investigation of resin treatment effects on the mechanical, thermal and surface properties of cotton...

Transylvanian

Review

Vol XXIV, No. 13, 2017

Transylvanian Review

Centrul de StudiiTransilvane| str. MihailKogalniceanunr. 12-14, et.5, Cluj-Napoca

Email: [email protected] / Online Submission System: http://transylvanianreviewjournal.org/

Litim et al. Transylvanian Review: Vol XXIV, No. 13, 2017

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Investigation of Resin Treatment Effects on the Mechanical, Thermal and Surface Properties of Cotton Yarns

Nasr Litim, Ayda Baffoun, Mohamed Hamdaoui and Saber Ben Abdessalem

Textile Materials and Processes Research Unit MPTex, National Engineering School of Monastir5019, Tunisia

Abstract

This paper presents an investigation of resin treatment effect on the mechanical and surface properties of different cotton yarns. Three types of untreated cotton yarn were used;a 100% cotton yarn, a sized 100% cotton yarn, and cotton yarn containing 5% of Elasthanne. All yarns were treated with cross linking agents which are Glyoxalic and Acrylic resin and mixed resin. This study allowed determining the best finishing conditions for preserving the mechanical properties during fabric finishing process. This research allowed understanding the effect of yarn composition and the effect of starch sizing composition on the quality of resin treatment. In fact, the analysis of surface morphology of treated yarns by SEM, thermal analysis of treated cotton yarns by DSC and the resin's thermal analysis by TGAallowed a better appreciative of the effect of resins treatmentconditions:resin concentration, curing temperature, curing time, dry time and dry temperature.Obtained results showed that sized cotton yarn is most preserving the mechanical properties under curing conditions; unlike stretch cotton yarnis more sensitive to high curing temperature and time.

Key words:Cotton yarn, finishing resin, thermal analyze, surface morphology, mechanical properties

Corresponding author: [email protected] MPTex, National Engineering School of Monastir 5019, Tunisia.

mailto:[email protected]


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Introduction

Cotton fibers are the mainlyused natural fibers in apparel industry. Theyareused fortheirrelativelyelevated aqueous absorption,strengthand resistanceto abrasion. Thes epropertiesallow obtaining comfortable and resistantwearatcompetitive cost.Their intrinsictendencytowardscreasinginwearandshrinkageonwashingconstitute their principaldisadvantages(M.S.Yen & C.C.Chen, 1987).

The first challenge to defeat this problem was applying formaldehydebased compounds, mostlyDimethyloldihydroxyethyleneurea (DMDHEU) as a crosslinker’s agent (E. Edwin Sunder & G. Nalankilli, 2012., W. D. Schindler &P. J. Hauser, 1994). These resins enter into the fibers and when catalyzed, createa polymeric network structure that avoids the fibers from creasing and shrinking. (W. D. Schindler & P. J. Hauser, 1994). A durable press finishing agent createscovalent bonds with cellulosic hydroxyl groups under hightemperatures;thereforeshape cross linkages between the cellulose molecules. Cross linkingusuallylead to an upgrading in wrinkle resistance and to reducein the strength of cotton fabric. Wrinkle recovery and tensile strength are the two major parameters which are used to evaluate the performance of crosslinked cotton fabrics. (H. Petersen et al, 1971,M.S.Yen & C.C.Chen, 1987, E. Edwin Sunder & G. Nalankilli, 2012). DMDHEUcrosslinkers is the majoritygenerally used crosslinkers as it offera high-quality durable press properties at low cost and is less damaging to the fabric strength, and other properties than other agents (W. D. Schindler & P. J. Hauser, 1994). The finishing treatment include simply impregnating the cellulosic fabric with the pre-condensate as a result that it penetrate into the fibers and then curing fabric to temperatures between 130°C-180°C in the existence of a catalyst. (T.F.Cooke &H.D Weigmann, 1982, C.Tomasino, 1992, C.Q.Yang, 1996.). In previously studies, we have experimentedcotton fabrics with the glyoxalic DMDHEU and copolymer acrylic, using a spraying technique. We obtained that the resin glyoxalic DMDHEU affect hard the mechanical and surface properties (tear strength, elongation at break, 3D rank and shrinkage) of treated fabrics before and after washing. However, copolymer acrylic resin affects the same properties with a miniature rate. N. Litim et al. (2016). Today, it is interesting to know the behavior of cotton yarns (raw or sized) treated with the resin especially in the course of the

