Chemical Engineering Journal 239 (2014) 284–289

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Chemical Engineering Journal

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Fixation of vitamin E microcapsules on dyed cotton fabrics

1385-8947/$ - see front matter � 2013 Published by Elsevier B.V.http://dx.doi.org/10.1016/j.cej.2013.11.034

⇑ Corresponding author. Tel.: +82 62 530 1341; fax: +82 62 530 1349.E-mail address: yshin@jnu.ac.kr (Y. Shin).

K. Son a, D.I. Yoo b, Y. Shin a,⇑a Dept. of Clothing & Textiles/Human Ecology Research Institute, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Koreab Dept. of Polymer and Fiber System Engineering, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Korea

h i g h l i g h t s

� Fixation of vitamin E microcapsuleson dyed cotton knit by pad-dry-curemethod.� Softener was treated in a

simultaneous step withmicrocapsules or in a separate step.� Microcapsules particles containing

vitamin E were stable to the processof laundering, rubbing and ironing.� The K/S value and hue of dyed fabrics

were hardly affected by processconditions or process order.� Colorfastness to repeated washing

was improved by microcapsules andsoftener treatments.

g r a p h i c a l a b s t r a c t

a r t i c l e i n f o

Article history:Received 31 July 2013Received in revised form 4 November 2013Accepted 15 November 2013Available online 25 November 2013

Keywords:Vitamin EPad-dry-cureNatural indigoCottonSoftenerColorfastness

a b s t r a c t

The fixation of vitamin E microcapsules was carried out by pad-dry-cure method on dyed cotton knit.Cotton knit was dyed with natural indigo, and subsequently treated with microcapsules containing vita-min E. In order to improve the hand of the microcapsules-treated fabric, a softener was treated in a simul-taneous step with microcapsules or in a separate step after dyeing process.

It was confirmed by SEM analysis that microcapsules were fixed on cotton fibers. Melamine–formalde-hyde microcapsules containing vitamin E was stable during the process of repeated washing, rubbing andironing. LC–MS analysis indicated that the amount of vitamin E decreased gradually with elapsed time.Regardless of the softener treatment order, softness improved and air permeability decreased. The K/Svalue and hue of dyed fabrics were hardly affected by process conditions or process order. Colorfastnessto repeated washing was improved by microcapsules and softener treatments. Based on the obtainedexperimental results, it can be concluded that the fixation of vitamin E microcapsules on dyed cotton knitby pad-dry-cure method was very reliable in terms of durability of microcapsules and color stability ofthe treated fabrics.

� 2013 Published by Elsevier B.V.

1. Introduction

Recently, there has been a growing concern of consumers fornatural dyed and functional fabrics. To meet this, researches onnatural dyed fabrics with functionality are being conducted [1–4]. A new terminology, so-called ‘cosmetic textiles’, is a conse-quence of the fusion of cosmetics and the textile industry through

various techniques, such as micro-encapsulation and has nowopened up new target groups and sustainable markets in the tex-tile industry [5,6]. The group of textiles that works to provide amoisturizing effect on human skin is called cosmetic textiles formoisturizing [5].

Vitamin E belongs to the group of liquid-soluble vitamins andthe its chemical term is alpha-tocopherol. Since vitamin E shutsout hazardous oxygen which is the cause of skin aging, and offersa superior moisturizing effect, it is often used as a functional cos-metics material [5]. Furthermore, vitamin E has been widely used

K. Son et al. / Chemical Engineering Journal 239 (2014) 284–289 285

as a useful ingredient in drug medicine, food, etc. [7–9]. However,vitamin E is subject to oxidation due to the low reliability on exter-nal factors, such as heat and oxygen. These disadvantages make itdifficult to apply vitamin E directly to textile finish [10].

In cosmetic textile fields, micro-encapsulation techniques con-taining core materials, or functional materials, such as fragrant[11–13], phase change material [14,15], and antimicrobials [16]are being applied in order to improve safety and durability of func-tional materials [17,18]. Also, with microcapsules containing vita-min E for underwear, T-shirts and bedding, which all have directcontact with the skins, the effect of vitamin E on the skin will beable to be sustained for a long period of time [19].

Meanwhile, the application of natural dyes on textile materialsis gaining worldwide popularity due to the increasing awareness ofenvironment, ecology and pollution control [20–22]. Natural indi-go showing distinctive blue color is one of the oldest known dye-stuffs. In particular, it is excellent in colorfastness andfunctionality such as antimicrobial properties, deodorization andanti-insect properties, compared with other natural dyes [23].

