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Fabrics containing cotton fibers were dyed in a continuous process by impregnating the fabric
with an alkaline solution of reactive dyes and then drying and heating it using electrically
generated infrared radiation followed by hot air. Optimal fixation of the dyes required a strongly
alkaline dye solution and heating the fabric to as high a temperature as possible consistent
with avoiding thermal damage to the fibers. Color consistency and quality were well-controlled
along the fabric length during both pilot- and industrial-scale continuous dyeing and the color
differences, relative to commercial products obtained by batch dyeing procedures with the same
recipes, were small. The infrared process offers reduced pollution loads in the washing liquors
from reactive dyeing because fixation yields were greater than those for the cold pad-batch dyeing
procedure, and no electrolytes or urea were needed in the initial dye solutions.
true equilibrium. Thus, neither type of trial would reach Table 2. Dye Fixation Yields for the Navy Blue Dyeing of
a true equilibrium in the pad bath but any tailing 100% Cotton with Solutions Containing Various Alkalis
caused by dye substantivity would have been visible at Different Concentrations
over the 2-3 bath replacements involved in the overall dye fixation yields %
trials. type and concentration of alkali
Dye Fixation Yields. Measurements of the reflec- temp at the 20 g/L 1.0 g/L 20 g/L Na2CO3 5.0 g/L
tance spectra of the dyeings (380-700 nm with a 10 nm IR oven exit, °C Na2CO3 NaOH 2.5 g/L NaOH NaOH
wavelength interval) were performed using a Diano 90 66.7 77.2 80.1 88.6
Match Scan II double-beam recording spectrophotom- 105 76.8 81.7 87.9 92.2
eter. This allowed calculation of the absorption spectra 120 81.7 83.8 93.6 96.5
of the dyeings (Kubelka-Munk K/S values as a function
of wavelength) and the CIELAB color coordinates for unexposed half of the sample. Despite the obvious
CIE D65 Illuminant and the CIE 1964 supplementary variations in daylight intensity, this comparison of
standard observer.4 In almost all cases, measurement identically exposed samples provided information on any
of the CIELAB color difference was with respect to the effect of the thermal dyeing process on the light fastness
appropriate commercial product obtained by jet dyeing of the dyeings.
of the polyester and subsequent cold pad-batch dyeing Finally, because a high-energy infrared heating pro-
of the cotton, using identical recipes to those given in cess involves possible thermal damage to both the cotton
this paper. and polyester fibers, the handle of the fabric was
Because a mixture of reactive dyes was used, and evaluated manually by comparing it with the handle of
because the polyester component was already colored standard fabrics dyed by the cold pad-batch procedure.
in two of the cases, the following equation was used to
evaluate the degree of reactive dye fixation,
Results
700 700
(∑
380
K/S(λ))W - (∑K/S(λ))P
380
Preliminary Trials. The initial work involved opti-
mizing both the physical and chemical variables used
% fixation ) × 100 in the thermal dyeing operation so as to maximize the
700 700 reactive dye fixation (maximum K/S values). The key
( ∑ K/S(λ))U - (∑K/S(λ))P physical operational variables were the fabric speed (2.3
380 380 m/min) that determined the residence time in the
infrared oven (36 s), the voltage supplied to the electri-
where the subscripts W, U, and P refer to dry samples cally heated tubular infrared sources (around 400 V),
of the washed dyeing, the unwashed dyeing, and the and the length of fabric in the hot air oven operating at
dyed polyester of the initial fabric, respectively. For 150 °C (2.3 m). The only important chemical variable
determining the dye fixation on fabrics of 100% cotton, was the strength and concentration of the alkali added
the summations for the polyester component were to the reactive dye solution just prior to impregnation.
ignored. This is only an approximate measure and its This phase of the work, for each of the recipes, quickly
validity is dependent upon the absence of ring-dyed confirmed what had been established previously.1,2
yarns that would produce a stronger absorption of light Optimum fixation required a relatively high concentra-
by the fabric.5,6 However, fixation yields for the reactive tion of a strong alkali (5 g/L NaOH) in the dye bath.
dyes were also measured by extracting the unfixed dyes This concentration is a compromise between maximizing
from the fabric before and after heating and determi- activation of the cotton toward reaction with the dyes
nation of the concentrations of the solutions and the and minimizing hydrolysis of the reactive groups of the
amounts of dye was done by spectrophotometry.1,2 The dyes during their residence in the dye bath. In addition,
fixation yields determined by extraction were within 2% high levels of dye fixation required heating the fabric
of those obtained using the above equation. in the infrared oven so that drying was complete and
Dyeing Quality Evaluation. The degree of dye the fabric temperature increased to 110 °C for the
bleeding during subsequent washing of the final dyed cotton/polyester and cotton fabrics, respectively. Heating
samples from the infrared process was compared to that to higher exit temperatures than these caused increased
from samples dyed by the cold pad-batch procedure in fabric stiffness and a deterioration of the fabric handle.
