Journal of Saudi Chemical Society (2012) 16, 1–6

King Saud University

Journal of Saudi Chemical Society
www.ksu.edu.sa www.sciencedirect.com

ORIGINAL ARTICLE

Prediction of low-sensitivity reactive dye recipe in exhaust dyeing influenced by material to liquor ratio and nature of salt
Mansoor Iqbal a,*, Zeeshan Khatri b, Aleem Ahmed a, Javaid Mughal a, Kamran Ahmed a
Applied Chemistry Research Center (Textile Section), PCSIR Laboratories Complex, Off University Road, Karachi 75280, Pakistan b Department of Textile Engineering, Mehran University of Engineering and Technology, Jamshoro, Pakistan Received 10 January 2010; accepted 6 April 2010 Available online 25 October 2010
a

KEYWORDS Reactive dyes; Colorimetric data; Liquor to material ratio; Sensitivity and rightfirst-time

Abstract Reactive dyeings were carried out by exhaust method on 100% cotton knits. A trichromatic combination was chosen with only change in blue component. Colorimetric data were produced under controlled dyeing conditions by comparing the color difference between the target shade and resulting shades. Giving a change in liquor ratio and nature of salt the colorimetric data were regenerated again produced the shades. The data will be helpful to predict the low-sensitivity reactive dye recipe, which lead to the concept of right-first-time dyeing. The aim of this research is to help a dyer to select the right recipe. A set of the dye recipes was applied by dyeing with reactive dyes on cotton. Sodium chloride shows best results in terms of dye sensitivity as compared to Glauber’s salt at low liquor ratio that is 1:10. Blue BRF in combination with yellow and red shows best result as compared to navy blue BF.
ª 2010 King Saud University. Production and hosting by Elsevier B.V. All rights reserved.

* Corresponding author. Tel.: +92 3443046460. E-mail addresses: mansoorprocessing@hotmail.com (M. Iqbal), texcenter_2004@live.com (A. Ahmed), kamranfarooq20@hotmail. com (K. Ahmed). 1319-6103 ª 2010 King Saud University. Production and hosting by Elsevier B.V. All rights reserved. Peer review under responsibility of King Saud University. doi:10.1016/j.jscs.2010.10.015

1. Introduction The two concepts namely quick-response (QR) and right-firsttime (RFT) have significant consequences for the technology of dye application. The concept of RFT dyeing is necessary for QR processing lines, but it is very welcome also for conventional dyeing. It was originally promoted from ICI and expended from right-first-time to the so-called right-on-time and right-every-time concept. The development of instrumental colorimetric in the 1990 in both exhaust and continuous dyeing operations significantly strengthened this concept. Both QR and RFT are of recent economical development in dyeing technology (Zolinger, 2003).