chemical priming step in the industry. The yarn has the basic element of any final textile structure. In fact, understanding and studying of the relationship design "yarn-resin" point of view; Cohesion, action, reaction, surface modification and mechanical properties of the compound, gives an overview and clarification of the effect of the resin treatment on the two-dimensional structure treated "Denim fabrics" thereafter. It is obvious that the crossing of the yarns and the constraints of weaving on fabric have a notable effect on the treatment of the "fabric-resin" structure and subsequently on the final quality of the finished article. For this reason, we are looking for a correlation between the treatment processed by the resin (currently) and that treated fabric (in the future). The aim of this study is to predict the effect of glyoxalic, acrylic resin and the mixture of the two resins at different proportions, on the mechanical properties of different conventional cotton yarns; simple TY, sized TF and stretch yarnYE at different process conditions; drying temperature, drying time and curing temperature and time.In this way, we investigate first thermal properties of used resins in order to evaluatethe influenceof the resin action and the finishing conditions on treated yarns.Acharacterization of surface morphology allowedto describe changes surface and understandingthe resins treatment concept. In that case, we have determinate the mechanical behavior (breaking tenacity and elongation, creep and relaxation rate) for the treated yarns. After that,for all yarns studied, we identified the main effect and the interaction of breaking tenacity and breaking elongation with others variables using design of experiments (DOE).The appreciation of yarn mechanical properties and used design of experiments allow us to identify relevant finishing parameters and determine appropriatetreatment conditions.

Materials and Methods

Three cotton yarns were studied. Thereare commonly used as warp and the weft in theDenimwoven structure. In experimental, choosing a sized yarn is objectively in this study,because in manufacturing finishing textile, the majority of denim fabrics aretreated with resin after sewing phase.The warp yarn in denim structure is sized beforestraight weaving phase (with starch or other).In this way, we select a sized yarn to investigate his thermal and mechanical behavior with resin in this structure (before weaving). More details of used yarns are given in (Table I).

Table I: Properties of the yarns

Yarn code Yarn Composition Ne

Twist (turns/meter)

Breaking Tenacity (cN /tex)

Breaking Elongation (%)

TF 100% sized cotton 12 470 18,05 6,44

TY 100% cotton 14 470 15,06 8,75

YE 95% cotton+5% Elasthanne 24 520 17,62 12,12

We used two types of finishing resin. These resins are usually used for fixing treatments of denim garments, permanent press and

wash and wear treatments. More details of used resin and catalysts gives in (Table II).


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Table II: Basic properties of resins and catalysts

Resin pH

(20°C) Viscosity

(cPo) (20°C)

Density

Resin description

Catalyst

Catalyst description

glyoxalic 3 - 5,5 184 1,3

Modified DMDHEU (Diethylene glycol 15 – 22 % and Formaldehyde < 0,1%, and methanol < 0,5 %) crosslink at

140°C

MG contains magnesium chloride

: MgCl2

acrylic 5,5 -7,5 107 1 co-polymer self crosslinked, crosslink at 100°C

PAZ

Water dispersion anionic, soluble of reticulate agent .It’s totally y free of thoxylatealkylphenoles, plasticizing agents

In addition, Acrylic resin may form ester links with cellulose chains as shown in Fig. 1.

Fig.1: Crosslinkage reaction of cellulose with acrylic resin at (95-140°C) for 5 min and pH at 7. (P. Ghos& D.Das, 2000)

In order to investigate the influence of resin characteristic and finishing conditions on mechanical and surface properties of cotton yarns, surface morphology of untreated and treated yarns was examined by SEM Hitachi SU 3500. A spit coater was utilized to precoat conductive gold onto the surface before examine the microstructure at 22 kV. The mechanical properties including breaking strength and breaking elongation of treated yarns are evaluated with LLOYD LS5 tensile tester according to the standard ISO 2062 (2014). Creep and relaxation testes of the treated yarn were performed in the following conditions: A loading speed of 100 (mm/min) and keeps time of 10 (min.)were used. A creep stress maintained at 5 (N)during 10 (min.) withloading speed of 100

(mm/min). DSCcalorimetric (PEP6)device was used to analyze treated cotton yarns and Thermogravimetric analysis (TGA 4000)was used for resin’s thermal analysis. All yarns were conditioned during 24 hours in a relaxed state (22°C, 60% RH) according to the standard ISO 13934-1. For the resin treatment, we used a pad dry cure process.The yarn is impregnated in a bath containing adiluted resin solution with a specific catalyst (20% resin + 80% water). Catalysts MG (magnesium chlorite) and catalyst PAZ have a proportion of 15% of resin weight. We have used design of experimentsshown in (TableIII).