The objective of this study was to develop natural dyed fabricswith moisturizing effect. We applied vitamin E microcapsules fin-ishing onto natural indigo dyed cotton knit to impart moisturizingfunctionality. Scoured and bleached cotton knit was dyed with nat-ural indigo powder and subsequently padded with melamine–formaldehyde microcapsules containing vitamin E. To improvethe hand of treated fabric, softener was treated in a simultaneousstep with microcapsules or in a separate step. Scanning electronmicroscopy (SEM) was used to confirm the presence and morphol-ogy of the microcapsules. The amount of vitamin E of treated fab-rics was evaluated by LC/MS analysis. The effect of microcapsulestreatment on physical properties, color and colorfastness wereinvestigated.

2. Experimental part

2.1. Materials

The fabric used in this study was scoured and bleached 100%cotton, which is characterized in Table 1. Natural indigo dye wasprepared from Polygonum tinctorium using the Korean traditionalniram method and contained 15.2%(w/w) of indigo and0.757%(w/w) of indirubin [24]. Melamine–formaldehyde micro-capsules containing vitamin E acetate was supplied in the slurrystate by Polychrom Co. Ltd. (Korea). Vitamin E acetate, also knownas tocopheryl acetate, is used as an alternative to vitamin E itself. Itis believed that acetate is slowly hydrolyzed once it is absorbedinto the skin, regenerating vitamin E [25]. The mean particle sizeof the microcapsules was 2.36 lm. Anionic softener (Prosoft) andacrylic binder (Poly Fix-A) were also used in its commercial form(Polychrom, Co. Ltd., Korea). All of the other chemicals were re-agent grade.

2.2. Preparation of dyed fabric sample

The reduction of natural indigo was achieved gently shaking thedye solution with 20 g/L of natural indigo powder and 5 g/L of so-dium hydrosulfite in a liquor ratio of 1:50 at 70 �C for 30 min. Thedyeing was done by dipping in a reduced dye bath at 45 �C for

Table 1Characteristics of knitted fabric.

Fiber Weave Density (threads, in.�1)

Wale Co

Cotton Plain 40 56

30 min. Dipped samples were followed by air oxidation for30 min. After complete oxidation, the samples were rinsed in tapwater and dried. Scheme 1 presents the dyeing process in thisstudy.

2.3. Fixation of the microcapsules on dyed fabrics

The dyed fabrics were impregnated for 10 min to enhance pen-etration with an aqueous solution composed of 3% (owb) micro-capsules and 3% (owb) acrylic binder in a liquor ratio 1:20,padded by two-dips/two-nips method, dried at 80 �C for 5 minand cured at 150 �C for 3 min. 3% (owb) softener was applied eitheras additive during microcapsules padding or after microcapsulestreatment. Sample codes, according to the treatment process, areshown in Table 2. The add-ons for the microcapsules-treated fab-rics were calculated according to the formula:

Add on ð%Þ ¼ ðb� aÞ=a� 100

where a is the fabric weight of the sample before treatment, and b isthe weight of the sample after treatment.

2.4. Evaluation of treated fabrics

The surface of the microcapsules-treated fabrics was observedusing a scanning electron microscope (SEM: JSM 5400F, JEOL Inc.,Japan). The amount of vitamin E was quantified as an acetate con-tent through an organic solvent extraction method using liquidchromatography–mass spectrometer (LC–MS: HP 1100 series, Agi-lent technologies Inc., USA). Ionization mode was API-ES, mass fil-ter mode was Q-pole and detector was HED-EM. The solution foranalysis was extracted from 2 g of vitamin E microcapsules-treatedfabric at 23 �C for 2 h with 50 mL of methanol using a shakingwater bath; 1 mL of these was utilized for analysis, and moreover,the acetate content was calculated from the prebuilt calibrationcurve.

Stiffness (drape stiffness; ASTM test method D 1388-64) and airpermeability (Frazier method; ASTM test method D 737-96) wereevaluated using the standard procedures. Stiffness was assessedby the resistance to bending. Air permeability was the rate of airflow through a fabric under differential pressure between thetwo fabric surfaces.

The Color value of dyed fabrics were evaluated in terms of thedye uptake (K/S values at 660 nm), the H V/C Munsell color values,CIE L⁄ a⁄ b⁄ coordinates and color difference (DE⁄), using a MacbethColoreye 3100 spectrophotometer under Illuminant D65 with a 10�standard observer.

