Silk fabric dyeing with natural dye from mangrove bark (Rhizophora apiculata Blume) extract

Silk fabric dyeing with natural dye from mangrove bark (Rhizophora apiculata Blume) extract

Industrial Crops and Products 49 (2013) 122–129 Contents lists available at SciVerse ScienceDirect Industrial Crops and Products journal homepage: w...

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Industrial Crops and Products 49 (2013) 122–129

Contents lists available at SciVerse ScienceDirect

Industrial Crops and Products journal homepage: www.elsevier.com/locate/indcrop

Silk fabric dyeing with natural dye from mangrove bark (Rhizophora apiculata Blume) extract Nattaya Punrattanasin a , Monthon Nakpathom b , Buppha Somboon b , Nootsara Narumol b , Nattadon Rungruangkitkrai c , Rattanaphol Mongkholrattanasit d,∗ a

Department of Textile Science and Technology, Faculty of Science and Technology, Thammasat University, Pathumthani 12121, Thailand National Metal and Materials Technology Center, National Science and Technology Development Agency, Pathumthani 12120, Thailand c Department of Textile Science, Faculty of Agro-Industry, Kasetsart University, Bangkok 10900, Thailand d Department of Textile Chemistry Technology, Faculty of Industrial Textiles and Fashion Design, Rajamangala University of Technology Phra Nakhon, Bangkok 10300, Thailand b

a r t i c l e

i n f o

Article history: Received 28 December 2012 Received in revised form 25 March 2013 Accepted 22 April 2013 Keywords: Natural dyes Mangrove bark Dyeing Silk Mordant

a b s t r a c t Natural dye extracted from mangrove bark was applied to a silk fabric by an exhaustion dyeing process. Aluminum potassium sulfate, ferrous sulfate, copper sulfate, and stannous chloride were used as mordants. The dyeing was conducted with and without metallic salt mordants, using three different mordanting methods: pre-mordanting, meta-mordanting, and post-mordanting. The color of each dyed material was investigated in terms of the CIELAB (L*, a* and b*) and K/S values. The color fastness to washing, crocking, perspiration, and water of the dyed samples was determined according to AATCC test methods, whereas the color fastness to light was tested according to the ISO standard. Optimum results were achieved when dyeing at 90 ◦ C for 60 min and at pH 3. Silk fabric dyed without mordant had a shade of reddish-brown, while those mordanted with stannous chloride, aluminum potassium sulfate, and copper sulfate produced a variety of pale to dark reddish-brown color shades. However, duller and darker shade was obtained with ferrous sulfate mordant. The color fastness to washing was mostly very poor to poor but there was no fading of the color, whereas the color fastness to light and crocking were mostly fair to good level. However, the perspiration and water fastness results showed good to very good levels, except for fabric mordanted with ferrous sulfate, whose color change rating was poor to fair for perspiration fastness. Tensile strength, tearing strength and stiffness of the fabrics before and after dyeing were also evaluated. © 2013 Elsevier B.V. All rights reserved.

1. Introduction Since natural dyes are biodegradable and less toxic and allergenic than synthetic dyes, they are considered to be environmentally friendly (Mongkholrattanasit et al., 2010). Although synthetic dyeing methods have taken over in the last century, dyeing materials are still abundant in the natural world today. The global demand for natural dyes per year is about 10,000 tonnes, which is equivalent to 1% of the world synthetic dye consumption (Sivakuma et al., 2010). Natural dyes have a wide range of shades that can be obtained from insects, minerals, fungi and various plant parts including roots, barks, leaves, flowers, skins, fruits and shells of plants (Allen, 1971; Mongkholrattanasit et al., 2011b; Velmurugan et al., 2005; Kamel et al., 2005; Zheng et al., 2011;

∗ Corresponding author. Tel.: +66 874843723. E-mail addresses: [email protected], [email protected] (R. Mongkholrattanasit). 0926-6690/$ – see front matter © 2013 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.indcrop.2013.04.041