Table III: Design of experiments DOE (7 factors / 3 levels).

Level Yarn composition Resin Resin

concentration % Dry temperature

TS (°C) Dry time DS (min)

Curing temperature TP

(°C)

Curing Time DP

(min)

L 1 100% sized cotton P1 10 80 1 120 5

L 2 100% cotton P2 30 90 3 140 10

L 3 95% cotton+5%

Elasthanne P3 60 100 5 160 20

P1: Glyoxalic resin, P2: Acrylic resin, P 3: Mixed resin (P1+ P2) In experimental, the yarn samples are impregnated in a bath containing a diluted resin solution; resin, catalyst (20% of resin weight) and water. Drying is carried out in a ream (HVF Mathis AG-Swisserland), while the curing step is realized in a drying

oven.So as to preserve uniformity and improving applied the resin to the treated yarns. Preliminary tests were carried out to get the same rate of add-on (70%) on the treated yarns for each condition of the experimental design.


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It is known that the quantity of catalyst used in a reaction depends on the reactivity of the reactants and the time and temperature of curing. Catalyst types, the amount of catalyst, or the temperature and time of curing are factors that can be varied to assist them in improving their reactivity. Conversely, reactants that have a high reactivity have less need for a strong catalyst and/or high temperature and longtime curing than do low reactivity reactants. Temperature and time of curing not only affect the rate of reaction but also affect yellowing of cellulosic fabrics(C.Q.Yang, 1991 & al, 2000). In this study, we have varied a curing temperature between 120°C and 160°C and curing time between 5and 20minutes. Other

factors that we select in (DOE) are shown in Table 3. In reality, too much temperature and time of curing may burn cellulosic fabrics and cause them to yellow. A temperature of 180 °C is normally used as the curing temperature for application of formaldehyde-free durable press. C.Q.Yang& al, (2000) Weselectaresin concentration equivalent 60 g.l-1 is explicit like upper limit. Itpurposes to inspect the effect of higher resin concentration on the surface, thermal and mechanical properties of treated cotton.To reduce the number of (DOE), we applied the Taguchi orthogonal array design for each yarns shown in (TableIV).

Table IV: Taguchi orthogonal array design L27 (3**7) Index yarns of resin

treatment i Resin Resin

concentration %

Dry temperature TS (°C)

Dry time DS (min)

Curing temperature TP (°C)

Curing TimeDP (min)

1 P1 10 80 5 160 20 2 P1 10 80 3 140 10 3 P1 10 80 1 120 5 4 P1 30 100 5 120 10 5 P1 30 100 3 160 5 6 P1 30 100 1 140 20 7 P1 60 90 5 140 5 8 P1 60 90 3 120 20 9 P1 60 90 1 160 10 10 P2 10 100 5 140 5 11 P2 10 100 3 120 20 12 P2 10 100 1 160 10 13 P2 30 90 5 160 20 14 P2 30 90 3 140 10 15 P2 30 90 1 120 5 16 P2 60 80 5 120 10 17 P2 60 80 3 160 5 18 P2 60 80 1 140 20 19 P3 20 (25+75) 90 5 120 10 20 P3 20 (25+75) 90 3 160 5 21 P3 20 (25+75) 90 1 140 20 22 P3 20 (50+50) 80 5 140 5 23 P3 20 (50+50) 80 3 120 20 24 P3 20 (50+50) 80 1 160 10 25 P3 20 (75+25) 100 5 160 20 26 P3 20 (75+25) 100 3 140 10 27 P3 20 (75+25) 100 1 120 5

P1: Glyoxalic resin, P2: Acrylic resin, P 3: Mixed resin (P1+ P2)

We noted (i) the index yarns of condition resin treatment, so we used for sized cotton yarn TFi, the unsized one TY i and YEi for the stretch yarns. The mean to investigate the crosslinking concept on treated cotton yarns, as well compare the specific effect of resin treatment and finishing conditions on the surface, thermal and mechanical properties (creep and relaxation test) of treated cottons yarns, we select a number of treated samples 1,9,12 and 24 from (Table IV). These indexed samples, presents a various factors of finishing conditions (resin nature, resin concentration, curing time and temperature, dry time and temperature).

