3954 Ind. Eng. Chem. Res.

2005, 44, 3954-3958

MATERIALS AND INTERFACES

Continuous Dyeing of Cotton with Reactive Dyes Using Infrared

Heat

Arthur D. Broadbent,* Julienne Bissou-Billong, Miriem Lhachimi, Youssef Mir, and

Serge Capistran
Département de génie chimique, Faculté de génie, Université de Sherbrooke, Sherbrooke, Québec,
Canada J1K 2R1

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.

Introduction following points were considered in relation to the

In previous papers,1,2 we had shown that cotton fibers
can be effectively dyed with reactive dyes using infrared
heat to promote fixation, i.e., the reaction of the dye with
the cotton cellulose. The process involved impregnating
a cotton fabric with an alkaline solution of a reactive
dye and then passing it through an infrared oven where
drying and heating promoted fixation of the dye. The
dye fixation yield is the ratio of the amount of the dye
that has reacted with the cotton cellulose to the amount
initially present in the impregnated fabric. The best
fixation yields were obtained when the dye solution was
strongly alkaline (5.0 g/L NaOH) and the dried fabric
was heated to the highest permissible oven exit tem-
perature consistent with avoiding any thermal damage
to the fibers. It was established that infrared heating
gave higher fixation yields than those obtained under
similar conditions but using hot air as the drying and
heating medium. We think that the better penetration
of the radiant energy into the wet fabric, and the more
uniform internal heating that this provides, is respon-
sible for the higher fixation yields. During the first
phase of drying with hot air there is considerable
migration of the dye solution to the yarn surfaces where
evaporation is occurring. The use of infrared heat
suppresses such migration, and the ring-dyeing of the
yarns that it causes, particularly if short-wave infrared
sources are used with maximum emission at around 1
µm.2
The purpose of this paper is to describe further work
on this process related to its industrial application. The
* To whom correspondence should be addressed. Tel.:
(819) 821-8000 Ext. 2172. Fax: (819) 821-7955. E-mail:
Arthur.D.Broadbent@USherbrooke.ca.
10.1021/ie040288r CCC: $30.25 © 2005 American Chemical Society
Published on Web 04/21/2005
previous studies:
1. In this study, we used industrial dyeing recipes
typically containing three reactive dyes. In the previous
work only solutions of single dyes were used. The dyeing
of deep shades that are difficult to produce with high
efficiency in an industrial operation was given priority.
2. Because of the significance of cotton/polyester fiber
blends in the marketplace, the process was studied
using both cotton and cotton/polyester fabrics.
3. Our industrial partner’s equipment consisted of an
electric infrared predryer situated in front of a conven-
tional gas-heated hot air drying frame. We therefore
studied a dyeing process in which the fabric was initially
impregnated with alkaline reactive dye solution and
then dried and preheated in an infrared oven. It then
passed immediately into a hot air oven to complete dye
fixation at a safe but constant temperature.
4. In this study, particular emphasis was placed on
dyeing fabric continuously, on both a pilot and industrial
scale, over an extended period to show that color
consistency and quality could be achieved. The dyeings
obtained were compared with those from actual com-
mercial production using the same dye recipes but
different dyeing procedures.
5. Alkaline reactive dye solutions for pad-batch dyeing
invariably have considerable amounts of added salt (20-
50 g/L) and, in thermal fixation processes, of urea (100
g/L) to aid fixation.3 In this study, these chemicals were
not used, taking advantage of the higher fixation
obtainable when using infrared heat, and thus allowing
a process with a greatly reduced pollution load in the
post-dyeing washing liquor.

