REZUMAT – ABSTRACT

The behavior in finishing of textile materials made of man-made fibers containing ZnO in blends with cotton

DOI: 10.35530/IT.069.03.1477

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REZUMAT – ABSTRACT

Comportamentul la finisare al materialelor textile realizate din fibre artificiale cu conținut de ZnO în amestecuri cu bumbac

Obiectivul acestui studiu a fost de a investiga comportamentul la finisare al materialelor textile realizate din fibre artificiale cu conținut de ZnO în amestec cu bumbac. Au fost studiate posibilitățile de reducere a concentrației agenților chimici considerați a fi agresivi pentru fibrele textile funcționale, temperatura çi durata proceselor, precum çi numărul operațiilor tehnologice efectuate, astfel încât calitatea vopsirii să nu aibă de suferit, iar probele vopsite să fie acceptabile din punctul de vedere al uniformității çi al rezistenței vopsirii. Pentru a evidenția influența auxiliarilor chimici utilizați în operațiile de finisare, temperatura procesului, pH-ul çi durata tratamentului asupra caracteristicilor fizico-chimice çi fizico-mecanice ale fibrelor funcționale, s-au aplicat diferite metode de tratare preliminară çi vopsire în diferite variante experimentale. Pentru evaluarea performanțelor tratamentelor preliminare din punctul de vedere al gradului de alb çi al hidrofiliei, țesăturile au fost testate înainte çi după efectuarea tratamentelor preliminare. În scopul determinării eficienţei tratamentelor realizate, ţesăturile finite (tratate preliminar çi vopsite) au fost testate din punctul de vedere al diferenței de culoare çi al rezistenței vopsirii. Țesăturile finite au fost, de asemenea, caracterizate din punctul de vedere al principalelor caracteristici fizico-chimice çi fizico-mecanice: masa, rezistența la tracțiune, rezistența la rupere, perme- abilitatea la vaporii de apă, permeabilitatea la aer. Analiza SEM a fost utilizată pentru a investiga morfologia de suprafață a țesăturilor tratate. Activitatea antibacteriană a probelor tratate a fost testată împotriva tulpinii test Staphylococcus aureus.

Cuvinte-cheie: fibre funcționale, tratament de finisare preliminară, proprietăți fizico-mecanice-chimice, activitate antibacteriană

The behavior in finishing of textile materials made of man-made fibers containing ZnO in blends with cotton

The objective of this study was to investigate the behavior in finishing of textile materials made of man-made fibers containing ZnO in blends with cotton. It has been studied the possibilities of reducing the concentration of the chemical agents considered to be aggressive for the functional textile fibers, the temperature and the duration of the processes, as well as the number of technological operations performed, so that the dyeing quality will not suffer and the dyed samples to be acceptable from the uniformity and fastness point of view. To highlight the influence of the chemical auxiliaries used in finishing operations, the process temperature, pH and the treatment duration on the phys- ical-chemical and physical-mechanical characteristics of the functional fibers, various methods of preliminary treatment and dyeing were applied in different experimental variants. In order to assess the preliminary treatments performance from whiteness degree and hydrophilicity point of view, the fabrics were tested before and after preliminary treatments. Finished fabrics (preliminary treated and dyed) were tested for the efficiency of the performed treatments in terms of color difference attributes and color fastness. The finished fabrics were also characterized in terms of the main phys- ical-chemical and physical-mechanical characteristics: mass, tensile strength, tearing strength, water vapor permeability, air permeability. SEM analysis was used to investigate the surface morphology of treated fabrics. Antibacterial activity of treated samples was tested against the Staphylococcus aureus test strain.

Keywords: functional fibres, preliminary finishing treatment, physical-mechanical-chemical properties, antibacterial activity

INTRODUCTION

Textile industry continuously searches for new tech- nologies in order to accomplish the consumers’ demands. Especially in recent years, new develop- ments allowed the production of functional and smart textiles which are capable of sensing changes in environmental conditions or body functions and responding to these changes. As a consequence, the number of bio functional textiles with an antimicrobial activity has increased considerably over the last few years [1–3]. Several major classes of synthetic

(quaternary ammonium compounds, silver, polyhex- amethylene biguanides (PHMB), triclosan) or natural antimicrobial agents (chitosan, plant extracts, essen- tials oils) are used in the textile industry in order to control the bacterial growth efficiently and to keep its durability [4–9].