Results and Discussion

Thermal analysis of used resin and treated cotton yarns with TGA

The aim of resins characterization is toanticipate their behavior towards finishing conditions and to determineappropriated curing temperature. Indeed, the curve of TGA shown in (Fig.2)presents the weight loss of the resins depending on temperature. The Acrylic resin presents a weight loss of 60% between 25°C and 140°C. The declined curve was finished by aninflection point at 100°C. From 140°C the weight stabilizes until 370°C, there will be the degradation of the neat resin remaining for higher temperature near 400°C. Moreover, for the glyoxalic resin, TGA curve presents a weight loss of 40% of initial weight between 25°C and 140°C progressively. The weight lossdeclined weakly and finished by aninflection pointat 180°C a value of 50%.We can observe that acrylic resin is subjected to chemical dissociation faster than glyoxalic resin temperature greater than 100 ° C.The acrylic resin starts itsself-crosslinked from 100 °C and then glyoxalic resin requires higher temperature 140 °C to crosslinking.


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50 100 150 200 250 300 350 400 450 500 550 600 650

0

20

40

60

80

100

Wei

ght l

oss

resin

(%)

Temperature (°C)

acrylic

glyoxalic

Fig. 2:Weight loss of glyoxalic resin and acrylic resin depending on temperature.

Shown in (Fig.2) the weight loss obtained for the resins between 100°C and 160°C corresponds to the endothermic peak of the heat flow depending on the temperature in (Fig.3). This result corresponds to breaking of chemical bond between resins

constituent and release gas. Theexothermic peak observed between 420°C and 600°C that express the degradation of the pure cross linking agent. Moreover, Acrylic resin requires a heat flow of 660°C, while glyoxalic exchange resin required a heat flow of 150°C.

50 100 150 200 250 300 350 400 450 500 550 600 650 700

-400

-200

0

200

400

600

800

Heat

flow

(mw)

Temperature (°C)

acrylic

glyoxalic

Fig. 3: Heat flow of glyoxalic resin and acrylic resin depending on temperature.


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50 100 150 200 250 300 350 400 450

-2

-1

0

1

2

3

4

5

6

7

8

9

Heat

flow

(m

w)

Temperature (°C)

untreatedTF

yarnTF1

yarnTF9

yarnTF12

yarnTF24

50 100 150 200 250 300 350 400 450

-2

-1

0

1

2

3

4

5

6

7

8

9

10

Heat

flow

(m

w)

Temperature (°C)

untreatedTY

yarnTY1

yarnTY9

yarnTY12

yarnTY24

(a) (b)

50 100 150 200 250 300 350 400 450

-2

0

2

4

6

8

He

at flo

w (

mw

)

Temperature (°C)

UntreatedYE

yarnYE1

yarnYE9

yarnYE12

yarnYE24

(c)

Fig. 4: DSC curves of untreated and treated yarns with resins; (a) sized treated yarns (b) treated cotton yarns, (c) stretched treated yarns. The analysis of DSC curve shown in (Fig.4a, b,c) illustrated the data of the thermal behavior of untreated and treated yarns. The DSC curves of treated sized yarn and untreated yarn presentaslightly endothermic peak near 87°C which defines inflexion pointof TF sized yarns (cotton with starch).The transition from the metastable state to the non-equilibrium state is through the passage of a glass transition temperature (Tg) when the disorder of macromolecular chains begins.In this manner, for the treated cotton yarn, the endothermic peak appears at 78°C which defines (Tg) of cotton. Indeed, from the glass transition temperature begin the evaporation of the rest water and promotes the chemical links inside of chemical network. In fact, the changes observed in the DSC curves indicate the suppression of additive resin products. As seen in (Fig.4)adissimilar endotherm is visible between 75°C and 88°C for all treated yarn.Thisresult probably is due to resin treatment effect on the glass transition temperature of cellulose. In the case of untreated cotton, the DSC curve exhibits an exothermic peak at about 340°C, generally associated with the formation of volatile products during the decomposition of the cellulose. Particularly, for the yarnsTF1 and TF12 shown in (Fig.4.a) and TY1 in (Fig.4.b), the DSC curves havea higherheat flow. This result is probably due to influence of curing temperature at 160°Cin the cellulose-resin network,while for the other treated yarns, the DSC curve is below than untreated cotton.The