Colorfastness to washing, rubbing, ironing and light of the dyedand microcapsules-treated fabrics were estimated by the followingstandard methods. Using a Launder-O-meter (Atlas Electric DeviceCo., Houston, TX), the washing test was carried out according to theAATCC test method 61-1989 at 40 �C for 45 min in water, whichhad a volume of 200 mL with 0.5% light detergent. The rubbing testwas carried out using a standard crockmeter (DL-2007, Daelim Co.,Ltd., Korea) under dry and wet conditions according to the AATCCtest method 8-2005. The ironing test was conducted in hot press-ing under dry and damp conditions (AATCC test method 133-2004). The light fastness test was evaluated according to theAATCC test method 16-2004 (option 3) using Xenon Test Chamber

Weight (g m�2) Thickness (mm)

urse

155 0.40

Scheme 1. Flow chart of dyeing process.

Table 2Sample codes according to the treatment process.

Sample code Treatment process

D DyeingD/MC Dyeing ? microcapsules treatmentD/MC-S Dyeing ? microcapsules and softener treatmentD/MC/S Dyeing ? microcapsules treatment ? softener treatment

286 K. Son et al. / Chemical Engineering Journal 239 (2014) 284–289

(Q-SUN, Xe-1-B, Q-Panel Lab Products, USA) after irradiation for20 h. Colorfastness rating for washing, rubbing and ironing wereassessed by a color change against the standard gray scale, andlight fastness rating was assessed by the color difference (DE⁄)using a spectrophotometer (values 1–5; where 1 = poor and5 = excellent).

3. Result and discussion

3.1. Morphology of vitamin E microcapsules-treated fabrics

Fig. 1 shows SEM photographs of the treated cotton knit accord-ing to vitamin E microcapsules and softener treatment process. Thespherical shaped microcapsules and binder were located at inter-stices between fibers and on the fiber surface. D/MC/S samplehas finer and more evenly distributed coatings than D/MC and D/MC-S sample. It was confirmed by SEM analysis that microcapsuleswere fixed on cotton fibers.

Fig. 2 shows the microscopic views of the fabrics tested at thegiven washing, rubbing and ironing conditions. The shape ofmicrocapsules observed on the fiber surface after 20 washing cy-cles, rubbing and ironing was similar to the SEM photographs priorto the tests (Fig. 1). Most of the microcapsules also maintained theround shape rather than a broken or distorted shape. Among sam-ples in Fig. 1, the D/MC and D/MC/S samples showed slight de-crease the binding of fibers after treats. This reveals thatmelamine–formaldehyde microcapsules are stable throughoutthe processes of washing, rubbing and ironing. We also deducedfrom the SEM observation that a softener treatment on the micro-capsules-treated fabric did not affect the durability of themicrocapsules.

3.2. Release of vitamin E from the microcapsules-treated fabrics

To investigate the release of vitamin E from the microcapsules-treated fabrics, the amount of vitamin E of the washed samples

(a) D/MC (b) D/M

Fig. 1. SEM photographs (X1000) of

with 5 and 20 cycles were measured by LC/MS analysis. The resultsare presented in Table 3. The amount of vitamin E after 5 washingdecreased by 345 lg/g (5.47%) compared to the sample withoutwashing. After 20 washing, the amount of vitamin E slightly de-creased by 61 lg/g (1.02%) compared to the sample washed 5 cy-cles. We found that the decrease in the amount of vitamin Eduring repeated washing was minimal. As observed in the SEMphotographs (Fig. 2), the minimal change was speculated as a re-sult of the superior durability of the microcapsules.

On the other hand, the amount of vitamin E on the treated fabricdecreased gradually with elapsed time for up to 18 weeks of stor-age, as shown in Fig. 3. The amount of vitamin E released for6 weeks in earlier stage was around 120.44 g/m2. Thereafter, theamount of vitamin E released for 12 weeks was decreased toaround 42.82 g/m2. Therefore, the rough number of vitamin E dif-fused through the wall of microcapsules might be about1.534 � 1023/m2 for 6 weeks and then it was decreased to5.455 � 1022/m2. This result indicated that vitamin E was releasedslowly and gradually through microcapsules wall.

3.3. Physical properties of vitamin E microcapsules-treated fabrics

Add on, stiffness and air permeability of the treated samplesaccording to natural indigo dyeing, vitamin E microcapsules andsoftener treatment processes are shown in Table 4. Add-ons of D/MC-S and D/MC/S samples discernibly showed higher values of0.25–0.30 than that of D/MC sample. Air permeability is an impor-tant factor in comfort of textile materials applied special finishingtechnique [6]. After dyeing and microcapsules treatments, the stiff-ness of the fabrics increased very slightly, while air permeabilitydecreased. As shown in the SEM photographs of Fig. 1, the fixationof the microcapsules with binder resulted stiffer and less air per-meable fabrics [15]. Also, the decrease in air permeability was pos-sibly due to the impregnation of cotton fabric with microcapsules;the coated microcapsules would fill up the gap between yarns,making the airflow pass more difficult through the fabric [6].Regardless of the softener treatment order, softness improvedand air permeability decreased with the addition of softener. Yet,D/MC/S sample, which was treated softener in a separate step,was stiffer and less air permeable compared with D/MC-S sample,which was treated softener simultaneously. It can be attributed bymore coating of softener in a separate D/MC/S sample [3]. Softenerwas more universally used in textile finishing than any other of fin-ishing agent. It could reduce the friction between fibers and yarns,

C-S (c) D/MC/S

microcapsules-treated fabrics.

