Colorimetric Study on Polyamides Dyeing With Weld and Pomegranate Peel Natural Dyes

Abstract

In this research, yellow color on nylon was produced by dyeing with weld (Reseda luteola) and pomegranate peel as natural dyes. The aluminum potassium sulphate salt was used as mordanting agent and four different methods of dyeing as non-mordanting, pre-mordanting, meta-mordanting, and after-mordanting were applied. The dyeing behavior of dyes was assessed by colorimetric evaluations and fastness properties. The spectrophotometric properties of dyed samples were also studied by Principal Component Analysis (PCA). Based on colorimetric evaluations, weld in comparison with pomegranate peel resulted in lighter and yellower colors. The rubbing fastness in all dyed samples was excellent, while samples dyed with pomegranate peel showed better washing fastness properties. Also, the best light fastness was obtained by the after-mordanting dyeing method. Overall, the best results of fastness properties were obtained by using after-mordanting method.

Keywords

natural dyes nylon weld pomegranate peel

Natural dyes have many advantages, such as low toxicity and allergic reactions, in addition to biodegradability, because they are taken from animal or plant matter without chemical processing. However, the use of natural dyes declined to a great extent with the advent of synthetic dyes, which have moderate-to-excellent color fastness properties, in 1865. During the decade of the 1990s, the textile and apparel industries, particularly the coloration industry, have been widely criticized for their role in polluting the environment. For these reasons, the use of carcinogenic dyes has been restricted, and the use of natural dyes has increased (Bechtold & Mussak, 2009; Bechtold, Turcanu, Ganglberger, & Geissler, 2003; Derksen et al., 2003; Farizadeh, Montazer, Yazdanshenas, Rashidi, & Malek, 2009; Gaspar, Moiteiro, Turkman, Coutinho, & Carnide, 2009; Ghoranneviss et al., 2011; Ghouila, Meksi, Haddar, Mhenni, & Jannet, 2012; Lokhande & Dorugade, 1999; Nagia & EL-Mohamedy, 2007; Sarkar & Seal, 2003).

The rapid changes in trends, fashion, and the demand for good fastness properties on different substrates require a basic database describing possible applications of natural dyes; otherwise, too much parallel optimization work has to be done by each dyehouse (Bechtold & Mussak, 2009; Haar, Schrader, & Gatewood, 2013).

Pomegranate peel (Punica granatum, Pooste Anar in Persian) is a representative source for plant-based yellow dyes. P. granatum is from the family Punicacea, which grows in Iran, India, Mediterranean countries, and all warm countries of the world; it was originally been a native of Persia. The main coloring agent in the pomegranate peel is granatonine (Figure 1), which presents in the alkaloid form of N-methyl granatonine (C₉H₁₅NO; Bechtold & Mussak, 2009; Keheyan & Giulianelli, 2006; Legua et al., 2012; Viuda-Martos, Fernandez-Lopez, & Perez-Alvarez, 2010). There is also a considerable amount of tannin, about 19%, in the pomegranate peel (Figure 1).

Figure 1.

Chemical structure of dyeing material in pomegranate peel (A) granatonine and (B) tannin (Bechtold & Mussak, 2009; Keheyan & Giulianelli, 2006).

Weld (Reseda luteola [Figure 2], Sparak in Persian), which grows widely around the world (Europe, Western Asia, and North America) is another representative source for plant-based yellow dyes. It is a perennial plant that produces a yellow dye (luteolin) from its foliage and flowers (Bechtold & Mussak, 2009; Cristea, Bareau, & Vilarem, 2003; Cristea & Vilarem, 2006; Gaspar et al., 2009). Weld, luteolin, and its sugar derivatives are considered to produce the most stable yellow shades and thus have been widely used for dyeing. The chemical structure of R. luteola is given in Figure 2.

Figure 2.

Reseda Luteola structure (Cristea et al., 2003).

