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Influence of Neem oil pretreatment on the dyeing and antimicrobial properties of wool and silk fibers with some natural dyes
⁎Corresponding author. dreman411@yahoo.com (E.M. El-Khatib)
-
Received: ,
Accepted: ,
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.
Peer review under responsibility of King Saud University.
Abstract
Wool and silk fibers pretreated with neem oil and dyed with chlorophyll, saffron red and yellow natural dyes using economic methods such as microwave heating and ultrasonic energy. The effect of neem oil concentrations on color strength (K/S) was measured. The results indicated that, wool and silk fibers pretreated with neem oil recorded higher color strength values than the untreated fibers. Fastness properties and the color yield of the dyes under investigation on wool and silk fibers were evaluated. The results indicated that, color fastness to rubbing, washing and perspiration of all dyes are excellent to good and are approximately the same in microwave and ultrasonic method. The antimicrobial activity against bacteria and fungi were tested, and the results indicated that the samples pretreated exhibited higher inhibition percent than the untreated fibers. The morphologies structure of the untreated and treated wool fibers were examined by scanning electron microscopy (SEM). The untreated samples have a rough surface. The pretreated samples of wool fibers were swelling compared to the untreated fibers .The diameter of the fibers increased and have smooth and even surfaces. The changes in the surface morphology due to the effect of active ingredients of treatment with neem oil. This behavior as swelling and increase in diameter of the fibers leads to high penetration of the dyes in the fibers.
Keywords
Wool fibers
Silk fibers
Neem oil
Chlorophyll
Saffron red
Saffron yellow natural dyes
Antimicrobial activity
1 Introduction
The rapid growth in technical fibers and their end-uses leads to many requirements for the application of innovative modification in dyeing and finishing in textile industry. Novel treatments finishes of high added value for apparel fibers are also greatly appreciated by demanding consumer market. Antimicrobial textiles with improved functionality find a variety of applications such as health, hygiene products and several medical applications (Joshi, 2009a, 2009b).
In the last few years, the increase in new antimicrobial fibers technologies and the growing awareness about cleaner surroundings and healthy lifestyle. Textile products based on synthetic antimicrobial agents such as triclosan, metal and their salts, organo metallics, phenols and quaternary ammonium compounds, have been developed. Although, the synthetic antimicrobial compounds are very effective against microbes and give a durable effect on fibers, but it caused water pollution. Consequently, there is a great demand for natural antimicrobial textiles based on eco-friendly compounds which not only help to reduce health hazards associated due to microbial growth on textile material but also improve the environment (Hebeish et al., 2012; Joshi, 2009a, 2009b). The use of natural products such as chitosan (Shin et al., 2010) and natural dyes for antimicrobial finishing of textile fibers has been reported (El-Khatib et al., 2016, 2014; Ali et al., 2014). Other natural herbal products, such as Aloe Vera, tea tree oil extracts, can also be used for this purpose (Sanjay, 2013). There is a large source of medicinal plants has active antimicrobial ingredients. The study on natural products rich in antimicrobial agents, is very limited and not well documented. The reactions of herbal products as compared to modern synthetic pharmaceuticals, with their reduced cost, can be exploited as an effective eco friendly alternative to synthetic antimicrobial agents for textile applications. Recent developments on plant based bioactive agents have opened up new opportunities in research. Most of the papers in this area concentrate on the technical details of applying individual natural products. The review on the natural product based on antimicrobial finishing agents for application on textiles has been reported (Kwong et al., 2006, Thilagavathi et al., 2007).
The consumers are now aware of the hygienic life style and there is a necessity for textile products finished with antimicrobial properties by natural /products. The inherent properties of the textile fibers provide environment for the growth of microorganisms. Also, the structure of the substrates and the chemical processes may initiate the growth of microbes. Humid and warm environment increase the problem. Infestation by microbes causes cross infection by pathogens and produce odor. In addition, the staining and loss of the performance properties of textile fibers are the results of microbial attack (Ramachandran et al., 2004). In recent years antimicrobial textiles have gained interest from both academic research and industry because of their potential to provide high-quality life and safety benefits to people (Purwar and Joshi, 2004). Textile products are prone to host micro-organisms responsible for diseases, unpleasant odors, color degradation and deterioration of textiles. Antimicrobial textiles can be used to produce many goods such as sportswear, outdoor apparels, undergarments, shoes, furnishings, upholstery, hospital linens, wound care wraps, towels and wipes. Self-sterilizing fabrics could have potential benefits to reduce disease transfers among hospital populations, bio warfare protection and other applications.