Vankar and Shukla, 2011; Vankar et al., 2009). Natural dyes are known for their use in coloring of food, leather, wood, as well as natural fibers like wool, silk, cotton and flax since ancient times (Mongkholrattanasit et al., 2011a). Natural dyes have also been used for printing and dye-sensititized solar cells (Wongcharee et al., 2007; Gómez-Ortíz et al., 2010; Rekaby et al., 2009; Agarwal et al., 2007). It is reported that some natural dyes not only dye with unique and elegant colors, but also provide antibacterial, deodorizing and UV protective functions to fabrics (Grifoni et al., 2011; Habbal et al., 2011; Lee, 2007; Lee et al., 2010; Mongkholrattanasit et al., 2011c; Reddy et al., 2012). At the present time, the use of natural dyes in textile application is witnessing very rapid growth. This is mainly attributed to strict environmental standards set by many countries to avoid the health hazards associated with synthetic dyes used in textiles. The recent ban on the use of azo dyes by the European Union has also increased the scope for the use of natural dyes (Sivakuma et al., 2010). Mangrove trees, also called “Khong Khang” in Thailand, are in the Rhizophora species and are widely used as medicinal plants of

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Fig. 1. Color composition of mangrove bark.

eastern and southeast Asia. The most common representatives are Rhizophora mucronata, Rhizophora mangle and Rhizophora apiculata (Tan and Jain, 2012). The mangrove forests have long been utilized by humans for firewood, charcoal and construction of dwellings, furniture, boats, and fishing equipment (Bandaranayake, 2002, 1998). Other applications include textile printing (Nakpathom et al., 2011), adsorbent for dyes (Tan and Jain, 2012; Tan et al., 2011), and production of tannin, which is used for leather tanning and dyeing. During charcoal manufacture, mangrove bark is removed from timbers to reduce the ash content of the charcoal product and it is regarded as solid waste (Tan and Jain, 2012). However, it is reported that these mangrove barks are rich in tannin (ranging from 15 to 36%) and can produce reddish brown dyes (Chapman, 1970; Duke and Allen, 2006). The major coloring components of tannin found in mangrove barks are condensed types, which are composed of four flavanoid monomers namely catechin, epicatechin, epigallocatechin and epicatechin gallate as illustrated in Fig. 1 (Rahim et al., 2007). To further explore the properties of exhaustion dyeing, the present research has investigated the dyeing and fastness properties of silk fabric using an aqueous extract of mangrove bark as a natural dye. Different factors affecting dyeing ability were examined.

2. Experimental 2.1. Materials A commercially scoured and bleached silk fabric (75.2 g m−2 , plain weave) was used. Mangrove bark (Rhizophora apiculata Blume) was supplied from a charcoal factory in Samutsongkhram province, Thailand. Four different laboratory grade mordants were used, i.e. aluminum potassium sulfate (AlK(SO4 )2 ·12H2 O), ferrous sulfate (FeSO4 ·7H2 O), copper sulfate (CuSO4 ·5H2 O),

and stannous chloride (SnCl2 ·5H2 O). A non-ionic soaping agent, Metapon X-80, was supplied by Ilin Enterprise Co. Ltd. (Thailand). 2.2. Instruments The mordanting and dyeing processes were conducted using a Gyrowash machine (James H. Heal & Co. Ltd., England). A UV–visible spectrophotometer (Halo DB-20, UV-Vis Double Beam Spectrophotometer, Australia) was used for absorbance measurement using quartz cells of path length 1 cm. The CIE L*, a*, b* and color strength in terms of K/S values of dyed samples were measured using a spectrophotometer (Hunter Lab Color Quest XE, USA) with illuminant D65 at 10 degree observer. 2.3. Extraction of natural dye from mangrove bark The collected mangrove bark was dried in sunlight and later crushed to small pieces before being used for dye extraction. The dye extraction was performed by mixing the plant material and distilled water in the weight ratio of 1:10 and boiling for 1 h. After that, the resulting solution was filtered to remove the residue and the dye solution was separated into two portions: (a) one for evaporating under reduced pressure with a rotary evaporator, and (b) one for dyeing. The crude dye extract obtained from the rotary evaporator was dried and then stored in a desiccator before use. To obtain a standard calibration curve, the crude dye extract was later ground and diluted with distilled water. The dilution of the mangrove bark extract showed a relatively clear solution with a linear dependence on the concentration–absorbance relation at an absorption peak (max ) of 278 nm. The concentration of 15 g L−1 was calculated from a standard curve of concentrations of the mangrove bark extract dye solution versus absorbance at the wavelength mentioned.