DSCcurves in the case of all treated cotton yarnshave a change on chemical structure.Researchers have seen that cotton treated with flame retardant finishing have two picks near 340°C and 470°C compared to untreated cotton in DSC curve D. Katović& al,(2012). In our case for all the treated yarns, a DSC curves deviation appears between 320°C and 380°C. Thismay be explained by the effect of heat on the progression of cross linking agent release.In fact, the quantity of chemical agent released is different depending on the initials finishing conditions. Shown(Fig.4,b) we can observe that all treated sized yarns TFi have a dissimilar glass transition temperature ‘Tg’ between 70°C and 75°C.This is probably due to the resin effect.The new physical state may be the result of the finishing conditions that affect the yarns properties compared to the untreated yarns. According to the (Fig.4.a,4.b),Near 300 °C, it observe that for all treated yarns an inflection point in aspect of DSC curve confirming the change in internal structure of the resin-fiber has more action with the cellulosic chains. We can observe that for the yarns TY1 and TF1 having a curing time 20 minutes superior to other treated yarns, this differentiation is noteworthy on the DSC curves as they exhibit larger exothermic picks, may explain the effect of curing time on the thermal history of processed fibers.C. E. Jr. Warburton (1972)noted that self-condensation of N-methylol compound is the preponderant chemical reaction when a film with (70% methacrylic


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acid /30% ethylacrylate) copolymer and DMDHEU is heated an exotherm is observed under definite conditions in DSC thermograms of films include DMDHEU and is credited to a quickmove of methylene either to methylene link. Esterification of polymer by methylol reagent probably also occurs to a limited extent, especially above about 160°C.Comparing the DSC curve of TYi and TFi shown in (Fig.4.a, b) we can conclude that they are different.Almost, the causeof starch effectis apparentin the yarns properties. The sized yarn resists better to the penetration of crosslinkers in the cellulose amorphous zone. The(Fig.4, c) presentsDSC curves of untreated and treated yarns YE with resins. It’s clear that DSC curve of stretched yarns have the same characteristic of others treated yarns shown in (Fig.4, a, b).An endothermic peak appears between 70°C and 75°Cthat may be make clear a change of cotton glass transition temperature. In the first part, between 25°C and 300°C the DSC curve of stretched yarns are similar to DSC curve of untreated one. All treated YE

yarns have a DSC curve upper the DSC of untreated yarn. The DSC curve of stretched yarns near 300°C C have an inflection point and an exotherm peaks appear after 350°C. For the untreated and samples YE1and YE12 have a similar outward appearance of DSC curve. While, for YE1and YE12 DSC curve have a necessity of heat flow less that untreated sample. This change is probably due to the glyoxalic and acrylic resin effect on cellulosic chain structure. In addition, the samples YE1and YE12 have anequal resin concentration 10%, but they have a dry and curing time and dry temperature different. This results confirmed that finishing time is a significant factor effecting the thermal behavior of stretched yarns YE. For treated sample YE24 with mixed resin P3, it has a DSC curve with minimum of heat flow compared with others untreated and treated samples.It may clarify that P3 resin has a thermal behavior similar to glyoxalic resin with majority of treated yarns shown in (Fig.4a, b, c).

Surface Morphology

Fig.5: a. Untreated yarn TF Fig.5: b. Treated yarn TF 1 Fig.5: c. Treated yarn TF 9

Fig.5: d. Untreated yarn YE Fig.5: e. Treated yarn YE 1 Fig.5: f. Treated yarn YE 9


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Fig.5:i. Untreated yarn TY Fig.5: j. Treated yarn TY 1 Fig.5: h. Treated yarn TY 9

Fig. 5: Surface morphology of untreated and select treated yarns

(Fig.5) presents SEM pictures showing surface morphology of treated untreated yarns. The surface aspect has clearly changed after treatment and there are traces of cracking and split on the yarn surface that is especially due to resin treatment effect. Acrylic resin presents a coating film on the surface of the fibers and between fibers. In literature, some researchers observed the similarresultsC.Q.Yang, (1996). Indeed, the resin concentration effect it’s clear according to SEM pictures in (Fig.5.c and 5.h) for a concentration of 60 g.l-1. The resin had a cover appearance on the fibers and occupies the spaces between fibers as shown in (Fig.5.b and 5.j).In this case, concentration is 10 g.l-1 and curing time is 20 minutes and cracks happen on the surface of sized cotton yarns (TF1). Shown the picture (Fig.5, f) for YE yarns, we can report that,for a concentration 60 g.l-1 and a curing temperature 140 °C, Acrylic resin aspect a more visible and cover the surface clearly. The same observation for previous picturesin (Fig.5, h) for TY yarns.According to picturesin (Fig.5, e, j), it can report that,

glyoxalic resin has a stronger negative effect on stretch YE yarn as TY cotton yarn viewpoint fiber crack. This effectmay be due to curing conditions. According to all pictures, the glyoxalic resin had an important negatively effects on mechanical behavior that Acrylic resin.This result is confirmed applying ahigher concentration and curing temperature. It is clear thathard physical conditions of cross linkingmake easy the penetration of resin in particular for stretch yarns but make the material brittle. This may beduetothe slippage and breakage consequence of the cellulose chains.