Neem (Azadira chtaindica), an evergreen tree of India, belongs to the plant family Meliaceae (mahogany). It has been recognized as one of the most sources of compounds with insect control, antibacterial and medicinal properties (Rajendran, 2012).
Neem has been used as a traditional medicine against various human ailments from ancient times in Egypt. However, Neem has also received a lot of attention worldwide for its potential use as a herbal pesticide and other healthcare formulations in countries such as India, China, USA, France, Germany and Italy. The active ingredients of Neem are found in all parts of the tree but in general, seed, bark, leaves and roots are used for extraction purpose. The most important limonoids are azadirachtin and salannin. The Neem extracts have been widely used in herbal pesticide formulation because of its pest repellent properties has a potential to inhibit growth of bacteria both Gram positive and Gram negative (Kut et al., 2005).
From the point of view, the neem seed is the most important part of the plant given its content in oil and its many active molecules. That is why special attention is paid to the seed. However, research on the seeds has increased since the isolation of azadirachtin as a natural insecticide. It has multiple uses mainly for the soap, pesticide and pharmaceutical (Sidhu et al., 2003). It also has antibacterial, antifungal and medicinal properties (Imam et al., 2012).
The aim of this work is the pretreatments for wool and silk fibers by neem oil to enhance dyeing and the antimicrobial activity. It is necessary to avoid cross infection by pathogenic microorganisms. These treatments control the infestation by microbes. They also interrupt metabolism in microbes in order to reduce the formation of odor and to safeguard the fibers products from staining discoloration and quality deterioration.
On the other hand, the aim of this research to use extracted natural pigments which extracted from plants such as chlorophyll, saffron red and yellow dyes for dyeing wool and silk fibers. Natural dyes have been used for coloring fibers to protect the environment and prevent pollution caused by industries. The dyeing was carried out by using economic methods such as ultrasonic energy and microwave heating. These methods are economic and better but not be used in industry.
2 Experimental
2.1 Materials
2.1.1 Wool fibers
Wool fibers10/2, and silk fibers supplied by El Mahalla company-Egypt. Neem oil extract was purchased from ELGmhoria company, Egypt.
2.1.2 Dyestuffs
– Chlorophyll (a) dye (Chlorophyll-100-WSP: A commercial product by HANSEN‘S Company.
– Saffron yellow and red dyes (Saffron is the dried stigma of flowers of Crocus sativus L. Saffron red and yellow).
2.2 Apparatus
2.2.1 Microwave
The microwave equipment used in this experiment was the Samsung M 245 with an output of 1550 Watt operating at 2450 MHz (see Figs. 1–5).
Neem oil extract (pretreatment agent).
Chemical structure of effective constituent of neem oil extract.
Chlorophyll plant, Chemical Structure of Chlorophyll (a).
Saffron yellow and red dyes (Saffron is the dried stigma of flowers of Crocus sativus L. Saffron red and yellow dyes).
Structures of the chemical constituents of saffron.
2.2.2 Ultrasonic
Thermostated CREST benchtop 575 HT ultrasonic cleaner of capacity 5.75 L, frequency 38.5 kHz and with a maximum 500 Watt output was used. The output power levels are from 100 up 500 Watt.
2.3 Pretreatment of wool and silk fibers by neem oil
Wool and silk fibers treated by pad-dry-cure techniques. The wool fibers treated by neem oil extract at different concentrations (20–50%)and silk fibers treated by neem oil extract at concentrations (2–10%), then padded to 100% wet pick up, dried at 80 °C for 5 min. then cured at 120 °C for 3 min.
2.4 Dyeing procedure
2.4.1 Dyeing wool and silk fibers using microwave method
In a dye bath containing 2 g/l of chlorophyll dye, saffron yellow and saffron red dye with a liquor ratio 1:50, the wool and silk fibers were dyed by microwave heating at pH 5, time for 5 min. The dyed samples were rinsed by warm water and then cold water, washed in a bath containing 5 g/l non-ionic detergent at 50 °C for 30 min, then rinsed and dried in air at room temperature.
2.4.2 Dyeing wool and silk fibers using ultrasonic method
Wool and Silk fibers were dyed with (2 g/L) chlorophyll, saffron red and yellow dyes using ultrasonic energy at L.R 1:50, pH 5. The samples were dyed at temperature 50 °C for 30 min, the power energy of ultrasonic 500 Watt then the samples rinsed with cold water, washed in a bath containing 5 g/l non-ionic detergent, at 50 °C for 30 min then rinsed and dried in air at room temperature.