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2.4. Mordanting and dyeing Four different dyeing conditions were varied (temperature, dyeing time, pH and dye concentration) to study the dye uptake behavior of mangrove bark dye extract on silk fabrics. 2.4.1. Temperature To investigate the effect of dyeing temperature, silk fabrics were dyed at seven different temperatures, i.e. 30 ◦ C, 40 ◦ C, 50 ◦ C, 60 ◦ C, 70 ◦ C, 80 ◦ C and 90 ◦ C using 50% on the weight of fabric (owf.) of the mangrove bark extract dye solution at a liquor ratio of 1:40 and at the original pH (=5.4) of the dye solution for 60 min. 2.4.2. Dyeing time Silk fabrics were dyed in six sets of 50% owf. of the mangrove bark extract dye solution at 90 ◦ C, at a liquor ratio of 1:40 and pH 5.4, for different time intervals (10, 20, 30, 40, 50, and 60 min. 2.4.3. pH Silk fabrics were dyed in 50% owf. of the mangrove bark extract dye solution in dyebaths at different pH values of 3, 5, 7, 9, and 11, at a liquor ratio of 1:40, at 90 ◦ C for 60 min. The pH of the dyebaths was adjusted to a desired value with acetic acid and sodium carbonate solution. 2.4.4. Dye concentration The dye concentration was varied at 20%, 40% and 60% owf. and three different mordanting methods were employed, i.e. premordanting, simultaneous mordanting or meta-mordanting, and post-mordanting, using four types of mordants (aluminum potassium sulfate, ferrous sulfate, copper sulfate, and stannous chloride) with a concentration of 40% owf. For the pre-mordanting method, silk fabric was impregnated in a mordanting solution at a liquor ratio of 1:40, at 60 ◦ C for 60 min before dyeing. In the postmordanting method, the dyed fabric was subjected to the same treatment. In the case of meta-mordanting, the mordant was added to the dyebath before dyeing. Silk fabrics were dyed at a liquor ratio of 1:40 and pH 5.4, at 90 ◦ C for 60 min. After dyeing, the dyed samples were rinsed with cold water, soaped with 1 g L−1 of Metapon X-80 at a liquor ratio of 1:40, at 90 ◦ C for 10 min, and finally rinsed with cold water and air-dried. 2.5. Evaluation of color strength, color fastness and physical properties To evaluate dyeing performance, the color strength (K/S) and CIELAB of the dyed samples were measured using a Hunter Lab Color Quest XE spectrophotometer with illuminant D65 and 10◦ observer. The K/S is calculated by the Kubelka–Munk equation, K/S = (1 − R)2 /2R, where R is the reflectance, K is the absorption coefficient, and S is the scattering coefficient. The color difference is expressed as E* and is calculated by the following Eq. (1): E ∗ =



2

2

(L∗ ) + (a∗ ) + (b∗ )

2

Fig. 2. K/S values with varying temperature from 30 ◦ C to 90 ◦ C at a liquor ratio of 1:40 and at pH 5.4 for 60 min.

