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Anti-Pilling and Resin Finishing of Rayon and Rayon/Cotton Fabrics using 2

3 3 2 Mixed Level Factorial Design

Article  in  AATCC Journal of Research · September 2020

DOI: 10.14504/ajr.7.5.5

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 AATCC Journal of Research

DOI: 10.14504/ajr.7.5.5 Accepted: 02/18/2020

Anti-Pilling and Resin Finishing of Rayon and

Rayon/Cotton Fabrics using 2332 Mixed Level
Factorial Design
By Farhana Naeem, Fareha Asim, and Muhammad Tufail, NED University of Engineering & Technology

Abstract
Pilling resistance characteristics of rayon and rayon/cotton fabrics was improved by combining anti-piling and resin finish
using a statistical technique. A 2332-mixed level factorial design was chosen. Five factors were selected: anti-pilling agent and
resin finish (at three levels), and fabric blend ratio, fabric weave, and curing method (at two levels). Two response variables—
pilling before and after wash—were analyzed at the sixth level using contour and interaction plots. A high pilling grade
(4.5) was achieved on plain rayon and rayon/cotton fabrics using one concentration range of anti-pilling agent and resin
finish (normal or shock cure), and for satin fabric using a different concentration range of anti-pilling agent and resin finish.
Normal curing gave good pilling grades compared to those using shock curing.

Key Terms
Anti-Pilling, Blends, Cotton, Finishing, Mixed Level Factorial Design, Rayon, Resin, Woven

Introduction The surface density of polyester, cotton, and their 70/30

blend, produced in plain, twill, satin, matt, and diamond
Consumers of textile goods not only require comfort, weaves, are dependent on fiber type, yarn count, pick
but functional and aesthetic properties as well.1 From the density, and weave structure. Due to the slack cover factor
comfort point of view, fabrics made of natural fibers such as of a finer yarn, pills form more swiftly compared to coarser
cellulosic fibers are desirable. However, from the aesthetic yarns. Plain weaves have a compact structure, which has
point of view, wrinkle and pill free appearance of the fabric more resistance to pilling than twill and satin due to their
is usually demanded. Cotton is one of the most commonly slack configuration, which facilitate fibers coming out and
used cellulosic fibers in textile. Another regenerated cel- increased pilling.12
lulosic fiber, rayon, has gained importance over the years
because of its extraordinary characteristics.2 When it comes Chemical finishes, including use of crosslinking agents, also
to aesthetic appeal, both fibers lack in wrinkle and pilling play a very important role in improving the pilling and sur-
performance. The wrinkle recovery of rayon fiber is worse face appearance of fabrics. These agents increase the pilling
than that of cotton.3 resistance by better abrasion of the pills.13

Pilling is the formation of small balls on the fabric surface Chemical finishes have been used for reducing the pilling of
that mainly develop due to abrasion. The pilling of fabrics textiles. In one such study, a polyester/viscose knitted fabric,
is a complex phenomenon consisting of different stages, when treated with various blends of aminoplast (melamine
which is subjective and includes several factors. The type of formaldehyde and dimethylol dihydroxyethyleneurea
fiber and its cross-sectional shape, type of yarn and spinning (DMDHEU)) resins along with crosslinking agent, had
method, fabric type (knitted or woven), weave type, and durable anti-pilling properties. A central composite design
constructions and finishes used for improvement, play vital (CCD) was used to determine the resin concentration,
roles in the pilling characteristics of fabrics.4–9 whereas response surface methodology (RSM) was used to
optimize the levels of different variables.14
Pilling is undesirable and is one of the major problems in
home textile and apparel products. It has an accelerating Different anti-pilling finishes can reduce fabric pilling;
influence on the removal rate of fiber from yarn structures however, the rate of improvement of various finishes was not
that tends to reduce the service life of fabrics.4,10 Different the same. In one such study, various finishes were tested at
spinning systems produce yarns of variant structure that four different pH levels (3.5, 4.5, 5.5, and 6.5). The data were
may influence pilling resistance.4,11 Due to the differences analyzed statistically using M-Sat Microcomputer with a
in spinning systems, ring-spun yarns have ~20-40% higher completely randomized design. It was concluded that among
hairiness than open-end spun yarns.5 all the anti-pilling finishes, Appretan N9211 at 80 g/L gave

