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2nd International Conference on Value Addition and Innovation in Textiles, Faisalabad, 2013

DYEING WOOL FABRIC WITH THE EXTRACTION OF SAMBUCUS NATURAL COLORING AGENTS

Nigar Merdan

Department of Fashion and Textile Design, Faculty of Engineering and Design, Istanbul Commerce University, Istanbul, Turkey

[email protected] Şeyda Canbolat

Department of Fashion and Textile Design, Faculty of Engineering and Design, Istanbul Commerce University, Istanbul, Turkey

[email protected]

E. Dilara Koçak

Department of Textile Engineering, Faculty of Technology, Marmara University, Istanbul, Turkey [email protected]

Mehmet Akalın

Department of Textile, Faculty of Technical Education Faculty, Marmara University, Istanbul/Turkey [email protected]

ABSTRACT

Sambucus ebulus L. and Sambucus nigra L. are the two species of Sambucus in Turkey. The leaves of Sambucus are used in Turkish folk medicine for snake bites, wounds, hemorrhoid and high fever.

Also Sambucus consists of tannin, volatile grease, coloring agents and organic acids. The coloring agents take place in the fruits from which they are extracted. In this study the naturel dyes extracted from the fruits of Sambucus nigra L. are used to dye wool yarns. After the samples were mordanted with a variety of mordents, the samples were dyed with the natural dying extracted from Sambucus nigra L. by ultrasonic and conventional methods. After the dying process, some samples were rinsed whilst others were squeezed without rinsing. Half of the samples were applied the finishing process with cationic fixer. Finally the features of dying and fastness have been investigated with regard to the type of mordents, the type of dying process and finishing process.

Key Words: Sambucus nigra L., Natural dyes, Fastness, Ultrasound Method, Conventional method 1. INTRODUCTION

Natural dyes derived from the sources of vegetable and animal have been used to dye a variety of materials. Natural dyes had been utilized in all of the coloring process [1] until the discovery of synthetic dyes in 1856, which, in turn, decreased the use of natural dyes [1, 2]. The synthetic dyes are preferable in that they provide a wide range of color, and that, compared to the natural dyes, they are cheaper, easier to supply and their fastness properties are better [3]. However natural dyes are advantageous in that they are non-toxic, non-carcinogenic and biodegradation [4]. By this time many investigation have been conducted based on dying of wool materials with natural dyes. McNeil and

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McCall investigated the effect of ultrasound method according to which quite a number of wool was dyed on reducing environmental impact. After the dying they examined the surface of wool material by scanning electron microscopy and fluorescence microscopy, which result in no indication of any surface damage in scanning electron microscopy. In contrast, fluorescence microscopy revealed the increasing number of sulfhydryl groups on the wool surface. Besides they determined that ultrasonic energy did not make any contributions to dyeing conditions used currently in industry. However it proved the potential to reduce the chemical and energy requirements of dyeing wool with reactive and acid dyes [5]. Mirjalili and his friends used the dyes which were extracted from weld by using soxhlet apparatus to dye wool fabrics. The solution which is a combination of the extraction of weld and ethanol solution was applied to wool fabric. Finally, all dyed specimens were tested for wash and light fastness properties, proving weld an alternative to synthetic acid dyes in comparison to synthetic dyes [6]. Shams-Nateri investigated madder absorption behavior on wool fiber and used spectrometer to understand absorption behavior. The color parameter and fastness properties of samples demonstrated that the quality of samples dyed in reconstructed dye bath is the same as initial wool dyeing. The economic analysis indicated that reuse of wastewater provided 19.91% cost saving in wool dyeing with madder [7]. Ghoranneviss and his friends researched the plasma effect on wool fabric by using argon gas instead of mordant in natural dying process. Furthermore they investigated the anti-bacterial effect of the dyes extracted from weld and madder. The results show that the plasma treatment has improved the natural dyeing properties of wool, offering a substitution for mordant treatment, and has also increased the efficiency of its antibacterial activity [8].In this study we have investigated wool dying with the natural dyes extracted from Sambucus nigra L. After the samples were mordanted with a variety of mordents the samples were dyed with the natural dye extracted from Sambucus nigra L. by ultrasonic and conventional methods. Following the dying process, some of the samples were washed with cationic fixer whereas others were washed with water. As a result, the features of dying and fastness have been investigated with regard to the type of mordents, the type of dying process and finishing process.

2. EXPERIMENTAL

2.1.Materials

In this paper wool yarns 47 Nm of 1-0.5 grams were used and then twenty two samples were prepared. Firstly twenty samples were mordanted with five different mordents which were potassium aluminum sulphate, citric acid, sodium bichromate, copper sulphate and cationic fixer-Denge Fix R (Denge Chemist). The remaining samples were dyed without mordent. After mordanting half of the samples were subjected to conventional dying process whereas the other samples were subjected to ultrasound dying process with the natural dyes extracted from Sambucus nigra L. Then half of the samples were applied conventional washing whilst the others were subjected to cationic finishing process. Finally the wash fastness, light fastness and color fastness of samples were tested.