Test Method 15-2009, and AATCC Test Method 107-2009, respectively. The physical properties of tensile strength, tearing strength, and stiffness in terms of bending length and flexural rigidity of the fabrics were measured according to ASTM D 5034-09, ASTM D 1424-09, and ASTM D 1388-96, respectively. 3. Results and discussion 3.1. Effect of dyeing conditions Dyeing silk fabrics in the mangrove bark extract dye solution showed that increasing temperature increased the color strength (K/S value). Based on Fig. 2, the maximum color strength was obtained at 90 ◦ C. The color of the dyed silk fabric was reddishbrown. The effect of dyeing time on K/S values is shown in Fig. 3. A longer dyeing time means higher color strength (K/S values) until dye exhaustion attains equilibrium, and there is no significant increase after further increases in dyeing time. The optimum time for dyeing the silk fabrics was obtained at 60 min. The effect of pH value on K/S values is illustrated in Fig. 4. The maximum dye uptake was observed at pH 3. Dye uptake increased from the initial pH 3 until pH 5, and then decreased at higher pH values. In the alkaline solution, reaction with hydroxide ions (OH− ) converts the ammonium ion (NH3 + ) to amino (NH2 ) groups and the fiber contains more carboxylate ion (COO− ) (Mongkholrattanasit et al., 2011b; Broadbent, 2001). Thus,

(1)

where E* is the CIELAB color difference between batch and standard. Here L*, a*, b* and hence E* are in commensurate units. L* denotes the difference between lightness (where L* = 100) and darkness (where L* = 0), a* the difference between green (−a*) and red (+a*) and b* the difference between yellow (+b*) and blue (−b*) (Park, 1993). All measured samples showed a maximum absorption wavelength value (max ) at 400 nm. The color fastness to washing, light, crocking, perspiration, and water of the dyed samples were determined according to AATCC Test Method 61-2010, ISO 105-B02: 1994, AATCC Test Method 8-2007, AATCC

Fig. 3. K/S values at dyeing times from 10 to 90 min at 90 ◦ C, at a liquor ratio of 1:40 and at pH 5.4.

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Table 1 Color values at varying dye concentrations (20%, 40% and 60% owf.) by pre-mordanting and using 40% owf. metal mordants, a liquor ratio of 1:40, a temperature of 90 ◦ C for 60 min. Type of mordants

Without mordant

AlK(SO4 )2

CuSO4

FeSO4

SnCl2

a

Dye conc. (%owf.)

Pre-mordanting K/S

L*

a*

b*

20

4.54

53.19

19.91

27.21

40 60

4.76 5.19

56.40 56.08

19.27 18.90

32.37 33.99

20

2.93

61.88

17.49

28.23

40 60

3.85 3.99

56.92 56.69

19.68 19.87

28.60 28.97

20

6.05

46.84

13.34

19.40

40 60

6.19 6.87

46.32 45.48

18.27 24.17

22.25 25.04

20

4.76

43.65

5.65

8.68

40 60

4.86 5.05

42.78 41.58

8.20 7.80

9.54 9.21

20

2.11

71.97

11.19

25.43

40 60

2.60 3.22

68.48 63.20

12.17 13.96

26.23 26.68

Color obtaineda

60% owf. dye concentration.

electrostatic repulsion between the anionic colorants and the protein fibers occurs, which leads to a decrease in the dye uptake. Tables 1–3 show the color values of the silk fabric dyed with mangrove bark extract dye solution. The K/S values increased with an increase of dye concentration. The mordant activity sequence for the pre-mordanting method was CuSO4 > FeSO4 > without mordant > AlK(SO4 )2 > SnCl2 and CuSO4 > without mordant > FeSO4 > AlK(SO4 )2 > SnCl2 for the meta-mordanting. In the post-mordanting, CuSO4 > FeSO4 > AlK(SO4 )2 > SnCl2 > without mordant was observed. In all cases, the copper sulfate mordant yielded the best dyeing results. Copper sulfate and ferrous sulfate mordants are well known for their ability to form coordination complexes and to readily chelate with the dye. As the coordination numbers of copper sulfate and ferrous sulfate are 4 and 6, respectively, some coordination sites remain unoccupied when they interact with the fiber. Functional groups such as amino and carboxylic acid on the fiber can occupy