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2 Where there is a close control of over the color strength of the dyestuffs and consistent substrate dyeability, it is often possible to operate so-called blind dyeing in which the computed dye recipe in the laboratory is used immediately for bulk dyeing. This shortens the dyeing time required, decreases dye house cost and offers quick response (QR) and rapid delivery to customer. Where repeat dyeing of the same color is required, it is usually possible to input the reflectance data gained from bulk dyeing in order to refine the database and thereby achieve a greater level of right-first-time (RFT) dyeing. Right-first-time, right-on-time, and right-every-time are the goal of the dyer, because it is the lowest cost of dyeing system that provides quick response for customer (Horrocks, 2000). Textile color is the most important quality parameter required by customer, which is difficult to achieve even with the support of modern colorimetry system and computer color matching due to the complexity of the dyeing processes (Globo, 2004). The robustness of recipe is defined as dispensing error that would produce a color difference of one unit between the correct recipe and the incorrect recipe. Robustness is the reciprocal of recipe sensitivity, and it follows that highly sensitive recipes are not very robust. Considering the RFT concept employing the low-sensitivity recipe may be an alternative approach. Should dyeing errors occur, the less sensitive the recipe to such errors, the more chance there is that the resultant shade will be successful (McDonaldd, 1997). The exhaustion of reactive dyes on cellulosic substrate is determined by number of factors; the most important are: the PH of dye bath, the temperature of dyeing, concentration of electrolyte, the time of dyeing and the liquor ratio (Beech, 1970). Theoretically, the material to liquor ratio in processing should be from 1:20 to 1:100, depending upon nature of fiber, construction and type of textile goods and type of machine used. The scenario has changed now and it is decided on various factors. It is very necessary to optimize the material to liquor ratio since it not only saves dyes, chemicals, energy, water and other resources hence improve the bottomline but also reduces load on pollution. Modern processing machines are designed with lower material to liquor ratio as one of the prime objective and it is also claimed as one of the features for sales campaign. The pad batch and continuous dyeing ranges operate at the lowest material to liquor ratio and the exhaust dyeing machines at the highest (Asolekar, 2000). Nearly all-major machine manufacturers now have units for dyeing at short liquor ratios. Investment in such units pays off because it cuts operating costs (energy, water, chemicals, dyes, etc.) and raises productivity by reducing processing times. The aim should be to dye at the shortest possible liquor ratio (Fowler, 1997). For the dyeing of cellulosic fibers with bifunctional reactive dyes, salt as well as alkalis is added at different stages. During the primary exhaustion stage, the dye is taken up into the fabric in the presence of added inorganic salt (Imada and Harroda, 1992). In this paper the concept of the color sensitivity of a dye mixture towards a target color has been developed. Errors may cause not only due to the colorant concentration but also due to the parameters such as temperature, time and liquor ratio as mentioned above. The present work has found an approximate method to predict the color sensitivity of a matching recipe to change in the dyeing parameter of liquor ratio and by changing the nature of electrolyte by using a computer color matching system. For the colorimetry, the reflectance values of the dyed samples were measured on an SF 650X spectrophotometer (Datacolor). CIELAB color values (lightness L*, chroma C*, and hue H*) were calculated and CIE-

M. Iqbal et al. LAB (color difference DE*, lightness difference DL*, chroma difference DC* and hue difference DH*) was determined (Test Method 153-1985, 1995). 2. Experimental 2.1. Material Scoured and bleached, optical brightener free 100% cotton knitted fabric with GSM 165 g/m2 was used for dyeing. A range of commercial reactive dyes from different manufacturers were used in the experimental work is shown in Table 1 with their respective color index numbers. The chemical auxiliaries used such as Sodium carbonate, Glauber salt, sodium chloride and soaping agent sandopan DTC non-ionic detergent were of commercial grade. 2.2. Equipmen – Dyeing was carried out on IR dyeing machine of AHIBA USA. – Color matching system of Datacolor SF 650X USA was used for the evaluation of colorimetric data. 2.3. Procedure Dyeing was started at 40 °C and the temperature was gradually raised to 60 °C. The stock solution of dyes along with salt (80 g/ l) at room temperature was prepared and at 60 °C soda ash (20 g/l) were added and dyeing was carried out for 60 min. After dyeing the fabric was soaped with 2 g/l soaping agent, washed again with cold water and drained at room temperature. For achieving the best result we add salt (80 g/l) and soda ash (20 g/l) in portion. A Burgundy color was selected as a target shade and dyeing was carried out under control conditions at a liquor to material ratio 1:10, temperature 60 °C, time 60 min. A set of dyeing recipes was applied and colorimetric data were generated as given in Table 2. The colorimetric data of standard/target sample are given below: Target shade : L ¼ 24:76; K=S ¼ 19:98; %F ¼ 80:05 a ¼ 23:25; b ¼ 4:46;

2.4. Measurement of color strength The fixation of the dye in percentage was calculated first by the determining the reflectance R of the dyed samples at the wavelength of minimum reflectance (maximum absorbance) on Datacolour SF 650X spectrophotometer. The color yield (K/ S) values were the calculated by using the Kubelka–Munk equation (Eq. (1)) and the dye fixation % was evaluated using Eq. (2).