Mechanical behavior of treated cotton yarns In order to understand the effect of resins on mechanical

properties, the breaking tenacity and breaking elongation for sized yarn TF, stretch YE and unsized TY treated cotton yarns are presentedin (Fig.6).

1 3 5 7 9 11 13 15 17 19 21 23 25 27

8

10

12

14

16

18

20

Brea

king

tena

city

(cN/

tex)

Resin treatment index (i)

TFtenacity

TYtenacity

YEtenacity

(a)


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1 3 5 7 9 11 13 15 17 19 21 23 25 27

4,5

5,0

5,5

6,0

6,5

7,0

7,5

8,0

8,5

9,0

9,5

10,0

10,5

11,0

11,5

12,0

12,5

13,0

13,5

Brea

king e

longa

tion (

%)

Resin treatment index (i)

TF

TY

YE

(b)

Fig.6: Breaking tenacity (a) and Breaking elongation (b) of TF, TY and YE treated yarns with resins.

The resin finishing of various cotton yarns treated with glyoxalic resin (modified DMDHEU), caused a strength loss and elasticity change.This change isverysignificant on TY and YE yarns, according to different researches (T. Waichiro 1971, T. L. Vigo, 1994.A.D.Vahid& al, 2012). Researchers noted that the treatment of cellulosic material by formaldehyde free containing glyoxalic resin as a durable press agent has two drawbacks: increasing strength loss and yellowing of treated fabric (C.M Welch & G.F. Danna, 1983). When cellulose is crosslinked, it naturally becomes less able to distribute stresses and strains imposed on fiber during mechanical deformation. Also the introduction of crosslink imparts dimensional stability to the fiber material and makes it more resistant to creasing, which restricts the movement among the fibers and yarns. Whereas, for yarn treated with acrylic resin, the tenacity remains slightly unchanged or increases more than anuntreated control yarn. The acrylic finishingproceeds as a plastic film coveryarn surface and make it harder and less extensible (R. Cheriaa &A. Baffoun, 2015). It is known that polyacrylate can block the space between the fibers and attach them together, which avoid the movement of the fibers.Researchers make clearly this change(S. Dannie & G. K. Stylios, 2012). Concerning sizedyarns, alltreated yarns present slightly lower tenacity compared to untreated yarn. This result isprobably dueto the poor penetration of resin monomer into fiber structure. Shown in (Fig.6), It observe that in the case of P1 and P3 resins have a negative effect consisting of a loss of tenacity and breaking

elongation for most conditions with low and high concentration.Theresin P2 allows a gain tenacity of about 4% for TF, 14% for TY and 7 % for YEwhen compared to untreated yarns. In addition P2 causes an elongation loss, of 7 % for TF yarn, 14 % for TY yarn and 18% for YEyarn when they compared to untreated yarns.It is clear that the treated stretch cotton yarn YE at different conditions shows the most notable loss of tenacity when compared to other treated yarns. On the other hand, the variation of mechanical properties loss with P1 or P3 is not dependent only of glyoxalic resin concentration which is 60 gl-1 a factor favoring the loss of mechanical properties but also on curing temperature and curing time, which are very influential factors on the cross linking reaction and therefore on the mechanical properties of yarns. The tenacity loss obtained can be explained byinter-molecular cross bond formation that reduces the possibility of equalize the stress sharing, which causes the reduction of the capability to resist the load(E. Edwin Sunder & G. Nalankilli, 2012). Researchers noted that approximately 20% of strength loss source from the cross linking. Such as strength loss can be minimized by curing conditions that reduce the intra-molecular crosslink in fibers. As we know, the fibre strength depends not only on cellulose macromolecular weight, but also on fibre crystallinity will contribute greatly to fibre strength (Xu Weilin,2003). The effect of various finishing resins on tenacity and elongation forall treated yarnsis presented in (TableV).

Table V: Effect of finishing resins on yarns tenacity and elongation.