Antimicrobial agents can be applied to textile by dif- xxxxxx methods such as pad-dry-cure, coating, spray- ing and foam techniques. It can also be applied directly by adding the antimicrobial agent into the spin- ning fiber solutions. Development of antimicrobial

fibers is based on the process of incorporating active antimicrobial agents into the fiber in its manufacturing stage and this technology is rather increasing today, mainly being supported by fiber manufacturers [10]. Some commercial bioactive fibres with antimicrobial agents and finishing products are: SeaCellR Active, a cellulose-base fibre; MicroFresh®, SoleFresh® and Guard-Yarn®, polyester or nylon yarns with Alpha San®, a zirconium phosphate-based ceramic ion- exchange resin containing silver; Trevira Bioactive®: polyester fiber with silver incorporated prior to the extrusion process; SmartSilver®, wool fibers with sil- ver added by typical exhausting dyeing methods and other finishing silver-based products like Smart

Italy) was used as stabilizer agent for H2O2 and Sequion 48/98 (Xxxxxxxx Xxxxxxx S.p.a, Italy) was used as a dispersant and sequestrant for calcium, magnesium and iron ions. Sirrix SB (Clariant), a multi-action anionic product, has been used as a dis- persant for fatty impurities, oxygen active generator, activator and stabilizer for H2O2. For pre-treatment operations performed at low temperatures, Imerol LTB (Archroma) was used, a chemical product espe- cially designed for the low temperature bleaching process, having superior wetting and removal prop- erties of fatty impurities, oils, accidental pigments and high emulsifying properties of impurities, and as

H O stabilizing agent was used the product formu-

Silver™, SilpureR, Sanitized®, AlphaSan® and Ultra- 2 2

Fresh. Cotton fibers are also being commercialized under a pre-treatment with ReputexR (PHMB attached to cotton) and more recently, polyamide with PHMB is sold as Purista®. Moreover, polyamide and polyester fibers treated with Tinosan AM 100®, cellu- lose acetate yarns named Silfresh®, Microban® tex- tile and Irgaguard® and Irgacare® products, all con- tain triclosan as antimicrobial agent [11].

Smartcel™ Sensitive fibers developed by Smartpolymer (Germany) are Lyocell fibers that have integrated ZnO into their matrix for skin protection and skin care, produced without aggressive chemical agents for the skin [12]. Textiles materials containing these novel zinc fibers allow natural, soft and pure skin care with an additional antibacterial and odor- reducing effect. The antibacterial effect of zinc is based on the “oligo dynamic effect” which describes a disruption in the antibacterial metabolism.

For the finishing of textile materials made of function- al fibers have to pay special importance on every technological process involved in the technological flow of finishing, so that the additives contained in the fiber structure, giving them functionality, are not elim- inated by the finishing, dyeing or final finishing pro- cedures applied. In this respect, the specific objective of this study was to investigate the behavior in finish- ing of textile materials made of man-made fibers con- taining ZnO in blends with cotton. It has been studied the possibility of reducing the concentration of the chemical agents considered to be aggressive for the functional textile fibers, the temperature and the dura- tion of the processes, as well as the number of tech- nological operations performed, so that the dyeing quality will not suffer and the dyed samples to be acceptable from the uniformity and fastness point of view.

EXPERIMENTAL WORK

Materials

For laboratory experiments 80% cotton/20% Smartcel™ Sensitive (with ZnO content) plain weave fabric with 290 yarns/10cm in warp and 230 yarns/10cm in weft, 246 g/m2 weight was used. For preliminary finished operations Kemapon PC/LF (Kem Color S.p.a, Italy) or Imerol JFS (Clariant) was used as wetting and detergent agents. Kemaxil Liq (Kem Color S.p.a.,

lated for low temperature process, Stabilizer LTB (Archroma).