Table 1 List of commercial reactive dyes used in the experiment for dyeing.
Brand name 1 2 3 4 Sumifix Yellow EXF Red EXF Blue BRF Navy blue BF Rifafix Yellow 3RN Red 3BN Blue BRF Navy blue BF CI number 145 195 221 222

Prediction of low-sensitivity reactive dye recipe in exhaust dyeing
Table 2
Recipe Rifafix yellow = 2% Rifafix red = 5.5% Rifafix blue = 0.7% NaCl: 80 g/l L:R = 1:10 Rifafix yellow = 2% Rifafix red = 5.5% Rifafix blue = 0.7% G-Salt: 80 g/l L:R = 1:10 Rifafix yellow = 1.97% Rifafix red = 5.5% Rifafix navy = 0.5% NaCl: 80 g/l L:R = 1:10 Rifafix yellow = 1.97% Rifafix red = 5.5% Rifafix navy = 0.5% G-Salt: 80 g/l L:R = 1:10 Sumifix yellow = 2% Sumifix red = 5.5% Sumifix blue = 0.7% NaCl: 80 g/l L:R = 1:10 Sumifix yellow = 2% Sumifix red = 5.5% Sumifix blue = 0.7% G-Salt: 80 g/l L:R = 1:10 Sumifix yellow = 1.97% Sumifix red = 5.5% Sumifix navy = 0.5% NaCl: 80 g/l L:R = 1:10 Sumifix yellow = 1.97% Sumifix red = 5.5% Sumifix navy = 0.5% G-Salt: 80 g/l L:R = 1:10

3

Set of dyeing recipes and colorimetric data at a L:R = 1:10.
DE 0.52 L* 24.90 a* 23.21 b* 4.51 K/S 19.80 %F 76.21

0.95

23.16

24.63

4.58

20.01

78.12

0.68

23.05

23.26

5.89

19.85

78.0

0.50

24.96

22.86

5.68

19.88

79.12

0.52

24.90

23.21

4.51

19.80

80.01

0.84

22.98

24.62

4.16

20.11

81.16

0.68

23.05

23.26

5.89

19.85

81.28

0.50

24.96

22.86

5.68

19.88

79.92

K=S ¼ ð1 À R2 Þ=2R % Dye fixation ¼

ð1Þ

K=S values of sample after soaping  100 K=S values of sample before soaping ð2Þ

By giving a change in the liquor ratio of 1:20 taking other parameters, the same set of dyeing recipes was again evaluated with the same above method. Change in color brought about by change in liquor to material ratio up to 1:20 was also measured on the basis of CIELAB color space in terms of L*a*b* (Cartesian coordinates) as shown in Table 3. 3. Result and discussion 3.1. Build-up properties The use of a combination of different types of dyes to achieve deep shades requires the components to have a high degree of compatibility. Proper selection requires to build-up properties

of the individual dyes to be known. The color yields of the Rifafix and Sumifix reactive dyes studied are shown in Figs. 1a and 1b. For each complete dying the K/S values were determined at different concentration. For both the dyes the values of K/S increase as the dye concentration increases, which shows good build up developing. Sumifix red dye shows a good build up devolving at low concentration as compared to Rifafix red, while Sumifix (blue and yellow) and Rifafix (blue and yellow) behave in more or less same pattern. 3.2. Effect of salt Using standard dyeing profile, cotton fabric was dyed with Rifafix and Sumifix reactive dyes at two dye combinations and the type of salt is varied to check shade sensitivity against the standard shade. Table 4 shows the effect of salts on colorimetric data for dye combination 1 at liquor ratio of 1:10. It is obvious from the table that Sumifix is least sensitive to common salt attaining maximum %F 80.01 and DE 0.52 against

4
Table 3
Recipe Rifafix yellow = 2% Rifafix red = 5.5% Rifafix blue = 0.7% NaCl: 80 g/l L:R = 1:20 Rifafix yellow = 2% Rifafix red = 5.5% Rifafix blue = 0.7% G-Salt: 80 g/l L:R = 1:20 Rifafix yellow = 1.97% Rifafix red = 5.5% Rifafix navy = 0.5% NaCl: 80 g/l L:R = 1:20 Rifafix yellow = 1.97% Rifafix red = 5.5% Rifafix navy = 0.5% G-Salt: 80 g/l L:R = 1:20 Sumifix yellow = 2% Sumifix red = 5.5% Sumifix blue = 0.7% NaCl: 80 g/l L:R = 1:20 Sumifix yellow = 2% Sumifix red = 5.5% Sumifix blue = 0.7% G-Salt: 80 g/l L:R = 1:20 Sumifix yellow = 1.97% Sumifix red = 5.5% Sumifix navy = 0.5% NaCl: 80 g/l L:R = 1:20 Sumifix yellow = 1.97% Sumifix red = 5.5% Sumifix navy = 0.5% G-Salt: 80 g/l L:R = 1:20