Samples Washing (20 cycles) Rubbing (dry condition) Ironing (damp test)

D/MC

D/MC-S

D/MC/S

Fig. 2. SEM photographs (X1000) of microcapsules-treated fabrics after washing, rubbing and ironing test.

Table 3Amount of vitamin E according to the washing in vitamin Emicrocapsules-treated fabrics (D/MC-S samples).

Washing (cycles) Amount of vitamin-E (lg/g)

0 6308 ± 1125 5963 ± 52

20 5902 ± 24

Elapsed time (weeks)0 2 4 6 8 10 12 14 16 18 20

Amou

nt o

f vita

min

E (g

)

700

800

900

1000

1100

Fig. 3. Release of vitamin E according to the elapsed time of D/MC-S samples(100 cm � 100 cm).

Table 4Add-on and physical properties of dyed and microcapsules-treated fabrics.

Samples Add-on (%) Stiffness (cm) Air permeability (cm3/min/cm2)

Control – 1.48 ± 0.01 109.46 ± 1.99D – 1.50 ± 0.01 107.44 ± 1.52D/MC 1.92 ± 0.05 1.52 ± 0.03 101.91 ± 2.52D/MC-S 2.22 ± 0.03 1.43 ± 0.03 97.87 ± 2.37D/MC/S 2.17 ± 0.02 1.45 ± 0.06 90.83 ± 4.37

K. Son et al. / Chemical Engineering Journal 239 (2014) 284–289 287

gave the treated fabric soft handle and improved drape property[26,27]. From these results, It was considered that the simulta-

neous treatment of softener with microcapsules was more efficientthan the separate treatment in points of better physical propertiesand simpler procedure.

3.4. Color of the vitamin E microcapsules-treated fabrics

Table 5 presents the K/S values and color properties accordingto indigo dyeing, vitamin E microcapsules and softener treatmentprocesses. The K/S value of dyed fabrics did not change signifi-cantly after subsequent treatments with different preparationmicrocapsules or softener. The hue (H, 3.7 PB) of the dyed sampleshifted slightly to 4.2–4.3 PB after the microcapsules and softenertreatment. Lightness of the treated sample was decreased afterseparate softener treatment (D/MC/S). The results showed thatsoftener could affect the shade of dyed fabrics. Some of softenerssuch as silicones would cause the shade to become darker. Thisis optical phenomenon which the proportion of reflected light de-creases in a medium with decreasing refractive index [28]. In addi-tion, the decrease of absolute a⁄ value and absolute b⁄ values afterthe microcapsules and softener treatments represented that bothgreen color decreased and blue color decreased. The color differ-ence (DE⁄), as a result of microcapsules and softener treatment,was in the range of 0.82–2.44. In particular, D/MC/S sample

Table 5K/S value and color properties of treated fabrics.

Treatment K/S value (660 nm) H V/C L⁄ a⁄ b⁄ DE⁄

D 6.85 3.7 PB 3.6/3.5 38.56 �2.39 �14.76 –D/MC 6.67 4.2 PB 3.6/3.4 37.53 �1.59 �14.38 0.82 ± 0.02D/MC-S 6.43 4.3 PB 3.7/3.5 38.61 �1.57 �14.63 1.46 ± 0.06D/MC/S 6.91 4.2 PB 3.4/3.2 35.21 �1.52 �13.86 2.44 ± 0.04

a⁄; Red(+)/green(�) color axis.b⁄; Yellow(+)/blue(�) color axis, DE⁄; color difference.

288 K. Son et al. / Chemical Engineering Journal 239 (2014) 284–289

showed the largest color difference of 2.44, as indicated by the rel-atively large change in L⁄, a⁄ and b⁄ values. While D/MC and D/MC-S sample had no color difference to the naked eye, the color differ-ence in D/MC/S sample was visible to the naked eye. This resultwas caused by the coating of softener on the surface of the dyedand microcapsules-treated fabrics. Parvinzadeh and Najafi re-ported that post-treatment with anionic, cationic, nonionic, microand macro emulsion silicone softeners changed color coordinatessuch as L⁄, a⁄ and b⁄ values of all cotton fabrics dyed with directdyes or sulfur dyes [29,30].