September/October 2020 Vol. 7, No. 5 | 32

 AATCC Journal of Research

the best result with a pilling grade of 4.5 at all pH levels. In concentrations (40, 100, and 150 g/L) of Appretan N9211
general, different pH values did not have a significant effect and Arkofix NF were used. The Catalyst FM concentration
on the pilling tendency of polyester/cotton fabric.15 used was 25% of the concentration of Arkofix NF, whereas,
Ceralube PIP and citric acid were kept at 20 g/L and 0.3 g/L
The pilling performance of rayon and rayon/cotton plain respectively in all recipes.
and satin fabrics was evaluated using different finishing
processes. It was concluded that Appretan N9211 helped to The fabric was finished using pad-dry-shock cure and pad-
increase the pilling resistance without significantly changing dry-cure methods. Shock curing is a fixation process that
the tensile, tear, and Berger whiteness of the fabrics.16 uses dry heat at an elevated temperature, usually 170–180 °C
for less than 60 s, depending on the material. For pad–dry-
Anti-pilling and resin finish methods have not been used in shock curing, the fabric was padded at 80% pickup, dried
combination to improve pilling resistance at various con- for 5 min at 130 °C, and shock cured at 170 °C for 30 s. For
centrations and using different curing methods. Combining pad-dry-curing, the fabric was padded at 80% pickup, dried
anti-pilling and resin finishes can not only improve pilling for 5 min at 130 °C, and cured at 150 °C for 3 min.
resistance of the fabric, but also improve wrinkle recovery,
may allow reduction of the anti-pilling agent concentration, Fabric Evaluation
and save production time. Rayon and rayon/cotton fabrics were evaluated using stan-
In this study, pilling properties of rayon and rayon/cotton dard test procedures. The pilling resistance before and after
fabrics were evaluated by combining anti-pilling and resin fabric washing was tested using ISO 12945-217 at 2000 rubs
finishes using various concentrations and curing methods. using a Nu-Martindale pilling and abrasion tester. The pilling
The statistical technique of mixed level factorial design was assessment was done in a dark room following the standard
used. This statistical method will give insight into the pro- requirement of light and pilling scales.18 Fabric washing was car-
ried out as per ISO 6330.19 The fabric was washed in a Wascator
cess and help predict the best process parameters to improve
washing machine at 40 °C and dried in a tumble dryer at low
pilling resistance.
heat using the normal cycle. The fabrics were conditioned under
Experimental standard conditions (20 ± 2 °C and 65 ± 2% relative humidity
(RH)) after tumble drying. Each response variable was tested
Fabric with two sets of replicates with a standard deviation of ±1%. The
The 100% rayon and 50/50 rayon/cotton plain and 5-end samples were tested under standard atmospheric conditions.
satin fabrics were used in the study. The rayon was made from The scales for pilling grades before and after washing
bamboo cellulose and was purchased from Sapphire Textile were assigned using standard replicas with the
Mills Ltd. Similar construction was adopted for both fabrics, following interpretation.
which consisted of 76 ends and 68 picks per inch and the yarn
count was 30’s (Ne) ring spun in both warp and weft direc- Pilling Scale17
tions. Weaving was done at the GulAhmed Textile Mills Pvt. 5 No change.
Ltd. The fabrics were pre-treated without singeing at Yunus
4 Slight surface fuzzing and/or partially formed pills.
Textile Mills Pvt. Ltd., according to industrial standards.
3 Moderate surface fuzzing and/or moderate pilling. Pills of varying
size and density partially covering the specimen surface.
Chemicals
Finishing chemicals were obtained from Archroma. Appre- 2 Distinct surface fuzzing and/or distinct pilling. Pills of
varying size and density covering a large proportion of the
tan N9211 was used as anti-pilling agent. It is a non-ionic
specimen surface.
acrylate copolymer dispersion and behaves as a self-cross-
linking agent. The resin finish recipe contained Arkofix NF 1 Dense surface fuzzing and/or severe pilling. Pills of varying size
and density covering the whole of the specimen surface.
(DMDHEU based resin, a cyclic urea derivative in water),
citric acid, Ceralube PIP softener (secondary polyethylene,
non-ionic softener to improve tear strength and provide soft Experimental Design
handle), and Catalyst FM (inorganic salt-magnesium chlo- A 2332 mixed factorial design was selected to investigate
ride solution in water to give better tear strength). the effect of influencing factors. The experimental model
and their respective levels are given in Table I. Five factors
Application Methods were used: Appretan N9211, Arkofix NF, fabric blend ratio,
The finishing liquor was prepared in one bath. The chemi- fabric weave, and curing method. These factors have been
cals were weighed in particular concentrations, made up in represented by A, B, C, D, and E respectively. Factors A
1 L of water, and stirred thoroughly before padding. Three (Appretan N9211) and B (Arkofix NF) were evaluated at three