Preliminary treatments

To highlight the influence of the chemical auxiliaries used in finishing operations, the process tempera- ture, pH and the duration treatment applied, on the physical-chemical and physical-mechanical charac- teristics of the functional fibers, various methods of preliminary treatment and dyeing were applied, in dif- xxxxxx experimental variants. Laboratory experiments were performed on the jigger (Roaches-England) lab- oratory apparatus at 1:10liquor ratio (material: liquor ratio), as follows:

• Strong alkaline pre-treatment-bleaching in suc- cessive phases (classical process) (Code V1): Alkaline treatment – Bath 1 ® 2 g/L Kemapon PC/LF,

2 g/L Sequion 48/98, 6 ml/L NaOH 38 °Be, 3 g/L trisodium phosphate, 90 minutes, 98 ºC; Bath 2 ® Bleaching: 1g/L Kemapon PC/LF, 2 ml/L Kemaxil Liq,

4 ml/L NaOH 38ºBe, 20 ml/L H2O2 30%; 60 minutes, 98 ºC;

• Mild alkaline pre-treatment-bleaching in succes- sive phases (mild process) (Code V2): Alkaline treatment – Bath 1 ® 2 g/L Kemapon PC/LF, 2 g/L Sequion 48/98, 2 g/L Na2CO3; 45 minutes, 98 ºC; Bath 2 ® Bleaching 1g/L Kemapon PC/LF, 2 mL/L Kemaxil Liq, 2.3 mL/L (pH = 12) NaOH 38 ºBe, 20 mL/L H2O2 30%; 45 minutes, 95ºC;

• Pre-treatment in single phase with a multiple action chemical auxiliary (mild process) (Code V3): 0.5 g/L Imerol JSF, 0.8 g/L Sirrix SB, 2.6 g/L NaOH 38ºBe, 6.5 g/L H2O2 30%; 30 minutes, 95ºC;

• Preliminary treatment – dyeing in single phase with a multiple action chemical auxiliary (prelimi- nary treatment followed by dyeing without intermedi- ate rinsing) (Code V4): Bath 1 ® 0.5 g/L Sirrix SB, 0.8 g/L, 2.6 g/L NaOH 38° Be, 6.5 g/L H2O2 30%; 30 min- utes, 95ºC ® Bath evacuation, without intermediate rinsings ® Bath 2 ® 0.2 mL Sirrix NE, 0.35 g/L Bactosol ARL liq. (catalase) ® adding of appropriate chemicals and dyes for dyeing operation;

• Pre-treatment in a single-phase with low con- centration of chemical auxiliary special formulat- ed for low temperature processes (Code V5) at:

0.5 g/L Imerol LTB, 1g/L Stabilizer LTB, 3 g/L NaOH 38 ºBe, 4 g/L H2O2 30%; 40 minutes, 80 ºC;

• Pre-treatment in a single-phase with higher con- centration of chemical auxiliary special formulat- ed for low temperature processes (Code V6): 1 g/L Imerol LTB, 1 g/L Stabilizer LTB, 6 g/L NaOH 38 ºBe, 4 g/L H2O2 30%; 40 minutes, 80 ºC.

After the preliminary treatment operations the sam-

ples were successively rinsed with water at 90 ºC, 70 ºC, 40 ºC and cold rinsing, except for V4V.

Dyeing operation

After the preliminary treatments, the dyeing operation has been performed by using the following dyeing recipe: 1.5% Drimaren Gelb CL-2R, 70 g/L NaCl (added in two portions), 20g/L Na2CO3 (added in two portions). After dyeing operation the samples were rinsed as follows: warm rinsing at 60 ºC, soaping with 1 g/L Kemapol SR (Kemcolor) at 90 ºC, 20 minutes, rinsing at 80 ºC, 40 ºC, 30 ºC and cold, 10 minutes each rinsing, followed by drying at room temperature.

Methods

Physical-chemical and physical-mecanical characteristics

In order to asses the preliminary treatments perfor- mance, the 80% cotton/20% SmartcelTM Sensitive fabrics were tested before and after preliminary treat- ments in terms of whiteness degree (SR EN ISO 105- J01:2003) and from hydrophilicity point of view by determining the wettability (drop test method accord- ing with SR 12751/1989 standard) and the water absorbency (capillarity test according with SR 6146/1989 standard). Finished fabrics (preliminary treated and dyed) were tested for the efficiency of the performed treatments in terms of color difference attributes (SR ISO 105 J03: 2001) and color fastness to washing (SR EN ISO 105-C10:2010), acid and alkaline perspiration (SR EN ISO 105-E 04: 2013) and light (SR EN ISO 105-B02: 2003).

The finished fabrics were also characterized in terms of the main physical-chemical and physical-mechan- ical characteristics, respectively: mass (SR EN 12127-2003), density (SR EN 1049-2: 2000-Method

A, B), tensile strength (SR EN ISO 13934-1/2013), tearing strength (SR EN ISO 13937-3: 2002), water vapor permeability (STAS 9005: 1979), air perme- ability (SR EN ISO 9237: 1999).