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2.2. The Extraction of Natural Dye

Sambucus nigra L. was used as the source of natural dye and 2.5 L permutit water was added to Sambucus ebulus L of 4.975 grams. After the combination was left to rest for 4 hours at the room temperature the dyes were extracted.

2.3.Mordanting

For the mordanting process four different mordent agents were used which are potassium aluminum sulfate, citric acid, sodium dichromate, copper sulfate and cationic fixer-Denge Fix R (Denge Chemistry).

1. Mordanting with Potassium AluminiumSulphate

The preparation of the mordent solution; 50 mL permutit water and 1 gram potassium aluminum sulphate were mixed. Then the wool yarns were processed with the mordent solution for an hour at the boiling temperature. When the solution cooled down to the room temperature, wool yarn was taken out from the solution and squeezed.

2. Mordanting with Citric Acid

The preparation of the mordent solution; 50 mL permutit water and 1 gram citric acid were mixed.

Then the wool yarns were processed with the mordent solution for an hour at the boiling temperature.

When the solution cooled down to the room temperature, the wool yarn was taken out from the solution and squeezed.

3. Mordanting with Sodium Dichromate

The preparing of the mordent solution; 50 mL permetit water and 1 gram sodium dichromate were mixed. Then the wool yarns were processed with the mordent solution for an hour at the boiling temperature. Finally the solution cooled down to the room temperature, the wool yarn was taken out from the solution and squeezed.

4. Mordanting with Copper Sulfate

The preparing of the mordent solution; 50 mL permutit water and 1 gram copper sulphate were mixed.

Then the wool yarns were processed with the mordent solution for an hour at the boiling temperature.

Finally the solution cooled down to the room temperature, the wool yarn was taken out from the solution and squeezed.

5. Mordanting with Cationic Fixer

The preparation of the mordent solution; 50 mL permetit water at 50ºC and 1 gram cationic fixer- Denge Fix R ( Denge Chemistry) were mixed and acetic acid was added into the solution, adjusting pH

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to 4.5-5.5. Then wool yarns were processed with the solution for 20 seconds at 50 ºC. After the solution cooled down to the room temperature, the wool yarn was taken out from the solution and squeezed.

2.4. Dyeing

2.4.1. Conventional Dyeing

In this method, the samples were applied liquor of ratio 1: 50 at the boiling temperature for an hour.

Then the samples were rinsed with cold water, hot water and cold water, respectively.

2.4.2. Ultrasonic Dyeing

The dying process was carried out with Maxwell Ultrasonic Dyeing device at 70 ºC for 15 minutes and the samples were exposed to 20 kHz ultrasonic power. Then the samples were rinsed with cold water, hot water and cold water, respectively.

2.5. Cationic Finishing Process

Half of the samples were washed with the cationic after treatment agent. Firstly the samples were subjected to overflow wash with 500 mL cold water. Then 10 g/ L stock fixer and acetic acid were added to 250 mL water at 50 ºC and acidic acid was used to adjust pH to 4.5-5. The samples were treated with this solution for 20 seconds. Then the samples were rinsed with cold water.

2.6. Evaluation of the Colors Obtained at the Dying Process

Color measurements of the samples were performed in the color measuring device of Gretaq Macbeth – Color Eye 2180UV. All the samples were measured from ten different regions of them and the average curves of wavelength-%reflectance were obtained via calculation of the arithmetic mean of the reflectance values obtained at the every wavelength. The calculations were performed with respect to D65 light source and 10o standard observer. At the measurements the sample which was not mordanted was accepted as standard and the samples mordanted were compared in terms of the colors. The calorimetric values were measured according to the CIELAB system and the equation 1 was used to determine total color differences [9].

     

* 2 * 2 * 2

*

L a b

E      

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Where ΔE* refers to the total color differences. In commercial regards, if ΔE*< 1, the value of color differences could be accepted in general. The negative value of ΔL* result in that the color of the samples compared is darker than that of the standard whereas the positive value of ΔL* results in that the color of the samples compared is lighter than that of the standard. In the same vein, the positive value of Δa* results in surplus of the red nuance whereas the negative value of Δa* results in surplus of the green nuance. The positive value of Δb* means that the yellow nuance is much whereas the negative value of Δb* means that the blue nuance is much.

