effect of fixation time on the antimicrobialproperties of the treated 100% cotton fabric. The treated sampleswere evaluated for antimicrobial properties against S. aureus andE. coli before and after washing.

It is seen from Fig. 5 that the inhibition zone increase as the fix-ation time increases from 150 to 180 s. Further increase in thereaction time decreases the inhibition zone.

3.5. Mechanism of antimicrobial activity of Actigard

Antimicrobial finishes inhibit or preferably kill microorgan-isms by a number of different mechanisms that act around thecell wall of the microorganism. Thus cell wall damage, alterationof cytoplasm membrane permeability, alteration of the physicalor chemical state of proteins and nucleic acids, inhibition of en-zyme action, or inhibition of protein or nucleic acids, inhibitionof enzyme action, or inhibition of protein or nucleic acid synthe-sis are all chemical approaches that can be utilized by antimicro-bial finishes to inhibit or kill the microorganism (Anand,Kennedy, Miraftab, & Rajendran, 2006; Parkih et al., 2005; Rast-ogi et al., 2003).

3.6. Effect of type of substrate

Releasing Actigard� leached from the treated cotton fabricand its interaction with E. coli or S. aureus would account forthe antimicrobial activity of the fabrics. It can be feasible that,for the same Actigard� concentration, fabric construction andsurface area may have a rule in alteration the antimicrobialproperties of the fabric. In order to investigate the effect offabric construction and fabric state, different bleached cottonfabric having different construction with and without pre-mercerization, were subjected to antimicrobial treatment withActigard�. Optimum conditions obtained previously (Figs. 1–5)were used to carry out the treatments. The fabrics were monitoredfor strength properties, wettability, roughness, crease recovery an-gle, whiteness index and antimicrobial properties before and aftertreatment. It should be noted here that, strength properties of thetreated woven fabric was expressed as tensile strength and elonga-tion at break, whereas for knitted fabric was expressed as burstingcoefficient. Different fabric construction include, twill, plain andsimple weave as knitted fabric. Results obtained for untreatedand treated fabrics are set-out in Table 4. Results obtained for un-treated and treated fabrics reveal that:

i. For the same fabric construction, both tensile strength andcrease recovery angle are higher for mercerized comparedwith unmercerized cotton fabric whereas elongation atbreak, wettability are comparable. Moreover, the WI is mar-ginally lower for mercerized fabric than unmercerized one.

ii. Treatment of cotton fabric with Actigard� marginallydecrease tensile strength elongation at break, roughnessand WI whereas, both wettability and crease recovery angleremain practically intact. This was observed irrespective towhether, the fabric pre-mercerized or not.

Table 4Effect of cotton fabric construction and mercerization on the antimicrobial properties of Actigard� treated fabric.

State of the fabric TS (Kgf)a (BC) El (%) Wett (s) Rous (lm) CRA (deg) WI Inhibition zone (mm)

Before washing After washing

S. aureus E. coli S. aureus E. coli

Bleached twill weave Mercerized 139 (144) 13 (15) 2 (2) 10.80 (14) 113 (114) 109.82 (114.1) 20 (0) 24 (0) 15 (0) 18 (0)Unmercerized 103 (109) 8 (14) 2 (2) 10.31 (17.31) 163 (184) 95.13 (99.44) 20 (0) 22 (0) 15 (0) 16 (0)

Bleached plain weave Mercerized 85.5 (88) 6 (7.5) 2 (2) 16.39 (19.85) 163 (191) 107.72 (112) 18 (0) 23 (0) 14 (0) 16 (0)Unmercerized 72.5 (76) 8 (8.5) 2 (2) 13.79 (19.44) 145 (155) 103.81 (109.37) 19 (0) 24 (0) 15 (0) 16 (0)

Simple weave cotton fabric 22 (30.5) 9 (9.5) 2 (2) 23 (24.95) 185 (259) 83.4 (98.28) 25 (0) 25 (0) 20 (0) 19 (0)

Knitted cotton fabric 8.9 (8.55) – (–) 5.5 (72) 13 (21.02) – (–) 100.62 (104.98) 19 (0) 22 (0) 15 (0) 18 (0)