these sites. Thus, the metal can form a ternary complex on which one site binds with the fiber and the other site binds with the dye (Bhattacharya and Shah, 2000). Stannous chloride and aluminum potassium sulfate form weak coordination complexes with dye; they tend to form quite strong bonds with the dye but not with the fiber, so they block the dye and reduce the dye interaction with the fiber (Bhattacharya and Shah, 2000). The obtained values (Tables 1–3) show that silk fabrics dyed without mordant had reddish-brown color, while those mordanted with aluminum potassium sulfate, stannous chloride and copper sulfate produced a variety of pale to dark reddish-brown color shades. With ferrous sulfate, the color shade was darker and duller. This may be associated with the change of ferrous sulfate into a ferric form by reacting with oxygen in the air. Ferrous and ferric forms coexist on the fiber and their spectra overlap, which results in a shift of ␭max and thus consequently a color change to a darker shade (Shin and Lee, 2006). Additionally, the tannins in the mangrove bark extract combine with ferrous salts to form complexes, which also result in a darker shade of fabric (Vankar, 2007). It can be concluded that silk fabric can be successfully dyed with mangrove bark extract due to the tannin content in mangrove bark (Chapman, 1970; Duke and Allen, 2006; Duke et al., 2006). Tannin contains phenolic compounds that can form hydrogen bonds with the carboxyl group of protein fibers. Furthermore, there are two other possibilities involved; (a) the anionic charge on the phenolic groups forms an ionic bond with cationics (amino groups) on the protein substrate; and (b) a covalent bond may also form by an interaction between any quinine or semiquinone groups present in the tannin and suitable reactive groups on the silk fiber (Agarwal and Patel, 2002).

3.2. Effect of dyeing technique on fastness and physical properties Fig. 4. K/S values at different pH values (3, 5, 7, 9 and 11) at a liquor ratio of 1:40, 90 ◦ C for 60 min.

The fastness ratings of silk fabric dyed with or without mordants at a dye concentration of 60% owf. and 40% owf. mordant

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Table 2 Color values at varying dye concentrations (20%, 40% and 60% owf.) by meta-mordanting and using 40% owf. metal mordants, a liquor ratio of 1:40, a temperature of 90 ◦ C for 60 min. Type of mordants

Without mordant

AlK(SO4 )2

CuSO4

FeSO4

SnCl2

a

Dye conc. (%owf.)

Meta-mordanting K/S

L*

a*

b*

20

4.54

53.19

19.91

27.21

40 60

4.76 5.19

56.40 56.08

19.27 18.90

32.37 33.99

20

3.00

61.83

11.69

24.21

40 60

3.04 3.36

61.40 59.80

11.49 14.70

24.17 27.00

20

4.62

55.41

10.76

19.61

40 60

5.44 5.47

49.59 49.97

13.50 15.31

20.63 22.18

20

3.06

49.98

2.73

7.46

40 60

4.15 4.89

44.47 41.09

3.69 3.86

7.26 6.81

20

0.38

85.83

3.61

10.07

40 60

0.94 1.06

77.58 78.27

8.87 8.15

18.90 20.37

Color obtaineda

60% owf. dye concentration.

concentration are presented in Tables 4, 6–9. Table 4 shows that the wash fastness ratings of both non-mordanted and mordanted dyed samples were very poor to poor (1–2), except for ferrous sulfate mordant, whose rating was fair to good (3–4). The low gray scale rating is caused by the original color of the dyed fabric visually

becoming more reddish after the washing test, as indicated by the positive values of a*, except for copper sulfate mordant (Table 5). This drastic color change may be attributed to (a) the ionization of the hydroxyl groups in the dye molecules under the alkaline condition of the standard detergent solution (Räisänen et al., 2002;

Table 3 Color values at varying dye concentrations (20%, 40% and 60% owf.) by post-mordanting and using 40% owf. metal mordants, a liquor ratio of 1:40, a temperature of 90 ◦ C for 60 min. Type of mordants

Without mordant

AlK(SO4 )2

CuSO4

FeSO4

SnCl2

a

60% owf. dye concentration.