33 | Vol. 7, No. 5 September/October 2020

 AATCC Journal of Research

different levels (40, 100, and 150 g/L), C (fabric blend ratio) Results and Discussion
was evaluated at two levels (100% rayon and 50/50 rayon/cot-
ton), D (fabric weave) was evaluated at two levels (plain and The anti-pilling and resin finishing of 100% rayon and 50/50
satin), and E (curing method) was also evaluated at two levels rayon/cotton were evaluated by the 2332 mixed level factorial
(normal cure and shock cure). design. The pilling of rayon and rayon/cotton was poor in
singed and unsinged states.14 Therefore, unsigned plain and
According to the 2332 model, there were 72 runs with each satin fabrics were treated with the finishing recipe. The pur-
run repeated twice, hence the total number of runs was pose of using unsinged fabric was to save energy, increase
144. Trials were carried out in random order correspond- the production rate, and reduce lead time.
ing to the design matrix (table available from the author by
request). The results were analyzed using Design-Expert The analysis of variance (ANOVA) of significant model
8.0.1 (Stat-ease, Minneapolis, MN, USA). terms for pilling before and after washing is given in tables
available from the author by request. The p-value of both
models was less than 0.05, which suggests that the mod-
Table I.
Design Factors and Respective Levels used in 2332 Mixed Level els were significant. Regression equations (Eqs. 1 and 2)
Factorial Design are given to explain the relationship between two or more
Factor Name Levels variables of interest.19 The main interaction plots for pilling
A Appretan N9211 40 g/L 100 g/L 150 g/L before and after wash is discussed in Figs. 1a–c to 2a–d and
B Arkofix NF 40 g/L 100 g/L 150 g/L Figs. 3a–d to 4a–b, respectively.
C Fabric blend ratio 100% rayon – 50/50 rayon/cotton
D Fabric weave Plain – Satin
Analysis of Pilling Before Wash
The sixth model (i.e., the response variable has the high-
E Curing method Normal – Shock
est degree of six) has been selected for the analysis of pilling
before wash. The details of ANOVA for significant factors and

Fig. 1. Contour plots for pilling resistance verses Appretan N9211 and Arkofix NF. (a) Plain–normal cure, (b) satin-normal cure, and (c) satin-shock cure.

September/October 2020 Vol. 7, No. 5 | 34

 AATCC Journal of Research

Fig. 2. Effect of interac-

tion plots for pilling
resistance. (a) Plot AD–
normal cure, (b) plot
AD-shock cure, (c) plot
CD-normal cure, (d)
plot CD-shock cure.

Fig. 3. Effect of interac-

tion plot AD for pilling
after wash. (a) 100%
rayon-normal cure,
(b) 100% rayon-shock
cure, (c) 50/50 rayon/
cotton-normal cure, and
(d) 50/50 rayon/cotton-
shock cure.