TS, tensile strength; BC, bursting coefficient. El, elongation at break; Wett, wettability; Rou, roughness; CRA, crease recovery angle; WI, whiteness index; IZ, inhibition zone.Actigard� (6% owb), pH was adjusted at 5 using 1% formic acid, wet pick up 100% and drying at 80 �C for 5 min, fixation at 100 �C for 150 s. Bursting coefficient was measuredfor Knitted fabric. Values in parentheses represent those obtained with untreated fabrics.


iii. Untreated twill weave cotton fabric did not show any anti-microbial activity towards S. aureus or E. coli. This was evi-denced by zero inhibition zone observed with mercerizedand unmercerized fabrics. Treatment of twill weave cottonfabric with Actigard� improves its antimicrobial propertiesand the inhibition zone increased to 20 mm and 24 mmtowards S. aureus and E. coli, respectively, before washingand increased to 15 mm and 18 mm, respectively, afterwashing. Similar results are obtained with plain weave, sim-ple weave and knitted fabrics.

iv. For given fabric construction, pre-mercerization did notimprove the antimicrobial properties of Actigard treatedsamples.

It could be emphasized from results of Table 4 that, the antimi-crobial properties of Actigard� treated cotton fabric did not rely onfabric construction or pre-mercerization.

Table 5Properties of cotton fabric treated with Actigard� and Fixapret� Eco in one step.

Types of cotton fabric Treatment TS (Kgf) El. (

Twill weave bleached mercerized Untreated 144 15I 139 13II 117 16

Twill weave bleached not mercerized Untreated 109 14I 103 8II 87 12

Plain weave bleached mercerized Untreated 88 7.5I 85.5 6II 83 6.5

Plain weave bleached not mercerized Untreated 76 8.5I 72.5 8II 63 8.5

Simple weave lawn Untreated 30.5 9.5I 22 9II 19 7

Types of cotton fabric Treatment BC (Kgf/cm2)

Knitted fabric Untreated 6.90I 8.90II 6.15

TS, tensile strength; El, elongation at break; Wett, wettability; CRA, crease recovery angCotton fabric was treated with an aqueous solution containing Actigard�, 6%, Fixapret�-Ecuring at 80 �C for 5 min, fixation at 160 �C for 150 s. Treatment I: cotton fabric treatetreatments.

3.7. Combined easy care and antimicrobial finishing

One stage process for antimicrobial treatment and low formalde-hyde finishing was undertaken using Actigard� as antimicrobialagent whereas Fixapret�. Eco was selected as low formaldehyde fin-ishing agent. The treated fabrics were evaluated for antimicrobialand easy care properties. Results obtained are set-out in Table 5.

It is seen from Table 5 that:

i. Treatment of cotton fabric with Actigard� only did notimprove easy care properties of cotton fabric whereas white-ness index slightly decrease. This was observed irrespectiveto the weaving structure.

ii. Cotton samples treated with antimicrobial and easy care fin-ishing in one-step process exhibit higher crease recoveryangle compared with the untreated or treated with Acti-gard� only, the crease recovery angle increase from 113�

%) Wett (s) CRA WI IZ (mm) before washing

S. aureus E. coli

2 114 114.1 0 02 113 109.82 20 243 286 86.35 30 32

2 184 99.44 0 02 163 95.13 20 223 270 85.96 30 34

2 191 112 0 02 163 107.72 18 233 291 86.65 31 35

2 155 109.37 0 02 145 103.81 19 243 268 87.1 31 34

2 259 98.28 0 02 185 83.4 25 253 262 78.61 32 38

Wett (s) WI IZ (mm) before washing

S. aureus E. coli

7.2 104.98 0 05.5 100.62 19 224.5 94.4 30 31

le; WI, whiteness index; IZ, inhibition zone; BC, bursting coefficient.co, 6%, and MgCl2, 2%. pH was adjusted at 5 using 1% formic acid, wet pick up 100%,d with Actigard�; treatment II: one-step process for Actigard� and Fixapret�-Eco

Table 6Properties of cotton fabric treated with Actigard� and citric acid in one step.