Nylon is a polyamide that is mostly manufactured through condensation polymerization of diamine and diacid. Generally, nylon is dyed with acid dyes as well as reactive and disperse dyes (Baig, 2010; Broadbent, 2001). Some researchers have studied dyeing nylon with natural dyes such as indigo, onion, lac, turmeric, kamala, and henna (Agrawal, 2012; Badri & Burkinshaw, 1993; Baig, 2010; Lokhande & Dorugade, 1999).

The literature survey indicates that there have been relatively few works investigating the dyeing of nylon with weld and pomegranate peel. It has been previously shown that principal component analysis (PCA) technique can be used to study the colorimetric properties of colors in textile dyeing. PCA is a useful statistical technique for finding patterns in data and expressing the data without much loss of information. It does so in such a way as to highlight the similarities and differences in the data. The other main advantage of PCA is that once patterns in the data, and we compress the data. Weld and pomegranate are important natural sources for producing yellow shades on the textile samples. In addition, there have been relatively few research works on the dyeing of nylon with these yellow-coloring natural dyes. On the other hand, in order to demonstrate the merits of the PCA technique for explanation and comparison of the colorimetric properties of natural dyes, we selected natural dyes, weld and pomegranate, with relatively similar shades and spectral shapes. In this research, the natural yellow color on the nylon fabrics was obtained with pomegranate peel and weld dyes by using different methods of dyeing as non-mordanting, pre-mordanting, meta-mordanting, and after-mordanting. The dyeing behavior and colorimetric and fastness properties of dyed samples were extensively investigated. The conventional methods of colorimetric evaluation and comparison in textile dyeing involve studying the spectrophotometric data (i.e., reflectance spectra), K-M spectra, and color values. In the present work, PCA was also carried out to provide sufficient information about the spectrophotometric and colorimetric properties of dyed samples. The applicability of the PCA method and advantages of the technique over the conventional methods have been reported in the literature.

Experimental Procedure

Material

Scoured nylon fabric (plain weave and medium weight) was purchased commercially. Weld (R. luteola) flowers and pomegranate peels were obtained from Yazd province, Iran. Aluminum potassium sulfate (KAl (SO₄)₂.12H₂O) and acetic acid were purchased from Merck.

Method

Dye extraction

First, fine dried powders of natural dyes were wetted for 24 hr and then boiled for 1 hr. The extracts were cooled and filtered, and subsequently the filtrate dye solutions were used for dyeing the nylon samples.

Dyeing

Four different methods were used for dyeing of nylon samples: (1) non-mordanting: The dyeing process was started at room temperature, and the temperature was raised to boil over 30 min; dyeing continued at boil for 1 hr with a liquor-good ratio of 40:1. Finally, the dyed samples were rinsed with tap water and dried at room temperature. (2) Pre-mordanting method: The samples were first mordanted by treating them with aluminum potassium sulfate salt at boiling temperature for 45 min in a bath with the liquor-good ratio of 40:1. The concentration of mordant was 5% on the weight of the sample, and the pH was adjusted at 5 using acetic acid. The fabrics were then rinsed with tap water and dried at room temperature. Subsequently, the mordanted nylon samples were dyed with solutions of natural dyes. The dyeing process was done similar to the non-mordanting method, and the dyed samples were then washed with tap water and dried at room temperature. (3) Meta-mordanting method: The mordant and dye were added to the dyeing bath simultaneously. Subsequently, the dyeing process was carried out by raising the temperature to boil and continued for 1 hr. After the dyeing, the samples were washed with tap water and dried. (4) After-mordanting method: in this method, the samples were first dyed with weld or pomegranate dye, similar to the non-mordanting method. The samples dyed were rinsed and dried and then the after-mordantation process was carried out with mordants at boil for 45 min. At the end of the mordanting period, the mordant bath solution was removed and the rinsing procedure started. Finally, the samples were dried at room temperature.