35 | Vol. 7, No. 5 September/October 2020

 AATCC Journal of Research

interaction terms are available from the author by request. The interaction terms are available from the author by request.
model p-value was <0.0001, which was less than 0.05, imply- The model p-value was <0.0001, which was less than 0.05,
ing that the model was significant. In this case A, C, D, E, AB, implying that the model was significant. A, B, C, D, E, AD,
AD, CD, CE, DE, ABD, ABE, CDE, A2B, ABCE, ABDE, A2BD, AE, BD, CD, CE, DE, A2, ABC, ADE, BCE, CDE, A2D, AB2,
A2BE, ABCDE, A2BCE, A2BDE, and A2BCDE were significant B2C, ABCD, BCDE, A2B2, A2CE, AB2D, AB2E, B2CD, A2B2C,
model terms. The lack of fit F-value of 0.31 suggests the lack of A2B2D, AB2DE, and A2B2CD were significant model terms.
fit was not significant relative to the pure error. The predicted The lack of fit F-value of 1.93 suggests the lack of fit was not
R2 of 0.7493 was in reasonable agreement with the adjusted significant relative to the pure error. The adequate precision
R2 of 0.878. Adequate precision of 19.93 specified an adequate of 25.945 specified a satisfactory signal.
signal. The plots of significant interactions of AB, AD, and
CD for pilling before wash are shown in Figs. 1a–c to Figs. The graphs of significant model terms have been presented in
2a–d. The significant interaction plot reveals that the pilling Figs. 3a–d to Figs. 4a–b. The significant factors and interac-
resistance of rayon and 50/50 rayon/cotton was dependent tion plots illustrate that pilling after washing was dependent
on the interaction and curvature effect of Appretan N9211 on the concentrations of Appretan N9211 and Arkofix NF,
and Arkofix NF concentrations, fabric weave, blend ratio, type of weave, blend ratio, and curing method. The pilling
and curing methods. The contour plot (Fig. 1a) for pilling resistance of plain fabrics was satisfactory for all concentra-
resistance of rayon /cotton plain fabric shows that the highest tions of Appretan N9211 (Fig. 3a–d). However, a pilling grade
pilling grade of 4.5 was achieved at various concentrations of 4 or more was achievable at the Appretan N9211 concentra-
of Appretan N9211 and Arkofix NF starting from the lowest tion of 90–130 g/L for satin fabrics with normal curing (Figs.
concentrations of 40 g/L of Appretan N9211 and 100 g/L 3a–c). Furthermore, it is evident from Fig. 3d that pilling after
of Arkofix NF. For rayon/cotton satin finished with normal washing of rayon/cotton satin was the poorest with shock
curing (Fig. 1b) the highest pilling grade of 4.5 was achievable
with 90 g/L of Appretan N9211 and 60 g/L of Arkofix NF. For
satin fabric finished by shock curing (Fig. 1c) the maximum
pilling grade of 4 was achievable with 110–150 g/L of Appre-
tan N9211 and greater than 40–50 g/L of Arkofix NF.
The pilling resistance of rayon/cotton plain weaves with normal
curing (Fig. 2a) showed good improvement in pilling grade
(4.5) at all concentration of Appretan N9211, whereas pill-
ing resistance of satin fabric showed improvement (grade 4 or
above) using an Appretan N9211 concentration of 100 g/L or
greater. The same trend can be observed for rayon/cotton fabric
that was shock cured (Fig. 2b). This difference in concentra-
tion in improving the pilling of plain and satin is due to the
slack configuration of satin fabric.14 The slack structure is due
to the long float on the satin fabric used in this research (i.e.,
5 harness—one weft yarn passes over four warp yarns). Since
the graph of interaction CE and DE depicted the same trend as
CD, it is not shown here. It is evident from Fig. 2c that the pill-
ing resistance of rayon and rayon/cotton improved significantly
(grade 4.5) after finishing using normal curing. Whereas, using
shock curing (Fig. 2d), the 50/50 rayon/cotton satin pilling rat-
ing was reduced to grade 3–4). The reduced regression equation
based on significant interactions has been shown in Eq. 1.
Pilling Resistance = +4.37 – 0.055AB + 0.13 AD – 0.12CD
– 0.13 DE + 0.14 A2B – 0.11A2BCE
Eq. 1

Analysis of Pilling after Wash

The sixth model was selected for the analysis of pilling after Fig. 4. Effect of interaction plot BD for pilling after wash. (a) 50/50 rayon/
washing. The details of ANOVA for significant factors and cotton-normal cure and (b) 50/50 rayon/cotton-shock cure.