the laboratory. Samples of the final dyeings (5.00 g) Table 2 shows data for the navy blue dyeing of the 100%
were washed at 50 °C for 30 min in a dilute aqueous cotton fabric illustrating the effects of alkali type and
detergent solution (50 mL of 0.5 mL/L of Sandoclean concentration, and of heating to higher temperatures,
PCL (Sandoz)) and the absorption spectrum of the on the dye fixation yields.
washing solution determined (380-700 nm with a 10 Similarly, for the burgundy dyeing on cotton/polyester
nm wavelength interval). The degree of unfixed dye using dye baths containing 20 g/L NaHCO3, 20 g/L
desorption was evaluated by summation of the absorb- Na2CO3, 1.0 g/L NaOH, or 5.0 g/L NaOH, and with a
ance values for the 33 wavelengths. In addition, the fabric temperature at the infrared oven exit of 110 °C,
CIELAB color differences4 between the initial and tested the dye fixation yields were 10, 65, 62, and 72%,
samples were measured. respectively. For the burgundy dyeing using 5.0 g/L
Samples dyed using the thermal process and ap- NaOH in the dye bath, the CIELAB color difference was
propriate comparison standards, dyed by a cold pad- 1.85 (slightly yellower) with respect to the production
batch procedure, were inclined at 45° to the horizontal standard for this shade obtained from the mill. This was
and exposed to daylight under glass with half of each a most satisfactory result. This dyeing was barely
sample covered to prevent fading. The sum of the K/S influenced by the presence of salt in the dye bath, the
values at 33 wavelengths was recorded each week and dye fixation yield only increasing from 72 to 75% with
the color loss of the dyed fabric compared to that of the an addition of 50.0 g/L of anhydrous Na2SO4. The
Ind. Eng. Chem. Res., Vol. 44, No. 11, 2005 3957
Table 3. Continuous Dyeing Trials on the Pilot and reactive dyes, using exactly the same recipes as given
Industrial Scale in this paper. For the navy blue dyeing, the average
burgundy forest green CIELAB color difference with respect to the laboratory
navy blue on on cotton/ on cotton/ cold pad-batch dyeing was quite high because of the
100% cotton polyester polyester much lower dye fixation in the latter case (68%). The
Pilot-Scale Dyeings dyeings on the pilot scale in the laboratory and those
dye fixation yield % 94.1 ( 0.8 72.0 ( 3.5 74.0 ( 5.0 at the mill were carried out under different conditions.
integrated K/S values 302.1 ( 1.6 295.8 ( 5.4 293.4 ( 6.0 The solution pickup at the mill (58%) was lower than
CIELAB color 6.05 ( 0.11 a 2.87 ( 0.38 2.84 ( 0.49 that in the laboratory (72%), but despite this, the dyed
difference 1.60 ( 0.32a
fabrics produced at the mill had colors only slightly
Mill Dyeings different than those of the standard shades.
dye fixation yield % 72.0 ( 1.4 65.7 ( 3.5
integrated K/S values 293.7 ( 4.06 305.3 ( 5.95
Washing and Light Fading Tests. The bleeding of
CIELAB color 2.00 ( 0.05a 2.19 ( 0.20 residual unfixed dyes during subsequent washing and
difference the light stability of the dyed samples were examined
a Measured with respect to a sample dyed in the laboratory by
and compared to those of identically treated samples
the cold pad-batch process. dyed by the cold pad-batch procedure. For the burgundy
production standard from the mill, a similar laboratory-
scale cold pad-batch dyeing, and a pilot-scale burgundy
reactive dyes in the burgundy recipe are less reactive
dyeing obtained by the infrared process, the values of
than those in the navy blue recipe.
the integrated absorbance values for the washing solu-
The high concentration of NaOH required to obtain tions were 7.30 ( 0.97, 2.61 ( 0.06, and 2.74 ( 0.27,
maximum dye fixation was of concern because the pH respectively. Both the sample dyed using infrared
value of the bath was high enough to possibly cause radiation and the laboratory-scale cold-pad batch dyeing
rapid hydrolysis of the reactive groups of the dyes. Trials contained slightly more than a third of the amount of
carried out over a period of time with the same alkaline unfixed dyes as the sample produced by our industrial
dye solution (5.0 g/L NaOH) showed that there was no partner. They also had much smaller variations in the
significant loss of color strength of any of the dyeings amounts of residual unfixed dyes among the samples.
