Rjet 424 (1)ecodye-paper Corrected.docx

Research

Extraction of dye from Ixora coccinea and Beta vulgaris for eco-dyeing Veerabhuvaneshwari Veerichettya*, Baby Shalini Ma, Balaji Sadhasivamaa, Saraswathy Nachimuthua aDepartment of Biotechnology, Kumaraguru College of Technology, Coimbatore-641049, Tamil Nadu, India *Corresponding Author E-mail: [email protected]

ABSTRACT: Dyeing is an important application in textiles because; it allows people to wear fabrics of different shades. Environmental issues of synthetic dyes led to gained customer interest in the natural dyeing sector again. In this article an effort has been made to use two plant sources as natural dye. Beta vulgaris commonly known as beetroot or sugar beet has several applications in food sector. Ixora coccinea is generally used as ornamental plant but it has been found to have several medicinal properties. In this study, extract from the flowers of Ixora coccinea and extract obtained from the peel of Beta vulgaris using methanol as solvent were analyzed for their phytochemical properties using TLC. The phytochemical compounds were identified as anthocyanins, phenolic acids in Ixora coccinea and carotenoids in Beta vulgaris. The extracts were then applied to treated, desized cotton fabric using various natural and chemical mordants. Based on analysis, the best mordant and technique for using mordant were determined for dyeing fabric. The fabric was subjected to dyeing and tested for its color fastness such as rubbing, washing and sunlight to know the best of all, with a view to natural dyeing of fabric and minimizing synthetic dyes, consequently to save environment. KEYWORDS: Ixora coccinea, Beta vulgaris, TLC, anthocyanins, phenolic acids, carotenoids, mordants, color fastness.

INTRODUCTION: Indians are considered as forerunners in the art of natural dyeing. Dyeing is an important application in textiles because; it allows people to wear fabrics of different shades. Initially, dyes were derived from naturally available plant materials predominantly leaves, flowers and from certain insect secretions (Cardon (2007)). The chemicals used for synthetic dyeing are toxic to the environment. Hence, the use of non-toxic, eco-friendly natural dyes on textiles has become a matter of significant importance due to increased environmental awareness. Natural dyes find their applications in various sectors such as in the coloring of textiles, cosmetics and drugs (Gulrajani et al (1992), Deo & Desai et al (1999), Cristea & Vilarem (2006), Chengaiah et al (2010)). Owing to their non-toxic effects, they are also used in coloring food products (Reddy et al (2005), Korankye (2010)). Natural dyes produce soothing and soft shades when compared to synthetic dyes. Although indigenous knowledge system has been practiced over the years in the past, the use of natural dyes has been diminished over generations due to excessive demand, lack of documentation, precise knowledge on the extraction and dyeing techniques. Due to these reasons, it has not commercially succeeded like synthetic dyes.

MATERIAL AND METHODS: 2.1 Collection of plant materials and Extraction of dye Ixora coccinea flowers were collected from the lawn of KCT (Kumaraguru College of Technology), Coimbatore. The waste/peel of Beta vulgaris (Mathur & Bhandari (2001), Sivakumar et al (2009)) was also collected. The samples were collected and allowed to shade dry for 5 days and ground using a mixer into fine powder (Fig 1). The powdered material was then sieved to get particles of uniform size. The powdered sample was then extracted using different solvents: Acetone, ethanol, methanol and ethyl acetate. 1g of each powdered material was extracted using 15ml of above mentioned solvents in an orbital shaker for 1 hr at 50 rpm. At the end of the extraction process, the extract was obtained after filtration using a Whattmann filter paper. The optical density of these extracts was taken using a UV-Visible spectrophotometer, wavelength ranging 200-600 nm. Acetone, ethanol and methanol extracts showed higher values.

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Fig 1. (A) Flowers of Ixora coccinea