P1 P2 P3 P1 P2 P3

TF ○ ○ − ○ ○ −

TY − ++ + − − ∆

YE ∆ ○ ∆ ∆ ∆ −

Effect on the yarn tenacity Effect on the yarn elongation

− Weak negative effect, ○ without effect, ∆ strong negative effect,+ Medium positive effect, ++ strong positive effect

An important loss of tenacity is obtained for stretch yarn and then comes the treated cotton yarn, while the minimum loss is obtained with sized yarn. This difference can be explained by the inter-fiber cohesion inside yarn structure and the initial mechanical properties. The loss of tenacity is important for the stretch yarn and it is due to its brittle structure against the effect of cross linking. In the case

of the yarns treated with acrylic resin, the finishing agent reinforces the inter-fiber cohesion and reduces the inter-fiber slippage. Y.Shin & al, (1989) noted two major factors contributing to the loss in mechanical properties: fiber degradation caused by the acid catalyst at elevated temperatures; and the restriction of stress distribution within the fibers due to their rigid cross linking

http://www.sciencedirect.com/science/article/pii/S0144861712002743


3627

by monomeric resins. Other researchers developed the wet fixation process for improving the retention of mechanical properties in finished fabrics (N.R.S. Hollies& N.F. Getchell, 1967). To better understand the effect of finishing agents on yarn mechanical properties, we studied the creep and relaxation

behavior of treated yarns at various resintreatment. We choose the resin treatment index 1, 9, 12 and 24 from the (TableIV). Obtained results are shown in(Fig.7, a)for creep test and (Fig.7, b) for relaxation test of treated yarns.

untre

ated

TF

TF1

TF9

TF12

TF24

untre

ated

TY

TY1

TY9

TY12

TY24

untre

ated

YE

YE1

YE9

YE12

YE24

0,0

2,0x10-6

4,0x10-6

6,0x10-6

8,0x10-6

1,0x10-5

1,2x10-5

1,4x10-5

1,6x10-5

1,8x10-5

2,0x10-5

Cre

ep r

ate

(m.s

-1)

Sample code

Creep.ratem

(a)

untr

eate

d T

F

TF

1

TF

9

TF

12

TF

24

untr

eate

d T

Y

TY

1

TY

9

TY

12

TY

24

untr

eate

d Y

E

YE

1

YE

9

YE

12

YE

24

0,000

0,001

0,002

0,003

0,004

0,005

0,006

0,007

Rel

axat

ion

rate

(N

.s-1

)

Sample code

relax.ratem

(b)

Fig.7:Creep rate (a) and relaxation rate (b) of treated yarns at different finishing condition

Referring to (Fig.7 a, b)and for the same finishing conditions, it's clear that treated yarns TF, TY and YE have a creep and relaxation rate less that untreated yarns. In addition, the treated sized yarns TF have lower creep rate and higher relaxation rate than that of treated cotton yarn TY and stretched yarn YE. This may be due to the effect of the starch on the surface of yarn which promotes the reinforcement of yarn and minimizes fiber slippage inside of yarn. The destruction of bonds, the slippage between the macromolecules and the internal friction retarding the deformation are the main causes of creeping.According to (Fig.7 a, b) we canobserve that the creep rate for the TY yarn,is twice more important that in the case of TF sized yarn.The relaxation rate of the sized yarn, is twice more important that in the case of TY yarn. This result can be due to starch effect on yarns outline that

improve the inter-fiber blocking reaction and intra-fiber sliding which induces the adhesive effect. Besides, for treated yarns YE, they have the higher amount creep rate compared to other treated yarn.However, treated yarns YE have a smallest amount relaxation rate compared to other treated yarn. This result can be to the concept of stretch yarn that contains an elastic polymer.

Main effect and interaction plot of resin treatment parameters

Using MINITAB® software was to investigate the effect of resin type, resin concentration, curing temperature and time, drying temperature and time on the mechanical properties(breaking tenacity and elongation) of treated yarns.


3628

Me

an

of T

F T

en

acit

y (

CN

/te

x)

321

17,40

17,25

17,10

16,95

16,80

60302010 1009080

531

17,40

17,25

17,10

16,95

16,80

160140120 20105

Resin Type Resin Conc. % TS (°C)

DS (min) TP (°C) DP (min)

Main Effects Plot (data means) for TF Tenacity (CN /tex)

Me

an

of

TF B

re

ak.E

lon

g.

(%

)

321

6,00

5,85

5,70

5,55

5,40

60302010 1009080

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6,00

5,85

5,70

5,55

5,40

160140120 20105



Main Effects Plot (data means) for TF Break.Elong. (%)

A b

Me

an

of

TY

Te

na

cit

y (

CN

/te

x)

321

17

16

15

14

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17

16

15

14

160140120 20105



Main Effects Plot (data means) for TY Tenacity (CN /tex)

Me

an

of

TY

Bre

ak.E

lon

g.