provided that the solution was not used for a period For the navy blue shade on the 100% cotton fabric dyed
exceeding 20 min. using the infrared procedure or by a cold pad-batch
One striking result of the optimization study was that method, the values of the integrated absorbance values
the hot air oven played almost no role in dye fixation. were 7.2 and 28.9 (single test of each sample). The very
We had initially assumed that 40-45 s of infrared high value for the cold pad-batch sample is a conse-
heating would not be sufficient to drive the fixation to quence of the much lower fixation yield for this dyeing
its optimum value and therefore chose to follow the (62%) and the inadequacy of the post-dyeing washing
infrared heating with hot air at a safe, constant high procedure in removing the large amounts of residual
temperature. The optimum dye fixation depended only unfixed dyes in this case. Color measurements and
on how high a temperature the cotton fabric reached in visual inspections on the washed and unwashed samples
the infrared oven. Even for dyeings where the fixation showed that the washing test did not result in any color
yield at the infrared oven exit was lower, as when using difference.
20 g/L Na2CO3 in the dye bath, further heating for 1 Exposure to daylight over periods of 3-6 weeks
min at 150 °C in the hot air oven did not increase the showed no decrease in the integrated K/S values for
yield by more than about 2%. either infrared or cold pad-batch dyeings. The thermal
Continuous Dyeing Trials on a Pilot and Indus- process thus had no influence on the color stability of
trial Scale. For the pilot-scale and industrial-scale the dyed fabrics to light exposure.
continuous dyeing trials, we measured the dye fixation At each stage in the project, fabric samples were
yield, the integrated K/S values determined from the examined to evaluate their handle. Provided that the
reflection spectrum, and the CIELAB color difference maximum temperatures at the infrared oven exit were
with respect to a cold pad-batch dyeing from the not exceeded, the dyeings produced by the thermal
finishing mill, unless otherwise indicated. Measure- process were of identical handle to those produced by
ments were taken at frequent intervals along the length the cold pad-batch method.
of dyed fabric, and also across the fabric width for
dyeings conducted at the mill. The results in Table 3 Conclusion
give the average values and the standard deviations of
The use of infrared radiation for drying and heating
each measured quantity over all the samples of a
fabrics containing cotton and impregnated with a strongly
particular dyeing. They show that the process was well-
alkaline solution of reactive dyes gave effective fixation
controlled and that, in all cases, any variations of the
and less residual unfixed dye in the final fabric. The
color difference along the fabric were negligible, a
thermal continuous dyeing process was well-controlled,
conclusion confirmed by detailed visual inspection by
did not result in end-to-end or side-to-side color varia-
our industrial partner. Note that the standard devia-
tions, and had no influence on color fading in daylight.
tions of the CIELAB color differences are all below 0.5.
The absence of electrolyte and urea from the reactive
Despite some temperature variations across the fabric
dye solution gave washing liquors with a much reduced
width at the exit of the infrared dryer at the mill, there
pollution load.
was no measurable or visible color variations across the
fabric width. The CIELAB color differences were deter-
Acknowledgment
mined with respect to the appropriate industrial dyeings
provided by our partner that were prepared by jet This project was funded by a Co-operative R&D grant
pressure dyeing of the polyester with disperse dyes from the University-Industry program of the Natural
followed by cold pad-batch dyeing of the cotton with Sciences and Engineering Research Council of Canada
3958 Ind. Eng. Chem. Res., Vol. 44, No. 11, 2005
and by Hydro-Québec and Consoltex Inc. The authors (4) McDonald, R. Colour Physics for Industry, 2nd ed.; Society
also gratefully acknowledge the collaboration of the of Dyers and Colourists: Bradford, UK, 1997.
Bureau de Liaison Entreprise-Université de Sherbrooke. (5) Motamedian, F.; Broadbent, A. D. The Effects of Dye
Distribution in Nylon Filaments on the Dyeing Color Yield and
Fastness Properties. Ind. Eng. Chem. Res. 1999, 38, 4656.
Literature Cited (6) Motamedian, F.; Broadbent, A. D. Modeling the Influence
of Dye Distribution on the Perceived Color Depth of a Filament
(1) Broadbent, A. D.; Thérien, N.; Zhao, Y. Effects of Process Array. Textile Res. J. 2003, 73, 124.
Variables on the Fixation of Reactive Dyes to Cotton Using
Infrared Radiation. Ind. Eng. Chem. Res. 1995, 34, 943.
Received for review December 6, 2004
(2) Broadbent, A. D.; Thérien, N.; Zhao, Y. Comparison of
Thermal Fixation of Reactive Dyes on Cotton Using Infrared
Revised manuscript received March 30, 2005
Radiation or Hot Air. Ind. Eng. Chem. Res. 1998, 37, 1781. Accepted March 30, 2005
(3) Broadbent, A. D. Basic Principles of Textile Coloration;
Society of Dyers and Colourists: Bradford, UK, 2001. IE040288R