Fig. 4. Effect of washing cycles on the color difference of treated samples.

Fig. 5. Effect of light time on the color difference of treated samples.

3.5. Colorfastness of the vitamin E microcapsules-treated fabrics

The fastnesses to washing, rubbing, ironing and light of thedyed fabrics were evaluated as per standards. The degrees of fast-ness are indicated by numbers, ‘1’ representing the lowest and ‘5’the highest. The colorfastness of dyed fabric (D) were relativelygood as the above 3/4 rating (Table 6). The solubility and the rateof movement of the dye outward from the fiber are the factordetermining fastness to washing. It is worth to mention that waterinsoluble dye such as indigo dye usually shows better fastness ascompared to water soluble dye [31]. Through microcapsules andsoftener treatment, all of the fabric samples showed an equal orhigher colorfastness ratings compared to the indigo dyed fabric.The application of softener on the textile materials ensure thatthey contain some moisture which make them soft. The swelledfabric due to having high surface obviously results to poor washand rubbing fastness [31]. However, the softener treated samples(D/MC-S and D/MC/S) have shown acceptable washing and rubbingfastness with improving softness (Table 4).

In practical point of view, it is very important that the colorretention according to repeated washing or continuous light expo-sure of natural dyed fabric with functionality. To investigate thecolor retention of vitamin E microcapsules-treated fabrics, the col-or difference (DE⁄) of the treated samples were determined afterwashing up to 20 cycles and after light exposure for 40 h.

Color difference by repeated washing of 5 and 20 cycles areshown in Fig. 4. Regardless of the treatment process, color differ-ence increased. Color difference of the dyed samples (D) were inthe range of 1.63–2.28. On the other hand, color difference of themicrocapsules and softener treated samples were in the range of0.76–1.73. The color difference of the dyed sample got larger thanthat of the other samples as more washing repeated. It speculated

Table 6Colorfastness data of the treated fabrics.

Treatment Washing (5 cycles) Rubbing Ironing Light (20 h)

Color change Stain Dry Wet Dry Damp

D 4 4 4 3/4 5 4/5 3/4D/MC 4/5 4/5 4/5 3/4 5 4/5 3/4D/MC-S 4/5 4/5 4/5 4 5 4/5 3/4D/MC/S 4 4/5 4/5 4 5 5 3/4

that vitamin E microcapsules and softener on the fiber surface pre-vented dye molecules washing out more or less.

Fig. 5 shows the color difference after light exposure of 5, 10, 20and 40 h. With an extension of exposure time to 40 h, no more col-or difference occurred. Especially, D/MC-S and D/MC/S samplesshowed more fading than D/MC sample. It was reported that soft-ener treatment caused more fading of cotton fabrics dyed with di-rect dye or sulfur dye for 2 days [29,30]. Color difference after lightexposure for 40 h was in the range of 1.50–4.25, which was largerthan that of repeated washing. The treated samples in this studyseems to choose drying method of less light exposure.

4. Conclusion

The fixation of vitamin E microcapsules was carried out by pad-dry-cure method on dyed cotton knit. Cotton knit was dyed withnatural indigo, and subsequently treated with microcapsules con-

K. Son et al. / Chemical Engineering Journal 239 (2014) 284–289 289

taining vitamin E. In order to improve the hand of the microcap-sules-treated fabric, a softener was treated in a simultaneous stepwith microcapsules or in a separate step after dyeing process. Thetreated fabrics were evaluated for SEM observation, amount ofvitamin E, physical properties, and color properties.

It was confirmed by SEM analysis that microcapsules were fixedon cotton fibers. Melamine–formaldehyde microcapsules contain-ing vitamin E was stable during the process of repeated washing,rubbing and ironing. LC–MS analysis indicated that the amountof vitamin E decreased gradually with elapsed time. Regardless ofthe softener treatment order, softness improved and air permeabil-ity decreased. The K/S value and hue of dyed fabrics were hardlyaffected by process conditions or process order. Colorfastness to re-peated washing was improved by microcapsules and softenertreatments. Based on the obtained experimental results, it can beconcluded that the fixation of vitamin E microcapsules on dyedcotton knit by pad-dry-cure method was very reliable in terms ofdurability of microcapsules and color stability of the treatedfabrics.

Acknowledgements

This research was supported by the Basic Science Research Pro-gram through the National Research Foundation of Korea (NRF)funded by Ministry of Education, Science and Technology (No.20100021015).

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