EXTRACTION OF NATURAL DYES FROM FLORAL WASTE

Dharmik Vaghela, Palak Munjani, Riddhi Upasani

Department of Petro-Chemical Technology, The Maharaja Sayajirao University of Baroda, Vadodara,
Gujarat- 390002, India
ABSTRACT
India, is a nation rich in religious diversity, boasts over 0.7 million temples that generate a substantial 9 million tons of
floral waste annually. This underscores a pressing issue of waste management, prompting the imperative to explore
efficient methods for disposing the floral waste.We conceived the idea of crafting natural dyes from the residual flower
waste found in various religious locations. Throughout history, natural dyes have been widely employed to color
materials such as food-grade items, leather, and natural fibers like wool, silk, and cotton. Despite the enduring tradition
of dyeing fabrics with natural extracts, this practice has faced a decline in popularity, attributed to the widespread
accessibility of affordable synthetic dyes. It's worth noting that these natural dyes, in contrast to commercially available
synthetic colors, might offer a safer alternative for human use. In India, temples witness the daily presentation of
numerous flower varieties, with Marigold (scientific name TAGETES ERECTA) and Rose (scientific name ROSA)
standing out as the most prevalent and ubiquitous choices. These flowers are rich in natural chemicals including essential
oils, flavonoids, carotenoids, and notably a primary pigmentation compound named Lutein, which is present in
Marigold.
Keywords: Floral waste, Waste Management, Natural Dyes, Tagetes Erecta, Rosa, Lutein.
I. INTRODUCTION
Dyes, organic compounds that add color, are used on diverse substrates like cosmetics, waxes, greases, plastics, paper,
leather, fur, hair, drugs, and textiles to enhance appearance. Historically, natural sources provided colors until synthetic
dyes became prevalent. Textile manufacturers shifted to synthetics due to availability and cost advantages. However,
most synthetic colorants are petro-chemically derived with hazardous processes, posing environmental threats. Growing
global awareness of eco-friendly products renews interest in textiles dyed with natural, eco-friendly dyes, particularly
those made from natural fibers.
Despite the popularity of synthetic dyes, natural dyes have a rich history in coloring food-grade materials, leather, and
natural fibers like wool, silk, and cotton. While natural dyeing has declined due to affordable synthetic dyes, it persists,
especially in the decentralized sector for specialist items alongside the widespread use of synthetic dyes in large-scale
textiles/apparel.
India, a religious country with over 0.7 million temples, generates about 9 million tons of floral waste annually.
Devotees offer flowers in temples, which often go unused, leading to environmental issues. This waste, including toxic
pesticides, contributes to 16% of river pollution, with over 8 million tons dumped yearly. The improper disposal of
flower waste poses threats of organic pollution, infectious diseases, and epidemics through contamination of drinking
water resources. Various flowers, like Moonflower (Dhatura), Red Hibiscus, Night Jasmine (Parijat), Lotus, Marigold,
Basil (Tulsi), Jasmine, etc. Amongst these, Marigold and Rose, are regularly offered in temples, exacerbating the
environmental impact.

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 II. CLASSIFCATION OF DYES
There are several ways of classification of Dyes.

Fig. 1: Classification of Dyes based on their methods of application, source of materials, and chemical structures.

III. MATERIALS
Cotton and silk served as substrates in the dyeing process, while Potash Alum and Sodium Hydroxide were
utilized as chemicals in the experiment. Initially, waste flowers were gathered from the temple near my house.
Subsequently, the collected flowers were sorted into two groups, Group 1 and Group 2, based on their quality.

Group 1 consists of the flowers which are suitable for extraction process and Group 2 consists of the flower which
directly goes to the composting for making the organic fertilizers which are not suitable to use in the extraction
process.

Further, the flowers of the Group 1 are then separated into its petals and receptacles. The petals of the flowers
are then shed dried and then after they are crushed to reduce it to the powder form and this powder of the dried
flower are then passed through the 212 microns’ screen. The undersized of the screening operation is used for
the extraction.
The scientific classifications are as follows.

Properties of Marigold: Properties of Rose:

Plant material: Marigold (Tagetes Erecta). Plant material: Rose (Rosa)
 Kingdom – Plantae  Kingdom – Plantae
 Order – Aster ales  Order – Rosales
 Family – Asteraceae  Family – Rosaceae
 Genus – Tagetes  Genus – Rosa
 Species – T Erecta  Species – Rose

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 IV. EXPERIMENTAL PROCESS
The dyeing of cotton with marigold and rose flower was carried out in four stages;
1) Pre-Treatment
2) Extraction of dyes from flower
3) Mordanting (fixing dye with fiber)
4) Dyeing
1) Pre-Treatment
Prior to the dyeing process, the fabric undergoes scouring to eliminate dust and other colorants. In this process,
cotton fabrics are washed with a detergent solution, maintaining the required fabric-to-liquor ratio. The scoured
material is then thoroughly rinsed with water and dried at a moderate temperature. Before dyeing or
mordanting, the scoured material must be soak in clean water for 30 minutes.
2) Extraction of colorants
After being plucked, flowers from the plant source were air-dried in an open setting with a warm air current.
Subsequently, they were crushed, dissolved in water, and boiled over a water bath for one hour within the
temperature range of 50-95⁰C for rapid extraction. The extracted color from the flowers was then filtered for
immediate use.
3) Mordanting
This technique involves fixing the dye on the fabric by employing a mordant. The mordant forms a compound
that binds the color to the fabric, imparting its properties to the cloth. In the absence of a mordant, most natural
dyes exhibit minimal or no effect on the fabric. To establish an affinity between the fabric and dye, a mordanting
chemical is essential for the majority of natural dyes.
We used Alum as a mordant. The alum (5%) is taken & dissolved in distilled water. After the soaking of cloth in
clean water it is dipped for 30 min. in our mordanted solution.

