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Effect of extraction methods of natural colorants on

dyeability of chemical pulp.

Sofia G. Papadaki*, Magdalini C. Krokida, G. Vlyssides, Emmanuel G. Koukios
National Technical University of Athens, School of Chemical Engineering, 9-Heroon Polytechniou str., Zografou Campus,
157 73 Athens, Greece.
Nowadays, there is a worldwide resurgence of interest in natural dyes, in the frame of the overall return to the natural resources.
This trend is based firstly on the fossil fuel depletion and secondly on the increasing public awareness of the environmental and health hazards related to chemical product.
Moreover, the natural dyes which are derived from wastes of agricultural and forestry activity or the food and beverage industry and not edible plants show vital importance
referring to sustainability.
The natural colorants could be classified in five groups, the polyphenolic compounds such as flavonoids and tannins, the isoprenoids, the tetrapyrroles, the quinones and the nheterocyclic compounds.
The process of coloring fibrous products is based on the simple mechanism of binding to the surface of the fiber or being trapped within them a chromophore, chemical compound
that brings color.
One characteristic property of natural dyes is their limited resistance against leaching, which is the case of paper recycling. For this reason, their application in paper industry
shows great importance.
According to the literature there are great evidence that different extraction methods affect drastically the dyeing capacity of various plants.

The scope of this work is the evaluation of different extraction methods of natural colorants on the dyeing capacity of Allium cepa L. peels on chemical pulp.


Chemical pulp consists almost the 70% of the worldwide produced pulp from wood
annually. Moreover, studies have shown that the absence of lignin in chemical pulp leads to
the need of using larger amounts of dye in order to obtain the required colour comparing
with mechanical pulp . Thus, the optimization of chemical pulp dyeing is a matter of further
Chemical pulp originated from spruce softwood was used. The supplied chemical pulp was
torn into small pieces by hand and added into deionized water (2 % w/w mixture
consistency).Then, vigorous mixing of the resulting mixture took place for 6 h using a
mechanical mixer at 2000 rpm. After filtration, the produced pulp had moisture content of
92% w/w and was stored in an airtight plastic pot at 4 oC.

General assumptions
Optimum dyeing conditions (Td = 40 oC and td = 30 min).
The limiting saturation value, describes the fact that beyond this limit any
increase of the / ratio is unable to cause any further colour change, as the
pulp fibres cannot absorb any more dye.
Even in mild conditions the limiting saturation value for A. cepa L. peels is
around / = 1.4. Therefore, the experiments for optimization of extraction
method occurred with extracts produced at / ratio of 0.6 units. By avoiding
the saturation limit, every colour change would be significant.

The peels of Allium cepa L. (cultivation Morada d Amposta, red onion) is a great source of
natural dyes as it contains numerous dyestaff components such as anthocyanins and other
flavonoids. Moreover, it is an agricultural and food industry residue, which means zero
supply cost and zero environmental impact.
The peels were naturally dried in a dark place at room temperature and relative humidity
(RH) 50% approximately, for one week.The dried peels were torn by hand (5.00-10.00 mm
grain size) and stored in dark and dry place.















25,6 26,0 26,1

B. Dyeing
All the produced extracts were used for the dyeing of chemical pulp. The dyeing process was
realised by simple impregnation of the chemical pulp in the dyebath. This procedure was
defined as conventional dyeing process. The dyeing conditions were stable at optimum
levels: 40 oC dyeing temperature (Td) and 30 min residence time (td). The dyeing was realised
using a liquor ratio of 55:1 ml/g (for 1.8 g of oven-dried pulp a dyebath of 100 ml was used).
C. Hand sheet formation and color measurement
Isotropic handsheet were formatted according to SCAN-C-26:76 and SCAN-C-M5:76
methods. The handsheets were stored in a dark and dry place for at least 24 hrs before their
color determination. The CIE L*a*b* system was applied for the color determination of the
produced sheets.
The final dyeing result derived from the total color difference (E*ab) between each dyed
sheet and a reference sample (undyed sheet). The total color difference is given from the
following equation:

where L*= L*sample - L*reference, a*= a*sample - a*reference and b*= b*sample - b*reference






A. Extraction
For the production of the natural dyes, conventional, ultrasound and microwave assisted
aquatic extraction took place.
Conventional extraction
The examined extraction conditions varied from 40 to 80 oC extraction temperature (Te) and
from 15 to 60 min residence time (te), all the possible combinations were examined.
Ultrasound assisted extraction
The experimental conditions varied from 40 to 80 oC Te and from 5 to 15 min te. A Vibre-Cell
VC 750 ultrasonic processor set at 250 W and 20 kHz was used during the ultrasound
assisted extraction.
Microwave assisted extraction
The experimental conditions varied from 40 to 80 oC Te and from 5 to 15 min te. A Milestone
Start D Microwave Digestion System set at 200 W and 400 W, in order to achieve stable low
Te and high Te , respectively, was used during the microwave assisted extraction.
In all cases, specific amounts of the ground bark were extracted with 125 ml of deionized water. In
each experiment the determination of the specific amounts of extracted plant material resulting from
the / ratio, which derives from the oven dry weight of the extracted plant material
divided by the oven dry weight of the pulp dyed with the plant extract. The final extract
obtained after filtration of the insoluble residues through a copper filter fabric.







Extraction conditions (Te, te)

Figure 1. Impact of different extraction methods on E*ab.

In all cases, the dyeing result is getting stronger as the conditions are getting
The conventional extraction shows the weakest dyeing result, even at severe
The ultrasound assisted extraction at high Te performs strong dyeing result in
contrast with low Te , where the weakest dyeing result of all methods is
The microwave assisted extraction performs very strong dyeing result, even at
extra mild conditions.

The presented results prove that the Allium cepa L. can be used sufficiently as a
source of natural colorants for the chemical pulp.
The low extraction temperature and short extraction residence time that were
achieved using both methods show great industrial interest because of their low
cost and environmental impact.
Microwave extraction predominates because of the remarkable low residence
time and extraction temperature needed.
The low dyeing temperature and relatively short dyeing residence time show
great importance respecting to the low cost and ecofriendly procedures.
Water, energy and raw materials saving through the exploitation of the remain
liquor after the dyeing process is suggested.
Alternative exploitation of the remain plant material (absorbent, fertilizer or
biofuel) is recommended.

The research has been supported by the Senator Committee of Basic Research, Program PEVE
2009, R.C. No 65/1784 of the National Technical University of Athens.
The authors wish to thank the Athenian Paper Mills - Softex for the donation of the spruce
softwood chemical pulp.

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