Dye conc. (%owf.)

Post-mordanting K/S

L*

a*

b*

20

4.54

53.19

19.91

27.21

40 60

4.76 5.19

56.40 56.08

19.27 18.90

32.37 33.99

20

5.56

53.71

21.99

32.76

40 60

5.88 8.15

50.81 47.37

20.75 22.59

28.30 30.60

20

7.19

43.38

18.23

21.58

40 60

8.60 8.66

42.35 42.32

20.89 21.10

23.95 24.57

20

5.46

37.96

5.79

6.77

40 60

6.78 8.43

34.36 31.44

5.16 4.99

5.90 5.49

20

4.05

57.64

24.04

32.54

40 60

5.47 6.52

53.44 50.46

23.51 24.13

31.69 30.94

Color obtaineda

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Table 4 Colorfastness to washing at 40 ◦ C (AATCC Test Method 61-2010). Fastness

Mordant With-out

Color change Color staining Acetate Cotton Nylon Silk Viscose Wool

Pre-mordanting

Meta-mordanting

Post-mordanting

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

1–2

1–2

1–2

3

1–2

1–2

1–2

3–4

1–2

1–2

1–2

3–4

1–2

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

Note: Al = AlK(SO4 )2 , Cu = CuSO4 , Fe = FeSO4 , Sn = SnCl2 . Table 5 K/S, E*, L*, a*, and b* of the dyed fabrics before and after the washing test. Type of mordants

K/S

E*

L*

a*

b*

Without AlK(SO4 )2 CuSO4 FeSO4 SnCl2

4.88 1.17 3.81 2.44 1.19

20.28 11.03 10.92 2.72 10.80

−15.96 −5.88 −7.13 −2.39 −6.20

7.37 1.92 −3.29 0.88 7.37

−10.12 −9.14 −7.59 −0.98 −8.40

Jothi, 2008) or (b) the decomposition of the dye itself, resulting in a colorless or a differentially colored compound (Jothi, 2008). However, with an increase in color strength of the samples after washing (positive values of K/S*), this means the color did not significantly fade. The light fastness was fair to good (3–4), except for the fabric mordanted with stannous chloride, whose rating was 1 (very poor) as shown in Table 6. Color fastness to crocking is found to be in the range of 3–4 (fair to good), except for the non-mordanted fabric, whose rating was 4 to 4–5 (good to very good) when subjected to wet and dry rubbing respectively, as seen in Table 7. The ratings obtained for color fastness to water in terms of the degree of color change and color staining were good to very good (4 to 4–5), as shown in Table 8. The color fastness to perspiration in acid conditions of fabrics dyed with and without mordants ranged from 4 to 4–5 (good to very good), except for the fabric mordanted with ferrous sulfate, whose color change rating was poor to fair (2–3), as seen in Table 9. Table 10 summarizes the physical properties of fabric dyed with and without mordants at a dye concentration of 60% owf. and 40% owf. mordant concentration by using post-mordanting technique. The tensile strength and tearing strength of both non-mordanted and mordanted dyed

Note: Post-mordanting method.

Table 6 Colour fastness to light (ISO 105-B02:1994). Type of mordants

Without AlK(SO4 )2 (Al) CuSO4 (Cu) FeSO4 (Fe) SnCl2 (Sn)

Color change Pre-mordanting

Meta-mordanting

Post-mordanting

3 3 4 4 1

3 3 4 4 1

3 3 4 4 1

Table 7 Colorfastness to crocking (AATCC Test Method 8: 2007). Type of mordants

Color staining Pre-mordanting

Without AlK(SO4 )2 (Al) CuSO4 (Cu) FeSO4 (Fe) SnCl2 (Sn)