4) Dyeing
The samples of cotton & silk must be colored using dye extract while maintaining the necessary M: L ratio. By
mixing 3.3 gm of dye powder with 100 ml of distilled water, the marigold & rose dye extract has been made. The
dyeing process followed industry standards. The material was dyed, then washed in cold water and dried at room
temperature. After that, it has been soaked in brine to fix the color.

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 V. METHODOLOGY
Various dye extraction techniques are employed in industries to extract dye using a range of solvents. The
following are some of these techniques.
1. Conventional methods
2. Degradation Chamber
3. Development of Consortium
4. Soxhlet Extraction Process
5. Ultrasound assisted solvent extraction
6. Microwave assisted solvent extraction
7. Sub and Supercritical Fluid Extraction (SFE)

Conventional method: Using this method, the experiment is conducted. Below is a general overview of the
experimentation, along with appropriate operating parameters.
• Aqueous extraction method: In this method, dye extraction from flowers involved preparing an aqueous solution
using dried flowers powder (3.3 g in 100 mL distilled water). The extraction process took place within a
temperature range of 50⁰C to 95⁰C for 2 hours. The extracted coloring materials from the flowers were utilized for
dyeing fabric and yarn samples. Following the completion of the extraction procedure, the flowers were removed
from the liquor and subjected to a second round of dye extraction.
The study involves conducting the experiment in three distinct methods to examine the impact of heating and
reflux on extraction, with observations focused on the results obtained from dyed samples.

1) Method for dyeing with heating having no reflux:

The undersize of the 212 microns’ sieve tray was taken for the purpose of extraction. 3.3 gm of undersized
powder in 100 mL distilled water was taken in the round bottom flask and the extraction was carried out at the
temperature 50-95⁰C for 1 hour, the water vapor is released in atmosphere.
The extract was then immediately filtered by vacuum filtration and used for the dyeing purpose. The mordanted
& without mordanted sample is dipped in dye for 15 min. & dried at room temp. After drying the sample was
washed with cold water & then dried at room temp.

2) Method for dyeing with heating having total reflux:

The undersize of the 212 microns’ sieve tray was taken for the purpose of extraction. 3.3 gm of undersized
powder in 100 mL distilled water was taken in the round bottom flask and the extraction was carried out at the
temperature 50-95⁰C for 1 hour, the water vapor is totally refluxed by the condenser.
The extract was then immediately filtered by vacuum filtration and used for the dyeing purpose. The mordanted
& without mordanted sample is dipped in dye for 15 min. & dried at room temp. After drying the sample was
washed with cold water & then dried at room temp.

3) Method for dyeing without heating:

The undersize of the 212 microns’ sieve tray was taken for the purpose of extraction. 3.3 gm of undersized
powder in 100 mL distilled water was taken in beaker and the extraction was carried out at the room
temperature 30⁰C for 1 hour with constant stirring.
The extract was then immediately filtered by vacuum filtration and used for the dyeing purpose. The mordanted
& without mordanted sample is dipped in dye for 15 min. & dried at room temp. After drying the sample was
washed with cold water & then dried at room temp.

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 Fig. 2: Experimental Setup

Fig. 3: Solubility of dye in no reflux condition Fig. 4: Solubility of dye in without heating condition

Fig. 5: Solubility of dye in total reflux condition

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Fig. 6: Result of Dyeing with heating having no reflux (The left side displays the result of the rose dye, while the
right side shows the result of the marigold dye)

Fig. 7: Result of Dyeing with heating having total reflux (The marigold dye has not efficiently resulted)

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 Fig. 8: Result of Dyeing without heating (The left side displays the result of the rose dye, while the right side
shows the result of the marigold dye)

VI. ANALYTICAL METHODS FOR DYE CHARACTERIZATION

For characterization, purified dye powder is to be taken for preparation of 1% aqueous dye solution separately
and is subjected to wavelength scan in a microprocessor or computer attached UV-Vis absorbance
spectrophotometer for 190-1100 nm range.
There are two methods widely used to analyze the dye characteristics.
1. UV-Visible spectroscopic study
The UV-Visible spectroscopic analysis involves scanning the spectra of purified natural dyes in both aqueous and
non-aqueous solutions, covering the wavelength range of 190-700 nm or beyond. This scan reveals peaks and
troughs at different wavelengths, providing insights into the main hue, absorption characteristics, and properties
of the dye under UV light. The UV-Zone, with or without peaks, is indicative of the dye's behaviour under UV light
and may be correlated with its fastness.
For instance, the colorant from Neem bark (Ashish et al., 2016) exhibits two absorption maximum peak at 275
and 374 nm, while beet sugar, in a recent study (Ashish et al., 2016), demonstrates absorption bands at 220, 280,
and 530 nm.