Types of cotton fabric Treatment TS (Kgf) El. (%) Wett (s) CRA WI IZ (mm) before washing

S. aureus E. coli

Twill weave bleached mercerized Untreated 144 15 2 114 114.1 0 0I 139 13 2 113 109.8 20 24II 145 14 3 278 86.6 24 25

Twill weave bleached not mercerized Untreated 109 14 2 184 99.44 0 0I 103 8 2 163 95.13 20 22II 108 10.5 3 273 82.54 27 24

Plain weave bleached mercerized Untreated 88 7.5 2 191 112 0 0I 85.5 6.0 2 163 107.7 18 23II 86 6.5 3 286 91.2 32 24

Plain weave bleached not mercerized Untreated 76 8.5 2 155 109.37 0 0I 72.5 8 2 145 103.8 19 24II 76.5 7.5 3 273 92.93 33 25

Simple weave lawn Untreated 30.5 9.5 2 259 98.28 0 0I 22 9 2 185 83.4 25 25II 25.5 5.5 3 261 72.03 33 26

Types of cotton fabric Treatment BC (Kgf/cm2) Wett (s) WI IZ (mm) before washing

S. aureus E. coli

Knitted fabric Untreated 8.55 72 104.98 0 0I 8.9 5.5 100.62 19 22II 7.7 3 88.34 31 24

TS, tensile strength; El, elongation at break; Wett, wettability; CRA, crease recovery angle; WI, whiteness index; IZ, inhibition zone; BC, bursting coefficient.Cotton fabric was treated with an aqueous solution containing Actigard�, 6%, citric acid, 7%, and sodium hypophosphate, 3%, pH was adjusted at 5 using 1% formic acid, wetpick up 100%, drying at 80 �C for 5 min, fixation at 170 �C for 120 s.Treatment I: cotton fabric treated with Actigard�; treatment II: one-step process for Actigard� and citric acid finishing treatments.


and 163� to 286� and 270� for mercerized and unmercerizedtwill weave cotton fabric, respectively. Similar results wereobtained for plain weave and simple weave fabric.

iii. The salient feature observed in Table 5 is the higher antimi-crobial properties of cotton fabric treated with Actigard� andDMDHEU (Fixapret� Eco.) in one bath. The inhibition zone

Table 7Properties of cotton fabric treated with Actigard� and gluteraldehyde in one step.

Types of cotton fabric Treatment TS (Kgf) El. (



Plain weave bleached mercerized Untreated 88 7.5I 85.5 6II 89 7


Simple weave lawn Untreated 30.5 9.5I 22 9II 32 7.5

Types of cotton fabric Treatment BC (Kgf/cm2)

Knitted fabric Untreated 8.55I 8.9II 7.4

TS, tensile strength; El, elongation at break; Wett, wettability; CRA, crease recovery angCotton fabrics treated with an aqueous solution containing, Actigard�, 6%, gluteraldhyd100%, drying at 80 �C for 5 min, fixation at 160 �C for 150 s.Treatment I: cotton fabric treated with Actigard�; treatment II: one-step process for Ac

increased significantly in the presence than in the absenceof Fixapret Eco. This was observed with all kind of cottonfabric under investigation, whether mercerized or not.

Results of Table 5 demonstrate that, combination between antimi-crobial finishing with Actigard� and easy care finishing treatment

%) Wett (s) CRA WI IZ (mm) before washing

S. aureus E .coli

2 114 114.1 0 02 113 109.8 20 243 276 90.4 41 30

2 184 99.44 0 02 163 95.13 20 223 270 74 42 30

2 191 112 0 02 163 107.7 18 233 285 94 40 28

2 155 109.37 0 02 145 103.8 19 243 270 91.18 40 27

2 259 98.28 0 02 185 83.4 25 253 260 52.27 36 33

Wett (s) WI IZ (mm) before washing

S. aureus E. coli

72 104.98 0 05.5 100.62 19 2240 77.59 37 24

le; WI, whiteness index; IZ, inhibition zone; BC, brusting coefficient.e, 5%, and Zn sulphate, 2%. pH was adjusted at 5 using 1% formic acid, wet pick up

tigard� and gluteraldehyde.


with Fixapret� Eco can be carried out successfully and the fabricsshow improved antimicrobial properties towards S. aureus and E. coli.