2.5 Measurements
2.5.1 Measurements of color strength (K/S value)
An Ultra Scan PRO spectrophotometer was used to measure the reflectance of the samples and hence, the K/S was measured spectrophotometrically at wave lengths (Chlorophyll dye: λmax 440, Saffron red dye: λmax 520 and Saffron yellow dye: λmax 385 nm). The color strength K/S of untreated and pretreated wool and silk fibers with neem oil extract dyed with Chlorophyll, saffron red and yellow dyes was evaluated.
2.5.2 Color data CIE LAB space
Color-difference formula CIE (L∗, a∗, b∗): The total difference CIE (L∗, a∗, b∗) was measured using the Hunter-Lab spectrophotometer (model: Hunter Lab DP-9000). CIE (L∗, a∗, b∗) between two colors each given in terms of L∗, a∗, b∗ is calculated from: L∗ value: indicates lightness, (+) if sample is lighter than standard, if darker than standard, a∗ and b∗ values: indicate the relative positions in CIE Lab space of the sample and the standard, from which some indication of the nature of the difference can be seen. Treated and untreated dyed wool and silk fibers were assessed, by measuring the color differences with each sample at five separate points and the average color difference (ΔE) between these points was determined.
2.5.3 Fastness properties
According to ISO standard methods. The specific tests were ISO 105-X12 (1987), ISO 105-C02 (1989) and ISO 105-E04 (1989), corresponding to color fastness to rubbing, washing and perspiration, respectively. The color changes of the samples were assessed against an accurate Gray scale.
2.5.4 Measurements of antimicrobial activity
The antimicrobial activities of wool and silk fibers dyed with chlorophyll, saffron red and yellow natural dyes and pretreated with neem oil was evaluated by using standard methods(serial dilution and plate count method according to Alen (1962). Experiment on soil bacteriology Burges Publishing Co. Minneapolis Minnesota USA.
The serial dilution blanks were prepared in bottles containing 99 ml distilled water and marked sequentially starting from 10−1 to 10−5 dilution and autoclave sterilized. 1.0 gm of each fabric sample was added in 99 ml solution i.e. 10–1 dilution. 1 ml from this was then transferred to 9 ml of the 10−2labeled test tube i.e. 10−2 dilution, using a fresh sterile pipette; and this was repeated for each succeeding step till 10−5. Nutrient peptone Agar media was used for counting of bacterial strains and for the counting of fungal strains potato dextrose agar (PDA) media was used. From 10−3, 10−4, and 10–5 dilution tubes, 0.1 ml of dilution fluid was then spread on sterilized petriplates in triplicates using the standard spread plate technique, for both bacterial and fungal strain isolation .The LB agar plates were then incubated at 37 °C for 24 h and the PDA plates were incubated at 27 °C for 72 h. After successful growth of microorganisms, characteristics of each distinct colony, e.g., shapes, color, transparency, etc. were determined. Gram stain was performed to observe the cellular morphology and gram reaction of the bacteria. The number of bacterial and fungal colonies in the fiber samples was counted and the density was expressed as Colony Forming Units (CFU). The antimicrobial activity was estimated and expressed as reduction in total count of fungi and bacteria in each treatment.
2.5.5 Scanning Electron Microscopy (SEM)
The surface morphology of untreated and pretreated wool fibers were investigated by using scanning electron microscopy (SEM), with a JSMT-20, JEOL-Japan. Before examination, wool fibers surface was prepared on an appropriate disk and randomly coated with a spray of gold. SEM was carried out at the National Research Centre (Egypt).
3 Results and discussion
3.1 Effect of concentrations of neem oil extract on wool fibers dyed with chlorophyll dye
The results obtained indicated that, the pretreatment using 30% concentration of neem oil extract gave the highest value of color strength (K/S) for wool fibers dyed with chlorophyll dye by microwave and ultrasonic methods as shown in Fig. 6, Fig. 7 illustrate samples of wool fibers untreated and pretreated with neem oil and dyed with chlorophyll dye by microwave method.
Effect of conc. of neem oil extract on the K/S of dyed wool fibers with chlorophyll dye by microwave and ultrasonic methods.
Samples of wool fibers untreated and pretreated with neem oil and dyed with chlorophyll dye by microwave method.
The Effect of Microwave heating mechanism is through ionic conduction, which is a type of resistance heating. Depending on the acceleration of the ions through the dye solution, it results in collision of dye molecules with the molecules of the fiber (Zhao and He, 2011).