(%

)

321

7,6

7,2

6,8

6,4

6,0

60302010 1009080

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7,6

7,2

6,8

6,4

6,0

160140120 20105



Main Effects Plot (data means) for TY Break.Elong. (%)

C d

Me

an

of

YE T

en

acit

y (

CN

/te

x)

321

16

15

14

13

12

60302010 1009080

531

16

15

14

13

12

160140120 20105



Main Effects Plot (data means) for YE Tenacity (CN /tex)

Me

an

of

YE

Bre

ak.E

lon

g.

(%

)

321

10,5

10,0

9,5

9,0

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10,5

10,0

9,5

9,0

160140120 20105



Main Effects Plot (data means) for YE Break.Elong. (%)

E f

Fig. 8: Graphic of main effect of breaking tenacity and breaking elongation for treated yarns.

Referred to(Fig.8),that presents the main effect plot of the breaking tenacity and elongation for treated yarns. It is clear that the resin type, resin concentration, curing temperature TP and curing time DP, drying temperature DS and drying time TS have a significant

effect on the breaking tenacity and breaking elongation of different treated cotton yarns TF,TY and YE. It is clearly that glyoxalic resin effect more than acrylic resin on the mechanicals properties; breaking tenacity and elongation unreliable to characteristic yarns.


3629

These results are completely in conformity with the experimental results where we showed previously on the mechanical behavior of treated cotton yarns as well the results of creep and relaxation behavior of treated cotton yarns. The interaction drawing is a representation of the answers information averages for every factor level. The level of the second

factor stays constant. This diagram is helpful to reviewer the presence of interaction. An interaction is present if the answer for a parameters level depends on/or the other parameters levels. In a diagram of the interaction, some parallel lines designate the absence of interaction (C.R. Hicks, 1982). More the lines depart of the parallel; more the degree of interaction is elevated.

Resin TypeResin Type

TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)

Resin Conc. %Resin Conc. %

60302010 1009080 531 160140120 20105

18,2

17,2

16,218,2

17,2

16,218,2

17,2

16,218,2

17,2

16,218,2

17,2

16,2

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for TF Tenacity (CN /tex)


TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)


60302010 1009080 531 160140120 20105

6,0

5,6

5,2

6,0

5,6

5,2

6,0

5,6

5,2

6,0

5,6

5,2

6,0

5,6

5,2

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for TF Break.Elong. (%)

A B


TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)


60302010 1009080 531 160140120 20105

18

16

14

18

16

14

18

16

14

18

16

14

18

16

14

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for TY Tenacity (CN /tex)


TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)


60302010 1009080 531 160140120 20105

8

7

6

8

7

6

8

7

6

8

7

6

8

7

6

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for TY Break.Elong. (%)

C D


3630


TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)


60302010 1009080 531 160140120 20105

16

12

8

16

12

8

16

12

8

16

12

8

16

12

8

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for YE Tenacity (CN /tex)


TS (°C)TS (°C)

DS (min)DS (min)

TP (°C)TP (°C)

DP (min)DP (min)


60302010 1009080 531 160140120 20105

12

10

812

10

812

10

812

10

812

10

8

Resin

3

Type

1

2

Resin

30

60

Conc.

%

10

20

TS (°C)

100

80

90

DS

5

(min)

1

3

TP (°C)

160

120

140

Interaction Plot (data means) for YE Break.Elong. (%)

E F

Fig.9: Graphic of interaction plot of breaking tenacity and breaking elongation for treated yarns.

Refereed to (Fig.9), that present graphic of interaction plot of breaking tenacity and breaking elongation of various treated yarns. It is apparent that we have an interaction in each response (forvarious treated yarns).We could see that all DOE response; resin type, resin concentration, TP , DP, DS and TS have a significant interaction between them in action on the breaking tenacity and breaking elongation of TF,TY and YE yarns.

Conclusion

In this paper, we have investigated the effect of glyoxalic and acrylic resin at various finishing conditions. This study allowed establishing the effect of resin treatment on the mechanical (breaking tenacity and elongation) and surface properties of various cotton yarns. It has been shown that for glyoxalic resin the treated sized yarn with starch is more resistant than treated simple yarn or stretch yarn. We have identified the main effect plot and asignificant interaction between different parameters of resin treatment. Besides, the design of experiments allows determining the optimal finishing conditions (resin concentration, curing temperature, curing time, dry time and dry temperature) for a better resin treatment with the minimum loss in mechanical properties of treated cotton yarn. These findings have a practical interest and allow forecasting the effect of resins on cotton denim fabrics before treatments.

Acknowledgements

The authors would like to thank, especially of Chimitex Plus Company, and the team of Sitex Company for providing materials for investigation. Finally, sincere thanks are also addressed to the scientific team of Textile Physics and Mechanics Laboratory (LPMT) for their support.

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