Similar results are obtained when antimicrobial finishing treat-ment is combined with anti-crease finishing using citric acid andgluteraldehyde. Results obtained are set in Tables 6 and 7, respec-tively. Results of Tables 6 and 7 are similar to that obtained in Ta-ble 5 and could be explained on similar basis.

Table 8Properties of cotton fabric treated with Actigard� and silicon softener in one step.

Types of cotton fabric Treatment TS (Kgf) El. (%)



Plain weave bleached mercerized Untreated 8.8 10I 85.5 7.5II 64 8

Plain weave bleached not mercerized Untreated 76 8.5I 72.5 8II 68 9

Simple weave lawn Untreated 30.5 9.5I 22 9II 20.5 10

Types of cotton fabric Treatment BC (Kgf/cm2) Wett

Knitted fabric Untreated 8.55 72I 8.9 5.5II 8.2 90

TS, tensile strength; El, elongation at break; Wett, wettability; Rou, roughness; WI, whiCotton fabric was treated with an aqueous solution containing Actigard�, 6%, silicon sof100%, drying at 80 �C for 5 min, fixation at 100 �C for 150 s.Treatment I: cotton fabric treated with Actigard�; treatment II: one-step process for Ac

Table 9Properties of cotton fabric treated with Actigard� and cationic softener in one step.

Types of cotton fabric Treatment TS (Kg) El. (%)



Plain weave bleached mercerized Untreated 88 7.5I 85.5 6II 84 7


Simple weave lawn Untreated 30.5 9.5I 22 9II 21 10

Types of cotton fabric Treatment B. C (Kgf/cm2) Wet

Knitted fabric Untreated 8.55 72I 8.9 5.5II 8.4 37

TS, tensile strength; El, elongation at break; Wett, wettability; Rou, roughness; WI, whiCotton fabric was treated with an aqueous solution containing Actigard� 6%, and cationicup 100%, drying at 80 �C for 5 min, fixation at 100 �C for 150 sec. Treatment I: cotton fa

3.8. One-step process for antimicrobial and soft finishing of cottonfabric

In this regards, bleached cotton fabric was treated separatelywith two kind of softening agent, namely Siligen� SIA Co. (siliconbased softener) and Leargine� NIA (cationic based softener) in ab-sence and presence of Actigard� as antimicrobial finishing agent.

Wett (s) Rou (lm) WI IZ (mm) beforewashing

S. aureus E. coli

2 14 114.1 0 02 10.80 109.8 20 245 10.45 104 39 29

2 17.31 99.44 0 02 10.31 95.13 20 225 10.15 90.65 37 31

2 19.85 112 0 02 16.39 107.7 18 235 15.89 105.1 39 30

2 19.44 109.37 0 02 13.79 104 19 245 13.59 103.21 38 31

2 24.95 98.28 0 02 23 83.4 25 255 22.31 82.81 39 30

(s) Rou (lm) WI IZ (mm) before washing

S. aureus E. coli

21.02 104.98 0 013 100.62 19 2212 98.18 34 33

teness index; IZ, inhibition zone; BC, bursting coefficient.tener (Siligen� SIA), 30 g/L. pH was adjusted at 5 using 1% formic acid, wet pick up

tigard� and silicon softener.

Wett (s) Rou (lm) WI IZ (mm) beforewashing

S. aureus E. coli

2 14 114.1 0 02 10.80 109.9 20 245 10.8 108 27 33

2 17.31 99.44 0 02 10.31 95.13 20 225 9 90.67 25 31

2 19.85 112 0 02 16.39 107.8 18 235 14.39 106.8 28 33

2 19.44 109.37 0 02 13.79 103.8 19 245 12.79 101.74 26 32

2 24.95 98.28 0 02 23 83.4 25 255 18.49 82.1 28 35

(s) Rou (lm) WI IZ (mm) before washing

S. aureus E. coli

21.02 104.98 0 013.76 100.62 19 2213.0 98.23 27 29

teness index; IZ, inhibition zone; BC, bursting coefficient.softener (Leargine� NIA), 30 g/L. pH was adjusted at 5 using 1% formic acid, wet pickbric treated with Actigard�; treatment II: Actigard� and cationic softener.