M. Iqbal et al.
Set of dyeing recipes and colorimetric data at a L:R = 1:20.
DE 0.85 L* 26.18 a* 22.68 b* 4.62 K/S 18.91 %F 74.20

1.32

25.04

26.23

3.28

19.46

76.95

1.87

24.85

22.89

4.56

19.65

77.16

1.87

24.85

22.89

4.56

19.65

78.63

0.62

25.28

22.86

4.77

19.12

79.63

1.62

24.18

23.60

4.63

19.81

80.23

1.87

24.85

22.89

4.56

19.65

79.63

1.87

24.85

22.89

4.56

19.65

78.68

5
5

4

4

K/S Value

K/S Value
K/S Sumifix Blue BRF K/S Sumifix Red EXF K/S Sumifix Yellow EXF

3

3

2

2

K/S Rifafix Blue BRF K/S Rifafix Red 3BN K/S Rifafix Yellow 3RN

1 0 1 2 3

K/S Sumifix Navy Blue BF

1
6

K/S Rifafix Navy Blue BF

4

5

0

1

2

3

4

5

6

Dye concentration (%)

Dye concentration (%)

Figure 1a

Build-up properties of Sumifix dyes.

Figure 1b

Build-up properties of Rifafix dyes.

Prediction of low-sensitivity reactive dye recipe in exhaust dyeing the standard. Table 5 shows same dye combination but at liquor ratio 1:20. It gives DE 0.62 with slightly decreased in % fixation. Colorimetric data show that the common salt has less effect on Sumifix reactive dyes. Followed by dyeing cotton with dye combination 2, we obtained the results tabulated in Tables 6 and 7, which show the effect of salts on colorimetric data for dye combination 2 at liquor ratio of 1:10 and 1:20, respectively. Table 6 depicts that Sumifix is more sensitive to common salt than Glauber’s salt at liquor ratio of 1:10. Whereas both salts have adversely affected on DE of Rifafix and Sumifix dyes at liquor ratio of 1:20 and slightly decreased in % fixation too. Colorimetric data show that the Rifafix and Sumifix dyes are not sensitive to both common salt and Glauber’s salt at liquor ratio of 1:10 whereas the dyeing at liquor ratio of 1:20 resulted adversely, both dyes are sensitive to both salts, refer Table 7. 3.3. Effect of dyes combinations Fig. 2 demonstrates a comparison of two different combinations within the dye class Rifafix at liquor ratio 1:10. The Rifafix dye combination 2 offers not only good DE 0.50 against the
1 0.8 0.6
DE
Common salt

5

Glauber's salt

0.4 0.2 0 Rifafix 1 Rifafix 2 Sumifix 1 Sumifix 2

Dye combination

Figure 2

Effect of dye combination on DE at liquor ratio 1:10.

82 80
% Fixation

Common salt Glauber's salt

78 76 74 72

Table 4 Dye combination 1 – effect of common salt and Glauber’s salt on K/S at L:R = 1:10.
Type of salt Rifafix K/S Common salt Glauber’s salt 19.80 20.01 %F 76.21 78.12 DE 0.52 0.95 Sumifix K/S 19.80 20.11 %F 80.01 81.16 DE 0.52 0.84

Rifafix 1

Rifafix 2

Sumifix 1

Sumifix 2

Dye combination

Figure 3 1:10.