(B) Beta vulgaris

2.2 De-sizing The fabric was de-sized and treated to remove starch if any, as it might hinder the bonding between mordant, dye and the fabric. For de-sizing, the cloth was initially boiled in soap water for about 30 minutes. Then, it was washed in a current of warm water and finally in cold water. The fabric was then left to air dry and tested for dye absorption in all the 3 solvents. The dye extracted using acetone did not fix properly in the fabric which leads to a conclusion that ethanol and methanol works better in the fabric. 2.3 Extraction of Mordant Most of the natural dyes need mordant to fix in the fabric as they tend to increase the fastness properties of the dye. Different natural mordants like pomegranate rind and orange peel were tried. The mordants were also extracted using ethanol as solvent in a similar fashion and the extract was finally concentrated using flash evaporator. 2.4 Dyeing of Fabric using different Mordanting Techniques After extraction process, the dyes were applied to the fabric by three different mordanting techniques: premordanting, simultaneous-mordanting and post-mordanting using a predetermined quantity of mordants (refer appendix I). After this process, fastness tests were done on the dyed fabrics. 2.5 Color Fastness Test Color fastness is a measure of two different properties of a textile – the degree to which it changes color when it is subjected to a particular treatment or environment, and the tendency of the textile to cause staining of other fabrics with which it comes to contact. These properties are assessed using grey scales. 2.6 Washing fastness Test A dyed fabric is in contact with pieces of adjacent fabrics was mechanically agitated in a soap solution, rinsed and dried. Any changes in the color of the specimen and the staining of the adjacent fabrics were assessed with standard grey scales. It is cut to size 10*4 cm and a composite specimen was prepared using adjacent pieces. A washing machine or Launder-o-meter is used for the test. The washing liquor is prepared according to the requirements of the chosen test. The time and temperature are also set accordingly in the machine. After the test is over, the composite specimens were removed, rinsed twice in cold water for ten minutes and squeezed. The stitches were removed along the two sides, open out the component pieces and dried at room temperature. The change in color of the treated test specimen and the degree of staining of the pieces of adjacent fabric were evaluated with the help of grey scales. 2.7 Rubbing fastness Test The sample size of 14*5 cm was taken for rubbing. The test specimen fixed to the rubbing device by means of clamps such that the long direction of the specimen is parallel to the rubbing track of the crock meter. A dry rubbing cotton cloth was fixed over the lower end of the finger of the crock meter. It was rubbed in a straight line along a 10 cm on the specimen, 10 times to and fro in 10 sec with a downward force 22 N or 9 N on the finger. The staining of the rubbed cotton cloths was assessed using grey scales. 2.8 Sunlight fastness Test The dyed fabric was cut to 7 pieces of about 15*5 cm each and stuck into chart. Each piece was identified as day 1 to day 7, after the specimen was prepared, it was subjected to sunlight. The 1st piece sample was exposed to sunlight for 1day, 2nd piece 2 days and so on till 7th piece 7 days. After 7 days change in color of all samples was assessed using grey scales.

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2.9 Identification of phytochemicals using Thin Layer Chromatography For Beta vulgaris, the solvent/mobile phase Hexane: Ethyl acetate (8:2) and for Ixora coccinea solvent mixture containing Hexane: Toluene (9.5:0.5) was efficient to resolve the compounds. The separated spots were visualized under UV light in order to identify and detect the compounds resolved in the plates.

3. RESULTS AND DISCUSSION 3.1 Extraction using Different Solvents The grounded Ixora coccinea (Ghurde M. U. et al (2016)) and Beta vulgaris plant samples were extracted using the following solvents: Acetone, ethanol, methanol and ethyl acetate. The absorbance was identified and noted to select the best choice of solvent for extraction. Acetone, ethanol and methanol showed higher values. But, the dye extracted from acetone and ethanol did not fix to the fabric properly. So, methanol was selected as the best solvent for extraction of the natural dyes from the plant materials (Fig 2).

Fig 2. Methanolic extracts of (A) Beta vulgaris (B) Ixora coccinea (C) Orange peel extract (D) Pomegranate rind extract

3.2 Absorbance of the Dye Extracted from Ixora coccinea and Beta vulgaris The dyes extracted separately from the flowers of Ixora coccinea and from the peel of Beta vulgaris were examined to spectrophotometer, from 100 to 600 nm and the maximum absorbance of the individual extract was determined. The maximum absorbance of the dye extracted from Beta vulgaris using methanol as solvent was at 287 nm and for Ixora coccinea maximum absorbance was at 483 nm (Fig 3) and (Table 1).

Fig 3. A. Absorption maximum of dye extracted from Beta vulgaris

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Fig.3. B. Absorption maximum of dye extracted from Ixora coccinea

Table 1- Percentage Absorption of the Dye applied on the cotton fabric Sample

OD before dyeing

OD after dyeing

% dye absorption

Ixora coccinea

1.137

0.945

16.88

1.367

0.412

69.86

1.578

0.632

59.94

0.175

0.124

29.14

0.532

0.329

38.15

0.513

0.289

43.66

(w/o) Ixora coccinea (Nm) Ixora coccinea (Cm) Beta vulgaris (w/o) Beta vulgaris (Nm) Beta vulgaris (Cm)

(w/o- without mordant, Nm- Natural mordant, Cm- Chemical mordant)

3.3 Identification of phytochemicals using Thin Layer Chromatography Upon separation by TLC, methanolic extract of Beta vulgaris showed yellow to bright orange color indicating the presence of carotenoids. Similarly, methanolic extract of Ixora coccinea showed brown and pink color indicating the presence of phenolic acids and anthocyanins respectively after subjected to TLC (Fig 4).