It is seen from Table 8 that, the antimicrobial properties of cot-ton fabric treated with Actigard� and silicon softener in one bath ismuch higher than those treated with Actigard� only. This was ob-served irrespective of type of cotton fabric. Higher antimicrobialproperties of cotton fabric treated with Actigard� in presence ofsilicon softener may be attributed to the protective coating actionof silicon softener to the surface of fabric. This in turn prevents themicroorganism to reach the surface of fabric and create unsuitablecondition for bacterial growth. This was confirmed by decrease inthe wettability of cotton fabric treated with Silicon softener andActigard� in one bath, from 2 s to 5 s.

It is also seen from results in Table 8 that the decrease in fabricroughness follows the decreasing order: II > I > untreated regard-less the used substrate.

Similar trend was obtained by using Leargine� NIA (cationicsoftener) in combination with Actigard�. Results obtained areset-out in Table 9. Results of Table 9 are similar to that of Table8 and could be explained on similar basis.

It could be emphasized from results of Tables 8 and 9 that, incorpo-rating Actigard� in soft finishing formulation enhance the antimicro-bial properties of the cotton fabric compared with those treated withActigard� alone whereas other physical properties are comparable.

Table 11Industrial trials for antimicrobial treatment of 100% cotton.

Fabric Dye name

A-colored fabricsPlain weave bleached mercerized cotton fabric

dyed with reactive then treated withActigard�

Cibacron Red FNR 0.05%

Twill weave bleached mercerized cotton fabricdyed with reactive then treated withActigard�

Remazol turquoise G plusRemazol brilliant yellow 4GLRemazol brilliant Red 3BS

Simple weave bleached cotton fabric dyed withreactive dye then treated with Actigard�

Remazol brilliant blue R SpecRemazol Brilliant Red 3BS

Knitted cotton dyed with reactive dye thentreated with Actigard�

Reactive black B plusReactive black HFGR plusReactive red ME4BL

Fabric

B-white fabricsBleached twill weave Actigard� treated cotton fabricBleached twill weave Actigard� treated cotton fabric and mercerized

Dyeing and antimicrobial conditions used are detailed in the experimental part.

Table 10Effect of dyeing and antimicrobial treatment sequence on the properties of Actigard� trea

Treatment sequence

Reactive dyeing Dyed sampleDyed then Actigard� treated (post-treatment)Actigard� treated then dyed (post-Dyeing)

Vat dyeing Dyed sampleDyed then Actigard� treated (post-treatment)Actigard� treated then dyed (post-Dyeing)

Direct dyeing Dyed sampleDyed then Actigard� treated (post-treatment)Actigard� treated then dyed(post-Dyeing)

aK/S was measured at 550 nm.Dyeing conditions: See the experimental part.Antimicrobial treatment condition: cotton fabric was treated with an aqueous solution codrying at 80 �C for 5 min, fixation at 100 �C for 150 s.

3.9. Effect of reactive dyeing sequence

In order to investigate the effect of reactive dying sequence onthe antimicrobial properties of Actigard� treated cotton fabric,bleached unmercerized plain weave cotton fabric was treated withActigard� then dyed. For other set of samples, reactive dyeing wascarried out before the treatment with Actigard�, the reactive dyeused in our study is Sunfix� supra red and the dyeing conditionswere taken from the manufactures. The treated samples were eval-uated for K/S, wettability and antimicrobial properties. Results ob-tained are set-out in Table 10.

Results of Table 10 depict the following:

i. Cotton fabric treated with Actigard� followed by reactivedyeing loses its antimicrobial properties. This was evidencedby zero inhibition zone either with S. aureus or E. coli. At thesame time, the K/S was slightly lower than that obtainedwith untreated and dyed samples. Losing the antimicrobialproperties of Actigard� treated samples, and then reactivedyeing is attributed to the solubility and removability ofActigard� under the effect of reactive dyeing conditions(higher temp. and alkali).