Effect of dye combination on % fixation at liquor ratio

Table 5 Dye combination 1 – effect of common salt and Glauber’s salt on K/S at L:R = 1:20.
Type of salt Rifafix K/S Common salt Glauber’s salt 18.91 19.46 %F 74.20 76.95 DE 0.85 1.32 Sumifix K/S 19.12 19.81 %F 79.63 80.23 DE 0.62 1.62

standard but also increased % fixation in cases of common salt used; the % fixation is shown in Fig. 3. The Sumifix results are less sensitive to both salts and show versatility of application; it is also observed, in this case, that the % fixation of Sumifix dye is achieved relatively high than the Rifafix dye. The dye combination 1 containing Sumifix blue BRF which shows good results than the combination 2 containing Sumifix navy blue BF. Fig. 2 also depicts that the dye combination 1 is less sensitive to common salt than that of Glauber’s salt.

Table 6 Dye combination 2 – effect of common salt and Glauber’s salt on K/S, %F and DE at L:R = 1:10.
Type of salt Rifafix K/S Common salt Glauber’s salt 19.85 19.88 %F 78.0 79.12 DE 0.68 0.50 Sumifix K/S 19.85 19.88 %F 81.28 79.92 DE 0.68 0.50
1.6 2
Common salt Glauber's salt

1.2

DE
0.8

Table 7 Dye combination 2 – effect of common salt and Glauber’s salt on K/S, %F and DE at L:R = 1:20.
Type of salt Rifafix K/S Common salt Glauber’s salt 19.65 19.65 %F 77.16 78.63 DE 1.87 1.87 Sumifix K/S 19.65 19.65 %F 79.63 78.68 DE 1.87 1.87

0.4

0 Rifafix 1 Rifafix 2 Sumifix 1 Sumifix 2

Dye combination

Figure 4

Effect of dye combination on DE at liquor ratio 1:20.

6
82 80
Common salt Glauber's salt

M. Iqbal et al. quor ratio 1:10. Dye combination 1 which contains blue BRF shows the best result as compared to navy blue BF. The less sensitive dye recipes which are very near to target shade are Sumifix yellow EXF 2%, Sumifix red EXF 5.5% and Sumifix blue BRF 0.7% at a liquor ratio of 1:10 with 80 g/l sodium chloride. The colorimetric data of this recipe: DE = 0.52, L = 24.90, a = 23.21, b = 4.51, K/S = 19.80, %F = 80.01. The dyer should take into account while selecting dye class and type of salt to be used in order to right-first-time dyeing. References
AATCC Test Method 153-1985, 1995. Color Measurement of Textile: Instrumental. Technical Manual of the AATCC. pp. 272–277. Asolekar, S., 2000. Environmental Problems in Chemical Processing of Textiles. IIT, Delhi. p. 18. Beech, W.F., 1970. Fiber Reactive Dyes. Logos Press Limited, London, p. 343. Fowler, P., 1997. New Trichromatic System for Enhanced Dyeing by the Exhaust Process. American Dyestuff Reporter. Globo, V., 2004. Influence of anionic dye sorption properties on the color of wool top. Tex. Res. J.. Horrocks, A.R., 2000. Handbook of Technical Textile. Wood Head Publishing, p. 211. Imada, K., Harroda, N., 1992. Recent developments in the optimized dyeing of cellulose using reactive dyes. J. Soc. Dyers Colourist 108, 210–214. McDonaldd, R., 1997. Color Physics for Industry. SDC Bradford, UK, p. 358. Zolinger, H., 2003. Color Chemistry. Wiley-VCH, p. 380.

% Fixation

78 76 74 72 70
Rifafix 1 Rifafix 2 Sumifix 1 Sumifix 2

Dye combination

Figure 5 of 1:20.

Effect of dye combination on % fixation at liquor ratio

Fig. 4 demonstrates another comparison of two different combinations within the dye class Rifafix at liquor ratio 1:20. Fig. 4 shows that Rifafix dye combinations are sensitive to both salt; only dye combination 1 in the presence of salt has close DE to the standard but the % fixation is decreased, refer Fig. 5. The Sumifix offers same profile as Rifafix except dye combination 1 which is relatively less sensitive in case of common salt. Overall liquor ratio of 1:20 shows adverse effect and dyes are more sensitive. 4. Conclusion Sumifix dye range is less sensitive and shows the best result as compared to Rifafix dyes in the presence of common salt at li-

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