Color measurements

The reflectance spectra of the dyed samples were measured using a Gretage Macbeth Color Eye 7000A spectrophotometer within the visible spectrum at 39 wavelengths with 10 nm interval from 380 nm to 760 nm. The $(\frac{K}{S})$ values were determined using the Kubelka–Munk equation. (Equation 1; Lee, 2005)

{(\frac{K}{S})}_{λ} = \frac{{(1 - R_{λ})}^{2}}{2 \times R_{λ}},

where K and S are the absorption and scattering coefficients, respectively, and R is the reflectance spectra of dyed fabric at λ_max.

CIELab coordinates (Kuehni, 2005; Lee, 2005; Schanda, 2007; Shams-Nateri, 2008; L*, a*, b*, C*, h, where, L* describes lightness, a* represents redness-greenness, b* represents yellowness-blueness, C* is the saturation, and h is the hue angle) were measured under 10 degrees standard observer and D₆₅ standard illuminant.

PCA

The PCA is the basis of a new statistical method used in data analyses and compression. It is a simple, nonparametric method of extracting relevant information from confused data sets. PCA is a quantitatively accurate method for achieving simplification. The method generates a new set of variables, called principal components, which are linear combinations of original variables. The first principal component is a single axis in space. When each observation has been projected on that axis, the resulting value from a new variable and the variance of this variable is the maximum among all possible choices of the first axis. The second principal component is another axis in space, perpendicular to the first. Projecting the observations on this axis generates another new variable. The variance of this variable is the maximum among all possible choices of this second axis. The full set of principal components is as large as the original set of variables, but it is commonplace for the sum of the variances of the first few principal components to exceed 80% of the total variance of the original data. The first principal component accounts for as much of the variability in the data as possible, and each subsequent component accounts for as much of the remaining variability as possible. By grading the Eigen vectors for descending Eigenvalues so that the largest is first, an ordered orthogonal method can be created with the first Eigen vector having the direction of largest variance of the data. In this way, directions in which the data set has the most significant amounts of energy and variation can be found (Mohtasham, Shams-Nateri, & Khalili, 2012; Shams-Nateri, 2011; Smith, 2002; Westland & Ripamonti, 2004).

Fastness properties

The dyed samples were tested according to International Organization for Standardization standard methods. The washing- and rubbing-fastness properties of the dyed samples were measured according to ISO 105-C02 (1989) and ISO 105-X12 (1987), respectively, and the changes in the color were assessed by the gray scale. The light fastness properties of the samples were measured according to ISO 105-B02 (1988), and the changes in the color were assessed by the blue scale.

Result and Discussion

Reflectance Spectra

The reflectance spectra of the nylon dyed with 50% of weld and pomegranate peel are shown in Figure 3. From this figure, it can be seen that the shape of reflectance spectra of samples dyed with the two dyes are different, and the nylon dyed with weld dye in all methods of dyeing is lighter than the nylon dyed with pomegranate peel. The K/S value of a dyed sample is directly proportional to the concentration of dye present in the sample (Dev, Venugopal, Sudha, Deepika, & Ramakrishna, 2009). Figure 4 shows the absorbance (K/S) spectra of the nylon dyed with weld and pomegranate peel dyes in four different methods of dyeing: non-mordanting, bottom-mordanting, meta-mordanting, and after-mordanting.

Figure 3.

The reflectance spectra of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

Figure 4.

The unit (K/S) of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

As shown in Figure 4, the unit (K/S) of the samples dyed with weld dye in all different methods of dyeing is almost similar to the samples dyed with pomegranate peel dye. So it can be found that the color strength of dyes is almost equal, and the difference in lightness was due to the difference in the shade of samples.

Colorimetric Analysis

The absorption behavior of weld and pomegranate peel natural dyes on nylon is studied by analyzing the color parameter such as lightness (L*), chroma (C*), and hue angle (h). The lightness of the samples dyed with weld and pomegranate peel dyes in all methods of dyeing is shown in Figure 5. It can be seen that the sample dyed with weld dye is lighter than the samples dyed with pomegranate peel dye, while the samples’ lightness values were decreased by mordanting. Figures 6 and 7 show the chroma and hue of nylon dyed in the different dyeing methods of non-mordanting, bottom-mordanting, meta-mordanting, and after-mordanting, respectively. As shown in these figures, the chroma and hue of the dyed samples are different, and the chroma and hue of the samples dyed with weld dye are higher.