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Fig.4. Thin layer chromatogram of (A) Beta vulgaris and (B) Ixora coccinea

3.4 Dyeing of Cotton Fabric using Different Mordants The dye extracted using methanol as solvent was applied to the de-sized, treated fabric using a variety of natural and chemical mordants. The best mordanting technique was chosen based on analysis by trials. On comparison with other mordants, it was identified that alum works better than rest of the chemical mordants. Even though other chemical mordants gave various shades, a pleasant aesthetic appeal was given only by alum. Similarly among the natural mordants, pomegranate rind extract produced better results than orange peel extract (Fig.5).

Fig.5. Naturally dyed cotton fabrics

Simultaneous-mordanting technique was identified to be the most effective for using natural mordants. Similarly post-mordanting technique was found to be effective for chemical mordants, which is similar to the results reported by Divya Lekshmi et al., 2013. After performing the color fastness tests of the dyed fabrics, it was seen that the Ixora coccinea dyed fabric without the use of any mordants showed very good rubbing fastness (Table 2). Also the fabric dyed with extract from Beta vulgaris dye using pomegranate rind extract as natural mordant showed very good to excellent washing fastness (Table 3). On exposure of these fabrics to sunlight, it was observed that the extract of Ixora coccinea along with pomegranate rind extract as natural mordant and alum as chemical mordant showed good light fastness (Table 4).

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Table 2- Rubbing fastness tests Sample

Change in color Grade

Staining Grade

Ixora coccinea

2/3

4/5

4/5

5

4

5

3

4/5

¾

5

2/3

5

(w/o) Ixora coccinea (Nm) Ixora coccinea (Cm) Beta vulgaris (w/o) Beta vulgaris (Nm) Beta vulgaris (Cm)

(w/o- without mordant, Nm- Natural mordant, Cm- Chemical mordant)

Table 3 - Washing fastness tests Sample

Change in color Grade

Staining Grade

Ixora coccinea

2

4/5

2/3

5

3

5

1

4/5

¾

5

2

5

(w/o) Ixora coccinea (Nm) Ixora coccinea (Cm) Beta vulgaris (w/o) Beta vulgaris (Nm) Beta vulgaris (Cm)

w/o- without mordant, Nm- Natural mordant, Cm- Chemical mordant

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Table 4 - Sunlight fastness test Sample Ixora coccinea

Day 1

Day 2

Day 3

Day 4

Day 5

Day 6

Day 7

½

½

½

1

1

1

1

¾

¾

¾

3

3

2/3

2/3

¾

¾

3

3

2/3

2/3

2

½

½

1

1

1

1

1

2/3

2/3

2

2

2

1/2

½

2

½

½

1

1

1

1

(w/o) Ixora coccinea (Nm) Ixora coccinea (Cm) Beta vulgaris (w/o) Beta vulgaris (Nm) Beta vulgaris (Cm)

w/o- without mordant, Nm- Natural mordant, Cm- Chemical mordant

4. CONCLUSION This study reveals that the pigment extracts obtained from the plant source Beta vulgaris can be of major use as colorants. TLC (Thin Layer Chromatography) separation of these extracts revealed the presence of various phytochemicals such as carotenoids, anthocyanins and phenolic acids in the extract. The extracts can hence be used as natural dyes to provide aesthetic color shades in cotton clothing. On performing the color fastness tests of the dyed fabrics, it was seen that the Ixora coccinea dyed fabric with pomegranate rind as natural mordant showed very good rubbing fastness. Also the fabric dyed with extract from Beta vulgaris dye using pomegranate rind extract as natural mordant showed very good to excellent washing fastness. On exposure of these fabrics to sunlight, it was observed that the extract of Ixora coccinea along with pomegranate rind extract as natural mordant and alum as chemical mordant showed good light fastness. On the whole, 100% cotton fabric dyed using the extract obtained from flowers of Beta vulgaris with the help of pomegranate rind as mordant is the most preferred.

ACKNOWLEDGEMENT: The authors are grateful to the Dr.R.Shanthi for her support and guiding us in using facilities at Department of Fashion Technology, Kumaraguru College of Technology.

CONFLICT OF INTEREST: The authors declare no conflict of interest.

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