Meta-mordanting

Post-mordanting

Dry

Wet

Dry

Wet

Dry

Wet

4–5 4 3–4 4 4

4 3–4 3 3–4 3–4

4–5 4 3–4 4 4

4 3–4 3 3–4 3–4

4–5 4 3–4 4 4

4 3–4 3 3–4 3–4

Table 8 Colorfastness to water (AATCC Test Method 107-2009). Fastness

Mordant With-out

Color change Color staining Acetate Cotton Nylon Silk Viscose Wool

Pre-mordanting

Meta-mordanting

Post-mordanting

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

4

4–5

4–5

4–5

4–5

4

4–5

4–5

4–5

4–5

4–5

4–5

4–5

4–5 4 4 4 4–5 4

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

Note: Al = AlK(SO4 )2 , Cu = CuSO4 , Fe = FeSO4 , Sn = SnCl2 .

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Table 9 Colorfastness to perspiration (AATCC Test Method 15-2009). Fastness

Mordants With-out

Color change Color staining Acetate Cotton Nylon Silk Viscose Wool

Pre-mordanting

Meta-mordanting

Post-mordanting

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

Al

Cu

Fe

Sn

4–5

4–5

4–5

2–3

4–5

4–5

4–5

2–3

4–5

4–5

4–5

2–3

4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

4–5 4–5 4–5 4–5 4–5 4–5

Note: Al = AlK(SO4 )2 , Cu = CuSO4 , Fe = FeSO4 , Sn = SnCl2 . Table 10 Tensile strength, tearing strength, bending length, and flexural rigidity values. Type of mordants

Undyed fabric Without AlK(SO4 )2 CuSO4 FeSO4 SnCl2

Tensile strength (N)

Tearing strength (N)

Stiffness Bending length (cm)

Flexural rigidity (mg cm)

Warp

Weft

Warp

Weft

Warp

Weft

Warp

Weft

556.8 508.6 493.5 437.7 427.8 402.0

544.6 438.6 404.4 383.1 365.3 336.0

19.0 18.2 17.5 16.2 15.7 15.2

18.7 17.2 16.5 14.5 14.0 14.1

2.24 1.74 1.55 1.60 1.49 1.88

2.10 1.80 1.88 1.76 1.95 2.25

0.80 0.42 0.29 0.33 0.27 0.53

0.64 0.46 0.52 0.43 0.60 0.91

Note: Post-mordanting method.

fabrics are less than those of the undyed fabric by 8–38% and 4–25%, respectively. In addition, the mordanted samples yielded lower strength values as compared to the non-mordanted. A reduction in stiffness (bending length and flexural rigidity) of all dyed fabrics also occurred, except for the stannous chloride mordanted sample in the weft direction. This may be because stannous chloride is oxidized on exposure to air and thus may impart a stiff hand to the fabric (Sumanta and Konar, 2011). 4. Conclusion A natural dye extracted from mangrove bark has been applied to silk fabric through exhaust dyeing. For the range of conditions used in the experiments, the optimum dyeing effect was achieved at a temperature of 90 ◦ C, 60 min dyeing time and pH of 3. Further improvement in color yield was observed with increasing dye concentration and additional mordanting. Each metallic salt mordant gave different color shades from medium to dark reddish-brown for aluminum potassium sulfate, stannous chloride, and copper sulfate to significantly duller and darker shades for ferrous sulfate. All mangrove bark dyed silk fabric exhibited fair to very good color fastness to crocking and fair to good light fastness with the exception of samples mordanted with stannous chloride, whose light fastness was very poor. The water and perspiration fastness ratings were good to very good, except for the fabric mordanted with ferrous sulfate, whose color change rating was poor to fair for perspiration fastness. However, the overall wash fastness was rated very poor to poor as a result of a change of color shade but there was no fading of the color after the washing test in the basic standard detergent solution. Acknowledgements This research was supported by Rajamangala University of Technology Phra Nakhon, Thailand.

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