2. Chromatographic analysis
Thin Layer Chromatography (TLC) analysis, as conducted by Ashish et al. (2016), serves as an initial assessment
tool for plants containing various phylo-compounds, including flavonoids (flavonols, flavones, flavanones,
chalcones/aurones), hydroxycinnamic acids, tannins, and Anthraquinone, which are the colour compounds
present in these plants.
Ashish et al. (2016) outlined a methodology for the separation and identification of natural dyes from wool fibres
using reverse-phase High-Performance Liquid Chromatography (HPLC) with a C-18 column. Employing two
quaternary solvent systems and one binary solvent system, the study produces chromatograms that unveil the
presence of dyes, isomers, and minor products in the analysed sample. The application of a linear gradient elution
method, as employed in the HPLC analysis of various dyes, such as those from plants, scale insects, red
anthraquinonoid, mordant dyes, and molluscan blue, red-purple, and indigoid vat dyes, enables a consistent
elution program suitable for determining different chemical classes of dye.
VII. DISCUSSION FOR THE EXPERIMENTAL RESULTS
The result and discussion of our experiments depends on the following parameters:
1. Effect of washing on color consistency of dyed sample:
Our studies indicate that a change of some of the colors could be noticed in the dyed samples after washing with soap.
This may be due to:
• The dye undergoes decomposition, leading to the conversion into a colourless or differentially coloured
compound.
• The dye detaches from the substrate due to the wear Dye-fiber bond between the natural dye and the fiber.

2. The color fastness (cf) to washing, light and rubbing on dyed cotton sample with alum as a mordant is
presented in the below table

Mordant Cf to washing (grade) Light Fastness (grade) Cf to Rubbing (grade)

Alum 4 4 Dry: 4-5
Wet: 4
Table 1: Color fastness of dyed Cotton sample with alum as mordant

3. Light fastness of dyed samples:

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Assessing the light fastness of dyed samples involves evaluating the inherent resistance of a dye or pigment to chemical
or photochemical deterioration. The chromophore of the dye contributes to this property, although the auxochrome can
significantly influence fastness in either direction. The arrangement of substitutions in dyes plays a crucial role in
determining their light fastness, where a specific substituent may enhance electron density around the reaction site,
facilitating oxidation, or conversely, reduce electron density, leading to an increase in reduction cases. Notably, the
structure of Marigold flower, characterized by two hydroxyl groups, demonstrates favorable fastness.

Fig. 9: Chemical structure of carotenoid

4. pH Value
The pH values of synthetic dyes range from 3.77 – 6.78. The pH value of the extracted dye also shows the pH value of
3.5 and 6.5 which is in the range of synthetic dyes. Thus, we can say that natural dyes can withstand the quality of
synthetic dyes.

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 Sr. Method Feed (in Solvent Temp. (in Heating time Stirring
No. grams) Concentration ⁰C) (in hrs.)
1 Dyeing with heating 3.3 100 ml 50-95 1 Not
having no reflux Distilled water Necessary

2 Dyeing with heating 3.3 100 ml 50-95 1 Not

having total reflux Distilled water Necessary

3 Dyeing without heating 3.3 100 ml Room No heating Not

Distilled water temp. Necessary
(30⁰C)
Table 2: Comparison between the methods performed during experiment

VIII. CONCLUSION
The present study showed that natural dye can be successfully extracted from the flowers of Tagetes Erecta &
Rose. The whole process of extraction is eco-friendly. The maximum dye extraction was observed at 95⁰C using
aqueous extraction method. The obtained results have shown that the dyeing potential of the marigold & rose
flower could be huge which can be used as a source of textile dyeing. The various color shades can be obtained
using safe and ecofriendly mordants.

Our experiment concludes the following:

1. For dyeing with Heating having no reflux
The impact of employing a mordant is noticeably greater than not using any mordant on the fabric. The color
absorbed by the textile treated with a mordant is more pronounced compared to the untreated fabric.
Furthermore, the efficiency of dye absorption by cotton cloth surpasses that of silk cloth in both scenarios,
whether mordant is used or not.

2. For dyeing with Heating having total reflux

In instances of total reflux, the color of the dye solution markedly contrasts with the condition of no reflux. This
distinction arises due to the absence of water vapor evaporation. The efficiency of fabric coloring is also
diminished in total reflux, attributed to the higher water content in the dye solution, resulting in a lower dye
concentration. Consequently, the coloring pigment is not as effectively absorbed by the fabric in this scenario.

3. For dyeing without Heating

When dyeing is conducted without heating, the extraction of color from the flower powder at room temperature
is notably inefficient, resulting in a less pronounced dyeing effect compared to the process involving heating.
Therefore, based on the aforementioned results, it can be deduced that optimal dyeing efficiency is achieved
within the temperature range of 50-95⁰C.

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