Microwave dyeing takes into account the dielectric and the thermal properties of matter. The dielectric property refers to the intrinsic electrical properties that affect the dyeing by dipolar rotation of the dye and influences the microwave field upon the dipoles. The aqueous solution of dye has two components which are polar, in the high frequency microwave field. It influences the vibration energy in the water molecules and the dye molecules (Zhan and Zhao, 2009).
There are many hypotheses explaining the possible action of ultrasonic energy on the dyeing system. Theoretical explanations have been presented which attribute this effect to wave's high energy influencing the dyeing system by means of mechanical or hydrodynamic forces associated with cavitations which affected on the structure of dye (Shokry et al., 2010).
3.2 Effect of conc. of neem oil on silk fibers dyed with saffron red dye and yellow by microwave and ultrasonic methods
The results obtained indicated that dyeing silk fibers with saffron red and yellow dye by microwave and ultrasonic methods. The samples pretreated with 4% neem oil exhibited highest value of color strength (K/S). Generally the pretreated silk fibers gave higher results than the untreated as shown in Figs. 8 and 10. Figs. 9 and 11 illustrate samples of silk fibers untreated and pretreated with neem oil and dyed with saffron red and yellow dyes by microwave method.
Effect of conc. of neem oil on silk fibers dyed with saffron red dye by microwave and ultrasonic methods.
Effect of conc. of neem oil extract on silk fibers dyed with saffron red dye by microwave and ultrasonic methods.
Samples of silk fibers untreated and pretreated with neem oil and dyed with saffron red dye by microwave method.
Samples of silk fibers untreated and treated with neem oil and dyed with saffron yellow dye by microwave method.
In addition, the colorimetric CIE L∗a ∗b∗C∗h data were evaluated for dyed wool and silk fibers were shown in Tables 1–5. The color strength changes remarkably as different concentrations of neem oil were used while the Lab values show that samples treated with 4% are darker in shades. The results obtained revealed that, the pretreatment with neem oil extract enhanced the leveling properties.
Sample No.
K/S
L*
a*
b*
C*
H
ΔE
0%
6.00
42.59
−6.97
16.69
18.08
112.66
46.27
20%
7.31
54.62
−6.78
18.35
19.56
110.29
58.01
30%
10.6
49.96
−7.63
17.76
19.33
113.24
53.48
40%
9.71
49.14
−6.39
16.87
18.04
110.74
52.34
50%
10.0
48.52
−8.46
16.85
18.85
116.65
52.06
Sample No.
K/S
L*
a*
b*
C*
H
ΔE
0%
20.00
39.44
65.93
27.89
63.39
26.10
74.66
2%
25.35
39.43
57.48
28.83
64.30
26.64
75.43
4%
31.83
37.77
56.46
28.02
63.03
26.39
73.48
6%
29.54
38.15
65.80
27.94
63.30
26.19
73.91
8%
21.84
37.18
50.52
20.19
54.41
21.78
65.90
10%
20.80
35.18
40.52
20.89
52.41
20.78
64.90
Conc. of neem oil extract
K/S
L*
a*
b*
C*
H
ΔE
0
2.69
63.30
43.91
4.83
44.17
6.27
56.76
2%
4.27
44.75
43.92
10.15
45.08
13.02
51.10
4%
23.32
60.66
56.92
20.05
60.35
19.41
71.24
6%
7.83
42.51
52.79
14.10
54.64
14.95
63.89
8%
5.17
49.65
49.93
14.85
52.02
16.28
59.08
10%
2.42
45.03
45.88
15.10
48.00
17.08
51.12
Conc. of neem oil extract
K/S
L*
a*
b*
C*
H
ΔE
0%
12.96
73.53
16.19
81.92
83.51
78.82
112.27
2%
22.27
71.29
20.64
88.93
91.29
76.93
115.82
4%
15.02
75.13
15.42
86.51
87.87
79.89
115.61
6%
17.40
70.97
17.43
83.30
85.11
78.18
110.81
8%
13.56
71.56
23.77
79.47
82.95
73.35
109.55
10%
12.56
70.56
23.75
76.42
81.90
71.35
107.53
Conc. of neem oil extract
K/S
L*
a*
b*
C*
H
ΔE
0
1.66
84.32
5.35
69.28
69.48
85.58
56.71
2%
3.05
79.76
9.00
56.28
56.99
80.02
41.66
4%
12.33
87.28
2.53
56.44
56.49
87.44
41.66
6%
10.23
73.75
10.90
82.80
83.51
82.50
88.36
8%
5.75
82.12
7.12
81.92
82.23
85.03
66.73
10%
3.86
79.97
6.08
5.86
66.14
84.73
50.63
3.3 Fastness properties and the color yield of chlorophyll, saffron red and yellow dyes on wool and silk fibers
Fastness properties and the color yield of the dyes under investigation on wool and silk fibers were evaluated. Table 6 indicate that color fastness to rubbing, washing and perspiration of all dyes are excellent to good and are approximately the same in microwave and ultrasonic methods, because the dye was fixed due to the treatment with neem oil. Alt = change in color, SC = staining on cotton, SW = staining on wool.