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2.7. Color Fastness

The light and washing fastness of the colored samples were tested according to ISO105-C06 and ISO105-B02. The washing fastnesses of the samples were performed by using the washing fastness equipment (Gyrowash/James H.HealCo.Ltd.). Then the results were evaluated with the gray scale.

The light fastness of the samples was performed by using the light fastness equipment with the reference of the blue scale (James H. Heal). The assessment of washing fastness grade which are performed 1 to 5, ″5″ corresponds the best value.

3. RESULTS OF THE MEASUREMENTS 3.1. Color Measurement

The wool materials were mordanted with four different mordents then the natural dyeing was extracted from the fruits of Sambucus ebulus L. which has sambusiyanin structure of the chromospheres group via conventional and ultrasonic method. The samples dyed without mordent via conventional and ultrasonic method were accepted as standard.

ΔL* (brightness-thickness), Δa*( redness-greenness), Δb*( yellowness-blueness) ve ΔC* (saturation) values of the samples are shown in Table 1.

Table 1. Spectrophotometer Color Measurement Values of the Samples

* * * *

Code Mordent c** u*** c u c u c u

1 Copper Sulfate

7.401 -6.082 -7.127 -9.861 7.629 10.636 5.079 10.595

2 Copper

Sulfate* 7.064 -4.199 -9.846 -6.298 12.561 7.481 10.116 6.876

3 Citric Acid 15.224 7.300 -2.909 -1.392 2.272 2.145 0.580 1.716

4 Citric Acid * 12.184 2.911 -5.672 -1.124 5.229 1.895 2.794 1.525

5 Potassium

Aluminium Sulfate

12.888 3.781 -9.206 -7.123 4.824 2.430 2.354 1.993

6 Potassium

Aluminium Sulfate *

8.159 -0.963 -

12.302

-10.567 8.334 6.932 6.370 7.221

7 Cationic Fixer

4.807 3.502 -2.449 -0.572 2.462 -0.657 0.926 -0.803

8 Cationic Fixer*

10.331 -5.072 -4.304 1.317 4.244 -1.016 2.063 -0.438

Note: The samples shown * were treated with cationic finish and the other samples were rinsed via conventional method.

* The sample treated cationic finishing after cold rinsed

**Standard: The unmordanted sample dyed via conventional method

*** Standard: The unmordanted sample dyed via ultrasonic method

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Figure 1. The ΔE* value of the samples

When the total color different (CIELAB ΔE*) was investigated, generally the ultrasonic dyeing was closed to the standard, but it was showed that the ultrasonic dyeing takes place the limits which were not accepted.

Figure 2. The value ΔL* of samples

When the L* values were investigated, samples dyed by using conventional method were lighter than the standard, and the colors became lighter by using ultrasonic method but lighter colors were obtained by using conventional method.

12,798 17,453 15,665 17,453 16,557 16,952 5,930 11,969

15,727 10,642 7,735 3,651 8,423 12,675 3,609 5,338

0 5 10 15 20

1 2 3 4 5 6 7 8

∆E*

code

∆E*

Conventional

7,401 7,064 15,224 12,184 12,888 8,159 4,807 10,331

-6,082 -4,199 7,300 2,911 3,781 -0,963 3,502 -5,072

-10 -5 0 5 10 15 20

1 2 3 4 5 6 7 8

∆L*

code

∆L*

Conventional

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Figure 3. The ∆a* valuesof the samples

When a* values were investigated green grade was obtained by the conventional and ultrasonic methods.

Figure 4. The ΔE* values of the samples

When the b* values were investigated an increasing was obtained on the yellow grade by using conventional method. For the ultrasonic method, color became blue when the cationic fixator was used as mordan and color became yellow for the other dyeings.

-7,127 -9,846 -2,909 -5,672 -9,206 -12,302 -2,449 -4,304

-9,861 -6,298 -1,392 -1,124 -7,123 -10,567 -0,572 1,317

-13 -11 -9 -7 -5 -3 -1 1

1 2 3 4 5 6 7 8

∆a*

code

∆a*

Conventional

7,629 12,561 2,272 5,229 4,824 8,334 2,462 4,244

10,636 7,481 2,145 1,895 2,430 6,932 -0,657 -1,016

-2 3 8 13 18

1 2 3 4 5 6 7 8

∆b*

code

∆b*

Conventional

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Figure 5. The ∆C* values of the samples

When the C* values were investigated, brighter colors were obtained by using conventional method.

For the ultrasonic method, brighter colors were obtained when the cationic fixator was used as mordan, and more dull colors were obtained for the other ultrasonic dyeings.

3.2. The Results of Fastness

The washing fastness of samples was performed with 4 g/l ECE detergent at 50 oC for 30 minutes.

The washing fastness of samples dyed with the natural dyeing extracted from Sambucus ebulus L. are shown in Table 2.