Antibacterial testing

Table 2

The antibacterial activity of the dyed samples and pre-treated in different variants was qualitatively determined according with the ISO 20645: 2004

HYDROPHILICITY FOR 80% COTTON / 20% SMARTCELTM SENSITIVE FABRICS PRELIMINARY TREATED IN DIFFERENT VARIANTS
Hydrophilicity		Code
	Raw	V1	V2	V3	V5	V6
Wettability, drop test [s]	˃ 600	˂ 1	˂ 1	2	˂ 1	˂ 1
Water absorbency [%]	-	58.52	52.44	44.09	45.75	51.65

(E) standard method, by using of cultures in liquid medium replicated at 24 hours of ATCC 6538 Staphylococcus aureus strains (Gram-positive). For determination, the samples were cut in circu- lar shape with a diameter of 2 cm and subse- quently disposed in the middle of Petri plates. The culture medium was poured into two layers in Petri plates, lower layer consists of culture medi- um free from bacteria and the upper layer being inoculated with the test bacteria, then incubated at 37 ºC and analyzed after 48 hours.

Scanning Electron Microscopy (SEM)

The surface morphology of treated samples in differ- ent variants was investigated by a FEI Quanta 200 Scanning Electron Microscope with a GSED detector, at 2000 x magnification and accelerating voltage of

12.5 kV – 20 kV.

Energy Dispersive X-ray analysis (EDX)

EDX was used to identify the presence of Zn in tex- tile materials. The analysis was made with a FEI Quanta 200 Scanning Electron Microscope coupled with EDX detector. The detector has the ability to convert the X-ray energy emitted by the samples into voltage signals that are specific to different chemical elements.

RESULTS AND DISCUSSIONS

Whiteness degree

The values obtained for the whiteness degree of 80% cotton/20% Smartcel™ Sensitive fabrics preliminary treated in different variants, are shown in table 1.

From the series of experimental variants is highlight- ed the alkaline pre-treatment – bleaching in succes- sive phases (classical and mild process) (V1 and V2) for which higher values of the whiteness degree were found. Lower values of the whiteness degree are obtained for the preliminary treatments in single phase using the multiple action chemical auxiliary (Sirrix SB) (V3) and also for the low temperature pro- cesses (Imerol LTB) (V5).

Tha values obtained for the hydrophilicity of 80% cot- ton/20% Smartcel™ Sensitive fabrics after the applied preliminary treatments are shown in table 2. From the table 2 it can be seen that the hydrophilici- ty is good for all applied preliminary treatment (below

Table 1

WHITENESS DEGREE
Code	Whiteness degree (Berger)	Whiteness degree (CIE)
V1	75.58	76.16
V2	73.25	74.40
V3	55.55	56.41
V5	45.99	45.82
V6	60.36	60.05

1 second according to drop test and water absorben- cy between 44% and 58% respectively). Slightly lower values of hydrophilicity is obtained for the fab- ric treated in single phase with the multiple action chemical auxiliary (mild process) (V3), for which a wettability of 2 seconds and 44% water absorbency have been obtained.

Color measurements

Colour differences attributes obtained for 80% cotton/ 20% SmartcellTM Sensitive fabrics preliminary treat- ed in different variants and dyed with Drimaren Gelb CL-2R are presented in table 3. As reference, the sample treated by strong alkaline treatment – bleach- ing in successive phases (classical process) (Code V1) was used. The values obtained reveal significant color differences between the analyzed samples. This behavior is due to the fact that the applied treat- ments provide a differentially removal of the natural impurities of cotton (pectin, waxes, pigments) depending on: the chemical auxiliaries used in the process, the main process parameters (pH, tempera- ture, treatment duration), the number of operations and rinsings performed with water at high tempera- ture, with implicit influences on whiteness degree and hydrophilicity. In conclusion, the dye uptake varies from one variant to another, being influenced by all these factors. Compared to the reference samples treated by strong alkaline pre-treatment – bleaching in successive phases (classic process) (V1), the total color difference (DE*) of pre-treated samples in

Table 3

COLOR DIFFERENCES ATTIBUTES FOR FABRICS PRELIMINARY TREATED IN DIFFERENT VARIANTS AND DYED
Code	Color differences
	DL*	DC*	DH*	DE*	Mark
V1	Refference
V2	–0.25	2.10	–0.33	2.14	4–5
V3	–2.13	4.62	–1.49	5.30	3–4
V4	–2.73	3.41	–1.66	4.67	3

different variants ranging between 2.14 and 5.30, which corresponds to a total color difference of ½ up to 2½ tons compared to the reference. Analyzing the obtained data, it is possible to appreciate that the classical treatment in successive phases, considered the reference standard, is the most effective in terms of removing the impurities of cotton and implicitly in terms of dye adsorption.