September/October 2020 Vol. 7, No. 5 | 36

 AATCC Journal of Research

curing; a pilling grade of 2.8 was achievable at 150 g/L of discussed. In future work, the effect of finishing on crease
Appretan N9211. The interaction plot BD in Figs. 4a–b shows recovery, tensile/tear strength, whiteness, yellowness index,
that 50/50 rayon/cotton satin with shock curing was affected and light fastness of 100% rayon and 50/50 rayon/cotton
by the concentration of Arkofix NF and a concentration fabrics will be reported.
>130–150 g/L was desirable to achieve a pilling grade of 3 or
above. The interaction plot BD for rayon fabrics followed the Acknowledgement
same trend as depicted in Fig. 3d for both normal and shock
The authors express their earnest thanks to Yunus Textiles
cured fabrics. Moreover, the reduced regression equation
Mills Ltd. for extending their support by pre-treatment of
based on significant interactions is shown in Eq. 2. Predicted
the fabrics and Archroma Pakistan for allowing us to carry
R2 of 0.9033 was in reasonable agreement with the Adjusted
out the necessary experimental work. This research was
R2 of 0.9599.
funded by NED University of Engineering & Technology.
Pilling Resistance After 1st Wash = +4.24 – 0.074AE +
0.076BD – 0.22CD – 0.21DE – 0.48A2 – 0.48A2D – 0.18AB2 References
1. Hussain, U.; Younis, F. B.; Usman, F.; Hussain, T.; Faheem, A. Journal
Eq. 2
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Conclusions 2.
3. Advantages and Disadvantages of Bamboo Fabric. Cozytown Linens
Blog. http://cozytownlinens.com/blog/general/advantages-and-
The pilling and wrinkle recovery of 100% rayon and disadvantages-of-bamboo-fabric (accessed June 2020)
50/50 rayon/cotton fabrics is poor. The purpose of combing 4. Öktem, T. Fibers & Textiles in Eastern Europe 2003, 11 (4), 58–61.
anti-pilling and resin finishes was not only to improve these 5. Chiweshe, A.; Crews, P. C. Textile Chemist and Colorist and American
characteristic of the fabrics, but to also reduce the production Dyestuff Reporter 2000, 32 (9) 41–47.
time and to investigate the effect of these finishes on other 6. Omeroglu, S.; Ulku, S. Fibers & Textiles in Eastern Europe 2007, 15
(1), 39–42.
physical properties of the fabrics. 7. Muhammad, R. A.; Islam, R. M. R. Annals of the University of Oradea.
In this research, detailed statistical analysis of the signifi- Fascicle of Textiles 2015, 16 (1 ), 9–14.
8. Syed, U.; Jhatial, R. A. Mehran University Research Journal of
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resistance before and after washing of 100% rayon and 9. Göktepe, Ö. Textile Research Journal 2002, 72 (7), 625–630.
50/50 rayon/cotton fabrics. The fitted regression equations 10. Cooke, W. Journal of the Textile Institute 1982, 73 (1), 13–19.
of two response variables modelled the relationship of every 11. Paek, S. L. Textile Research Journal 1989, 59 (10), 577–583.
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factor on the finishing process. The interaction plots of fabric
Fascicle of Textiles 2015. 16 (1), 9–14.
weave, blend ratio, Appretan N9211, Arkofix NF, and cur- 13. Schindler, W. D.; Hauser, P. J. Chemical Finishing of Textiles;
ing methods revealed that pilling of rayon and rayon/cotton Woodhead Publishing Ltd.: New York, NY, USA, 2004; p 52.
fabrics could be improved up to grade 4.5 by applying anti- 14. Montazer, M.; Mazaheri, F.; Khosravian, S.; Azimi, M.; Bameni
pilling agent and resin. However, it was difficult to state one Moghadam, M.; Sadeghi, A. H. Journal of Vinyl and Additive
Technology 2011, 17 (3), 213–221.
single condition for all the fabrics tested as high pilling grade 15. Tusief, M. Q.; Mahmood, N.; Saleem, M. J. Chem. Soc. Pak. 2012, 34
depended significantly on the concentration of Appretan (1), 53–57.
N9211, Arkofix NF, and the curing method. It was concluded 16. Naeem, F.; Asim, F.; Tufail, M. AATCC Journal of Research 2018, 5
that a high pilling grade (4.5) before and after washing of (6), 8–16.
plain weave fabrics was possible using 40 g/L of Appretan 17. ISO 12945-2, Textiles-Determination of fabric propensity to surface
fuzzing and to pilling, Modified Martindale, 1st ed., International
N9211 and 40–100 g/L of Arkofix NF with normal or shock Organization for Standardization, Geneva, Switzerland, 2000, pp 1–9.
curing. Whereas, for satin weave fabrics, the concentration of 18. Montgomery, D. C. Design and Analysis of Experiments; 5th ed., John
Appretan N9211 varied from 90–150 g/L, Arkofix NF ranged Wiley & Sons: Hoboken, NJ, USA, 2001; p 87.
from 40–60 g/L, and normal curing was the most suitable cur- 19. ISO 6330, Textiles-Domestic washing and drying procedures for
textile testing, 3rd ed., International Organization for Standardization,
ing procedure. The graph of model adequacy shows that the
Geneva, Switzerland, 2012, pp 1–32.
hypothesis of normality and independency were not violated.
The regression equation modelled the relationship of each
factor with the finishing process. Furthermore, the Predicted Author
R2 values were in reasonable agreement with the Adjusted R2 Farhana Naeem, NED University of Engineering & Technol-
values, which ensured that the models accounted for most of ogy, Main University Road, Karachi 75270, Pakistan; phone
the variability. +92.321.344.9854; farhanap@neduet.edu.pk.
The effect of anti-pilling and resin finishing on the pilling
resistance of 100% rayon and 50/50 rayon/cotton fabrics was

37 | Vol. 7, No. 5 September/October 2020

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