Table 2. The Fastness Value of Dyeing Samples

The Washing Fastness Values Change in

Color

Staining

Type of Mordent CA Co PA PES PAN Wo

Without Mordent(c) 2 5 4-5 4 5 5 4-5

Without Mordent(u) 1 5 4-5 4 5 4-5 4-5

Copper Sulfate (c) 1-2 5 4-5 4 5 5 5

Copper Sulfate*(c) 2-3 5 4-5 4 5 4-5 5

Copper Sulfate(u) 1 5 4 3-4 5 5 5

Copper Sulfate*(u) 2-3 5 4-5 4 5 5 5

Citric Acid(c) 1 5 4-5 3-4 5 5 4-5

Citric Acid *(c) 2-3 5 4-5 3-4 5 5 4-5

Citric Acid (u) 2 4-5 4-5 3-4 5 4-5 4-5

Citric Acid*(u) 3 4-5 4 3-4 5 4-5 4-5

Potassium Aluminum Sulfate(c)

1-2 5 4-5 3 5 5 5

Potassium Aluminum Sulfate*(c)

1-2 5 4-5 4 5 4-5 5

Potassium Aluminum Sulfate(u)

1-2 5 4-5 4 5 5 5

Potassium Aluminum Sulfate*(u)

2-3 5 4-5 4 5 5 5

Cationic Fixer(c) 1 5 4-5 3 5 4-5 4-5

Cationic Fixer*(c) 2-3 4-5 4-5 3 5 4-5 4-5

Cationic Fixer (u) 1 4-5 4-5 3-4 5 5 5

Cationic Fixer*(u) 2 5 4-5 4 5 5 5

5,079 10,116 0,580 2,794 2,354 6,370 0,926 2,063

10,595 6,876 1,716 1,525 1,993 7,221 -0,803 -0,438

-1 4 9 14 19

1 2 3 4 5 6 7 8

∆C*

code

∆C*

Conventional

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* The sample treated with cationic finishing after cold rinse c:conventional method

u:ultrasonic method

When the result of wash fastness was investigated, after the washing, the color of the samples changed and the values of staining changed 4 to 4-5 and 5. Maximum staining value was determined for wool dyeing with the extraction of Sambucus ebulus L.

Conclusion

In this work, a comparison of conventional and ultrasonic methods of dyeing using the natural dyes extracted from Sambucus ebulus L. was carried out. CIELab colorimetric coordinates showed that the dyeing with ultrasonic method resulted better thanks to sonication energy. Also this method provides saving from water, auxiliary chemicals, time and energy. When the ultrasonic method was compared with the conventional method in terms of fastness value, no observation regarding any essential differences was obtained. However in both methods, the wash fastness proved good quantity.

Especially the wash fastness values of wool materials should be accepted for the industry. In conclusion the dyeing which is carried out with the natural dyes extracted is eco-friendly.

REFERENCES

1. Hunger K., “Industrial Dyes”, Wiley-VCH, Weinheim, 2003

2. H.T. Deo, B.K. Desai ‘Dyeing of cotton and jute with tea as a natural dye’, ColorationTechnology, Volume 115, Issue 7-8, pages 224–227,1999

3. Thomas Bechtold, Amalid Mahmud-Ali, Rita Mussak, ‘Natural dyes for textile dyeing: A comparison of methods to assess the quality of Canadian golden rod plant material’, Dyes and Pigments, 75, (2007) ,287-293

4. Optimization of alkaline extraction of natural dye from Henna leaves and its dyeing on cotton by exhaust method,Shaukat Ali, TanveerHussai in, Rakhshanda Nawaz, Journal of Cleaner Production, vol.17, 2009, p. 61–66

5. Ultrasound for wool dyeing and finishing, S.J. McNeil , R.A. McCall, Ultrason Sonochem. 2011, 18(1), p. 401-6

6. Eco-friendly dyeing of wool using natural dye from weld as co-partner with synthetic dye, Mohammad Mirjalili, Khosro Nazarpoor, Loghman Karimi, Journal of Cleaner Production, Volume 19, issue 9-10 (June - July, 2011), p. 1045-1051

7. Reusing wastewater of madder natural dye for wool dyeing; Ali Shams-Nateri, Journal of Clean Production, Vol 19, 2011, 775-781

8. Influence of plasma sputtering treatment on natural dyeing and antibacterial activity of wool fabrics, Mahmood Ghorannevissa, Sheila Shahidib, Abbas Anvaric, Zahra Motaghid, Jakub Wienere,Irena Slamborovaf, Progress in Organic Coatings, vol 70, 2011, p. 388–393

9. Fairchild, M.D., (1997), “Color Appearance Models”, ISBN 0-201-63464-3, Addision Westley Longman, Inc.

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