Color fastness

Regardless of the pre-treatment method, applied prior to dyeing operation, color fastness to washing, acid and alkaline perspiration, dry and wet rubbing are very good, with marks obtained for change of shade and staining of the multi-fiber standard between 4–5/5 (table 4).

The main physical-mechanical characteristics are present in the table 5. Analyzing the obtained results,

Table 4

COLOR FASTNESS
Code	Washing				Acid perspiration				Alkaline perspiration				Rubbing
	Color change	Color staining			Color change	Color staining			Color change	Color staining			Dry	Wet
		CO	PA	W		CO	PA	W		CO	PA	W
V1	4-5	4-5	4-5	4-5	4-5	4-5	4-5	5	4-5	4-5	4-5	5	4-5	4-5
V2	4-5	4-5	4-5	4-5	4-5	5	4-5	5	4-5	4-5	4-5	5	4-5	4-5
V3	4-5	4-5	4-5	4-5	4-5	5	4-5	5	4-5	4-5	4-5	5	5	4-5
V4	4-5	4-5	4-5	4-5	4-5	4-5	5	5	4-5	4-5	5	5	5	4-5
V5	4-5	4-5	4-5	4-5	4-5	4-5	5	5	4-5	4-5	5	5	5	4-5
V6	4-5	4-5	4-5	4-5	4-5	4-5	5	5	4-5	4-5	5	5	5	4-5

Table 5

PHYSICAL-MECHANICAL CHARACTERISTICS
Code	Mass [g/cm2]	Density [No counts/10cm]		Tensile strength [N]		Elongation at break [%]		Tearing strength [N]
		Weft	Warp	Weft	Warp	Weft	Warp	Weft	Warp
Raw fabric	246	290	230	1788	717	21.8	11.30	71.3	38.9
V1	260	310	236	1716	787	26.8	18.26	33.1	15.67
V2	260	324	238	1823	786	26.5	19.51	31.9	15.50
V3	261	314	232	1778	780	28.0	18.92	54.4	35.4
V4	265	306	240	1892	818	38.0	15.0	61.2	39.5
V5	000	000	000	1879	627	32.1	25.9	44.9	34.5
V6	263	312	234	1757	671	30.4	18.05	38.3	19.36

Fig. 1. Water vapor permeability of fabrics treated in different variants

Fig. 2. Air permeability of fabrics treated in different variants

it can be observed that, during the finishing process, the fabric contraction took place, leading to the increasing of the mass (g/m2) and density in the warp and weft direction, compared to the raw fabric, with- out significant differences between variants. This behavior is normal for the finishing processes of cot- ton fabrics carried out in aqueous medium and high temperatures. Tensile strength does not show signifi- cant changes after finishing treatments, just only small variations (decreases or increases) ranging from 0.5 to 5.8 % as compared to the raw fabric, but these variations can be considered negligible.

Tearing strength shows decreases values in the case of classic treatment variant – hot alkaline treatment in the presence of NaOH (V1) and also for the mild alka-

line treatment in the presence of Na2CO3 (V2), with more than 50% decreases of values in warp and weft

direction. From the applied treatments, the prelimi- nary treatment with the multiple action chemical aux- iliary followed by dyeing without intermediate rinsings

(V4) affects the least the tearing strength of the treat- ed samples.

The air and the water vapor permeability recorded for the 80% cotton/20% SmartcellTM Sensitive fabrics have certain variations between the experimented finishing variants, in close relation with the fabrics density. Higher values of this caracteristics is obtained for the fabric pre-treated with the multiple action chemical auxiliary followed by dyeing without intermediate rinsings (V4) (figures 1–2), for which the lowest value of the density in weft direction is obtained.

SEM-EDX

Electronic images recorded at a magnification of 2000 x for textile materials treated in different vari- ants are shown in figure 3. Analyzing the obtained images can be observed that applied preliminary treatments do not change differentially the surface of functional man-made cellulosic fibers.

Quantification of the Zn content existing in the matrix of SmartcellTM Sensitive fibers is shown in table 6.