Figure 5.

The lightness of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

Figure 6.

The chroma of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

Figure 7.

The hue of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

In order to further investigate the color parameters of nylon dyed with weld and pomegranate peel dyes, a* and b* were calculated. The chromaticity distribution of the samples dyed is shown in Figure 8. In this figure, the vertical axis is b* (blueness-yellowness) and the horizontal axis shows a* (greenness-redness). It is clearly indicated that the samples dyed with weld dye are yellower than the samples dyed with pomegranate peel dye. Also, the samples dyed with weld dye have a green shade, while the samples dyed with pomegranate peel dye have a red shade.

Figure 8.

The CIELab color values of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

PCA

The Eigenvalues of the principal components of reflectance spectra for the samples dyed using different dyeing methods of weld and pomegranate peel dyes are shown in Figure 9. As seen in this figure, the Eigenvalues of the first principal components are the largest and most important values. Consequently, only the first principal component was investigated. Figure 10 shows the first principal component of the dyed samples. As shown in this figure, the principal component of the samples dyed with weld and pomegranate peel dyes in all methods of dyeing is different. So, variable reduction with PCA also shows the difference in reflectance spectra between the samples dyed with weld and pomegranate peel dyes.

Figure 9.

Eigenvalues of principal components of nylon dyed with (A) weld and (B) pomegranate peel dyes.

Figure 10.

Principal component analysis of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

Fastness Properties

The fastness properties of nylon dyed with weld and pomegranate peel are shown in Table 1. As can be seen, the rubbing fastness of samples dyed with weld and pomegranate peel dyes in all methods of dyeing is excellent. The washing fastness of dyed nylon was improved by mordanting. In all methods of dyeing, the washing fastness of nylon dyed with pomegranate peel dye was better than samples dyed with weld. The light fastness of dyed samples ranges from very poor to good. Overall, the best results were given by the after-mordanting method. However, the light fastness of after-mordanting is better than some other types of natural dyes used for nylon dyeing (Agrawal, 2012; Badri & Burkinshaw, 1993; Lokhande & Dorugade, 1999).

Table 1.

The Fastness Properties of Nylon Dyed With Weld and Pomegranate Peel Dyes With Different Dyeing Methods.

No	Dyeing Method	Dye	Fastness Properties
			Light	Washing	Rubbing
			Light	Washing	Wet	Dry
1	Non-mordanting	Weld	5	3	4–5	5
2	Non-mordanting	Pomegranate peel	3	4	5	5
3	Pre-mordanting	Weld	1–2	3–4	4–5	4–5
4	Pre-mordanting	Pomegranate peel	4–5	5	5	5
5	Meta-mordanting	Weld	2	4	5	5
6	Meta-mordanting	Pomegranate peel	2	5	5	5
7	After-mordanting	Weld	6	4	4–5	5
8	After-mordanting	Pomegranate peel	4–5	5	5	5

Conclusion

In this research, weld and pomegranate peel natural dyes, which produce yellow colors, were used for dyeing nylon fabrics. The obtained result shows that the samples dyed with weld and pomegranate peel have different reflectance spectra, unit (K/S), and shades of yellow color. The PCA method also showed the difference between the color of samples dyed with weld and pomegranate peel. The results of fastness properties of the samples dyed showed that the rubbing fastness is excellent for both the natural dyes. The washing fastness of nylon dyed was improved with mordanting. The best light-fastness was obtained by the after-mordanting dyeing method. Overall, the best results of fastness properties were obtained by using after-mordanting method.

Footnotes

Acknowledgment

The authors would like to express the grateful thanks to Iran National Science Foundation (INSF) for supporting this research.

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This research was funded by Iran National Science Foundation (INSF).

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