Dye
Fastness to rubbing
Wash fastness
Fastness to Perspiration
Alkaline
Acidic
Dry
Wet
Alt
SC
SW
Alt
SC
SW
Alt
SC
SW
Chlorophyll dye
5
5
4–5
4–5
4–5
5
4–5
4–5
4–5
5
5
Saffron yellow
4–5
4–5
5
5
4–5
5
4–5
4–5
5
4–5
4–5
Saffron red
4–5
5
5
5
4–5
5
4–5
4–5
5
4–5
4–5
Untreated
4
3
3
4
4
4
3
3
3
4
4
3.4 Antimicrobial activities of wool and silk fibers
The antimicrobial activities of dyed wool and silk fibers dyed with chlorophyll, saffron red and yellow dyes and pretreated with different concentrations of neem oil were expressed as reduction percents in total count of fungi and bacteria associated with 1 gram of treated fibers as shown in Figs. 12–14 (El-Mohamedy and Abdalla, 2014a, 2014b).
Antimicrobial activities of wool fibers untreated and treated with neem oil extract and dyed with chlorophyll natural dye.
Antimicrobial activities of silk fibers untreated and treated with neem oil extract and dyed with saffron red natural dye.
Antimicrobial activities of silk fibers untreated and treated with neem oil extract and dyed with saffron yellow natural dye.
Antimicrobial activity, expressed as growth reduction of the microorganisms, could be explained as follows, the hydroxyl groups in neem oil structure interfere with the bacterial metabolism by stacking at the cell surface and binding with DNA to inhibit m-RNA synthesis. The increasing of concentration of neem oil shows more tendencies to deposit on the surface of the fibers resulting in hydroxyl groups more easily accessible to microorganisms. Wool fibers treated with neem oil and dyed with the chlorophyll natural dye display high growth reduction of microbes.
3.5 Surface morphology
The morphologies structure of the untreated and pretreated wool fibers were examined by scanning electron microscopy (SEM). Effect of treatment with 30% conc. of neem oil using scanning electron microscope (SEM) for wool fibers, Fig. 15a, Fig. 15b represent the SEM images of untreated and treated wool fibers respectively. The untreated samples have a rough surface as shown in Fig. 15a, the treated samples as shown in Fig. 15b indicate that the treated wool fibers were swelling compared to the untreated fibers, the diameter of the fibers increase and have smooth and even surfaces. The changes in the surface morphology due to the effect of active ingredients of treatment with neem oil.
SEM for untreated wool fibers.
SEM for pretreated wool fibers with 30% conc. of neem oil extract.
4 Conclusion
Dyeing wool and silk fibers with chlorophyll, saffron red and yellow natural dyes pretreated with neem oil extract as (pretreatment agent) by microwave heating and ultrasonic energy methods, exhibited higher results of color strength (K/S) value than the untreated fibers.
Microwave dyeing takes into account the dielectric and the thermal properties of matter. The dielectric property refers to the intrinsic electrical properties that affect the dyeing by dipolar rotation of the dye and influences the microwave field upon the dipoles. The aqueous solution of dye has two components which are polar, in the high frequency microwave field. It influences the vibration energy in the water molecules and the dye molecules.
The antimicrobial activities of wool and silk fibers pretreated with different concentration of neem oil and dyed with chlorophyll, saffron red and yellow natural dyes were expressed as reduction percentages in total count of fungi and bacteria were increased. The antimicrobial activities of wool and silk fibers pretreated with neem oil gave higher results than untreated fibers. These treatments control the infestation by microbes. They also interrupt metabolism in microbes in order to reduce the formation of odor and to safeguard the fibers products from staining discoloration and quality deterioration.
It was found also that the use of microwave and ultrasonic energy in dyeing processes offers advantages from the point of view uniform dyeing and conservation of energy and time. The dyed fibers are used in manufacture of carpets by handlooms.
Acknowledgment
This project was supported financially by the Science and Technology Development Fund (STDF), Egypt, Grant No 10390.
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