V1 V2 V3 V4

V5 V6

Fig. 3. SEM images of textile materials treated in different variants

Raw material V1 V2 V3

V4 V5 V6

Fig. 4. Images of Petri plates after 48 h incubation

Table 6

Table 7

Zn CONTENT
Zn content		Code
	Raw	V1	V2	V3	V4	V5	V6
Wt %	11.39	1.32	9.92	9.63	7.62	2.34	5.59
At %	2.59	0.30	2.28	2.21	1.71	0.51	2.10

Analyzing the obtained data, it can be appreciated that regardless of the finishing applied variant, the Zn presence was identified in the percentage of mass between 1.32% and 9.63%. It should be noted, how- ever, that the appreciation of the Zn content is quali- tative and by this method it was not possible to make a definite differentiation between the experimented variants.

Antibacterial activity

Images of Petri plates after 48 h incubation are shown in figure 4.

The results obtained from the evaluation of antimi- crobial activity for the treated samples in different experimental variants are shown in table 7.

From the evaluation of the results obtained for all the variants. an antibacterial effect against the Staphylococcus aureus test strain is observed. In the case of the raw fabrics (unfinished) and the samples treated according to the pre-treatment in single phase with a multiple action chemical auxiliary Sirrix SB (code V3), the inhibition zone or the Staphylococcus aureus test strain in the whole medium of the culture was not observed, thus completely inhibiting the growth and inhibition of the test microorganism.

ANTIMICROBIAL ACTIVITY
Sample	Inhibition zone [mm]	Evaluation
Raw material	-	Satisfactory effect
V1	2.5	Satisfactory effect
V2	4	Satisfactory effect
V3	-	Satisfactory effect
V4	5	Satisfactory effect
V5	2	Satisfactory effect
V6	4	Satisfactory effect

CONCLUSIONS

Laboratory experiments have highlighted that the hydrophilicity obtained after pre-treatment is very good for the all experimental variants, slightly lower values of hydrophilicity is obtained for the fabric pre- treated in single phase with the multiple action chem- ical auxiliary by a mild process (V3). The strong alka- line treatment – bleaching in successive phases (V1 – classical process), being considered the refer- ence standard process, is the most effective in terms of removing the impurities of cotton and implicitly in terms of hydrophilicity, whiteness degree and dyes adsorption. However, tearing strength shows signifi- cant decreases values in the case of classical treat- ment variants – hot alkaline treatment in the pres- ence of NaOH (V1) or mild alkaline treatment in the presence of Na2CO3 (V2), with over 50% decreases of values in warp and weft direction. The preliminary treatment affecting the least tearing strength of the treated sample is the one who uses the multiple action chemical auxiliary in the first process step

being followed by the dyeing, without intermediate rinsings between technological operations (V4). In terms of tensile strength, there are no significant dif- ferences between experimented finishing treatments, yet existing small variations (decreases or increases) compared with the raw fabric, being considered neg- ligible. Color fastness to washing, acid and alkaline perspiration, dry and wet rubbing fastness are very

good, with marks obtained for all the samples between 4–5/5. An antibacterial effect against the Staphylococcus aureus test strain is observed for all finished samples, with or without in inhibition zone.

ACKNOWLEDGEMENT

This work was supported by a grant of the Ministry of Research and Innovation (MCI), contract no. 26N/14.03.2016, PN 16 34 03 04.

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Authors:

XXXXX XXXXXXX0 XXXXX XXXXXXX0 DOINA TOMA1 XXXXXX XXXXXX0,2

XXXXXXXXX XXXXXXXXX XXXXX0 XXXXXX XXXXXXX0

1 R&D National Institute for Textiles and Leather (INCDTP), 00, Xxxxxxxx Xxxxxxxxxx xxxxxx, Xxxxxxxxx, 000000, Xxxxxxx e-mail: xxxxxx@xxxxxx.xx

2 University of Bucharest, Faculty of Chemistry, Regina Xxxxxxxxx Xxxxxxxxx 0-00, 000000, Xxxxxxxxx, Xxxxxxx

3 R&D National Institute for Textiles and Leather (INCDTP), Leather and Footwear Research Institute (ICPI) Division, 00, Xxx Xxxxxxxxx xxxxxx, Xxxxxxxxx, 000000, Xxxxxxx

Corresponding author:

XXXXX XXXXXXX

e-mail: xxxxx.xxxxxxx@xxxxxx.xx