Shade (%) K/S Inhibition zone (mm)

S. aureus E. coli

0.05 0.46 3.5 3.8

2.60 19.67 3.3 0.6plus 0.25

0.014

. plus 2.40 7.51 3.2 4.50.23

3.90 34.16 3.0 3.43.360.65

WI Inhibition zone (mm)

S. aureus E. coli

109.82 3.2 3.395.13 3 3.1

ted cotton fabric.

K/Sa Wettability (s) Inhibition zone (mm)

S. aureus E. coli

5.89 2 0 05.30 2 0 04.95 2 32 261.77 2 0 01.92 2 14 181.72 2 29 3314.05 2 0 016.37 2 19 2414.68 2 29 25

ntaining Actigard� 6%, pH was adjusted at 5 using 1% formic acid, wet pick up 100%,


ii. Cotton fabric reactive dyed then treated with Actigard�

shows higher antimicrobial properties as indicated by higherinhibition zone (32, 26 mm against S. aureus and E. coli,respectively) on the other hand, the fabric exhibit lower K/S than untreated then dyed (see Table 11).

3.10. Effect of vat dyeing sequence

Results obtained are set-out in Table 10. It is clear that:

i. Vat dyeing of pre-treated cotton fabric samples reduces theirantimicrobial properties. This was evidenced by (14, 18 mmfor both S. aureus and E. coli, respectively). On the other handthe K/S was slightly increased than that obtained withuntreated then dyed samples. Decreasing the antimicrobialproperties of Actigard� 87 treated sample then vat dyedcompared with sample dyed then antimicrobial treated isattributed to solubilization of Actigard� under the effect ofvat dyeing conditions (higher temp and alkali).

ii. Vat dyed Cotton fabric then treated with Actigard� showshigher antimicrobial properties as indicated by higher inhi-bition zone (29, 33 mm against S. aureus and E. coli, respec-tively) along with decrease in K/S values.

3.11. Effect of direct dyeing sequence

Results obtained from Table 10 show that the antimicrobialproperties of cotton fabric treated with Actigard� followed by di-rect dyeing are decreased. This was evidenced by (19, 24 mm forboth S. aureus and E. coli, respectively). On the other hand the K/S was slightly increased than that obtained with untreated thandyed samples. Decreasing the antimicrobial properties of Actigard�

treated sample then direct dyeing compared with sample dyedthen antimicrobial treated is attributed to solubilization of Acti-gard� under the effect of direct dyeing conditions (higher temp).

Post-treatment of direct dyed cotton fabric samples showshigher antimicrobial properties as indicated by higher inhibitionzone (29, 27 mm against S. aureus and E. coli, respectively).Whereas, the fabric exhibit slightly increase in K/S compared tountreated then dyed sample.

4. Conclusion

The most appropriate conditions for treatment cotton fabricwith Actigard� are: padding the cotton fabric in aqueous solutioncontaining 6% Actigard� at pH 5 (adjusted using formic acid) thesqueezed to wet pick up of 100%, drying at 80 �C for 5 min, fixationat 100 �C for 150 s.

Untreated cotton fabric did not show any antimicrobial activitytowards S. aureus or E. coli. Treatment of with Actigard� improves

its antimicrobial properties towards S. aureus and E. coli where theinhibition zone increased to 20 mm and 24 mm, respectively, be-fore washing and increased to 15 mm and 18 mm, respectively,after washing. Treatment of cotton fabric with Actigard� margin-ally decrease TS, elongation at break, roughness and WI whereas,both wettability and crease recovery angle remain practically in-tact. This was observed irrespective to whether, the fabric pre-mer-cerized or not. Moreover, the antimicrobial properties of Actigard�

treated cotton fabric did not rely on fabric construction or pre-mercerization.

Incorporating Actigard� in softening finishing formulation oreasy care finishing formulation using Fixapret� Eco, citric acid orgluteraldehyde, enhance the antimicrobial properties of the cottonfabric compared with those treated with Actigard� only whereasother physical properties are comparable. The results show alsothat cotton fabrics dyed with reactive dye, direct dye or vat dyethen treated with Actigard� show higher antimicrobial and lowerK/S properties than those Actigard� treated fabric the similarlydyed.

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Enhancing antimicrobial properties of dyed and finished cotton fabrics