Table 1. Dyeing Recipes
burgundy on forest green on navy blue on
cotton/polyester cotton/polyester 100% cotton
Levafix Remazol Triactive Gold
Yellow EG Yellow RNL Yellow DF-RL
12.0 g/L (Dyestar) 4.47 g/L (Dyestar) 3.83 g/L (Tritex)
Levafix Brilliant Remazol Triactive
Red ERN Red RB Red DF-4BL
23.3 g/L (Dyestar) 0.935 g/L (Dyestar) 6.15 g/L (Tritex)
Drimarene Remazol Navy Cibacron Dark
Blue K-2RL Blue GG Blue WR
4.70 g/L (Sandoz) 6.16 g/L (Dyestar) 20.4 g/L (Ciba)
Experimental Procedures
Materials. Our industrial partner provided all dyes
and chemicals, and the dye recipes and fabrics. The
white bleached 100% cotton fabric used for the navy blue
dyeing was a simple woven fabric with a superficial
weight of 144 g/m2. The cotton/polyester fabrics used
for the burgundy and forest green shades were both
woven with a 100% polyester multifilament warp and
a 50/50 blended cotton/polyester filling. The superficial
weights were 185 g/m2 (burgundy) and 183 g/m2 (forest
green). The polyester fibers in both fabrics were pre-
dyed with a mixture of disperse dyes at 130 °C under
pressure in a jet dyeing machine at the finishing plant.
Three recipes for deep shades, each containing three
reactive dyes to dye the cotton, were used in this study
(Table 1). The amounts of the dyes used are in terms of
the bath concentrations. These recipes and dyes were
provided by our industrial partner and the dye sup-
plier’s names are given in parentheses.
Equipment. The pilot-scale continuous dyeing equip-
ment (Figure 1) consisted of a set of drive rollers, a small
impregnation unit (pad) with a 1.0 L dye bath, an
electric infrared oven that has been described previ-
ously,1,2 and an electrically heated (12 kW) hot air oven
(1.3 m3) with forced air circulation (19 m3/min). The
infrared oven was fitted with tubular electric sources
placed 5 cm above and below the fabric that passed
straight through the heating zone. Each tube consisted
of an iron/aluminum filament surrounded by a quartz
envelope and gave maximum emission at around 3 µm
at the maximum operating voltage of 450 V. Since the
fabric entering the hot air oven was dry, most of the
hot air was recycled. This unit was capable of heating
a dry fabric to a surface temperature of over 200 °C in
less than 30 s. The fabric speed (2.3 m/min) determined
the residence time in the infrared oven (35 s) and the
length of fabric passing over the adjustable rollers in
the air oven regulated the time in the hot air (60 s).
Dyeing Operations. The dyeing process consisted
of three stages: (1) impregnating the fabric with the
alkaline solution of the reactive dyes in the pad bath
and then squeezing out the excess solution to give a
water retention of 72-75% (on a dry basis, measured
by weighing and drying), (2) running the fabric at a
given speed through the infrared oven with each of the
four modules of emitters operating at the same voltage
(around 400 V, total power 13.1 kW), and finally (3)
passing the fabric through the air oven typically running
with the air at 150 °C.
Preliminary trials to establish the optimum operating
conditions for the best fixation were conducted using
fabric samples (200 × 25 cm) sewn into a leader cloth
(in the fabric accumulator) that then passed through
the infrared oven and the hot air unit. Once optimum
operating conditions had been established, continuous
Ind. Eng. Chem. Res., Vol. 44, No. 11, 2005 3955
Figure 1. Schematic of the pilot-scale equipment used for
continuous dyeing.
dyeing trials were carried out under those conditions.
This involved dyeing from 80 to 120 m of fabric at a
speed of 2.3 m/min. The bath volume was maintained
constant by addition of freshly prepared dye-alkali
solution (5.0 g/L NaOH). The bath had a volume of 1.0
L and therefore the volume of solution in it would be
totally replaced in about 13-14 min. Dye reactive group
hydrolysis was shown not to be problematic over this
time period.
Fabric samples for analysis were cut before, during,
or after the dyeing operation. Those taken after the
completion of dyeing were washed four times to remove
any unfixed dyes using the following protocol: 60 s at
20 °C, 30 s at 60 °C, 90 s at 90 °C, and 60 s at 40 °C
using stirred water at a 100:1 liquor-to-fabric ratio.
These conditions provided a reasonable simulation of
those encountered in the finishing mill where a continu-
ous washing unit was used. After the final washing all
dyed samples were air-dried.
For comparison purposes, the cotton was also dyed
using a semi-continuous dyeing operation (cold pad-
batch) either in the laboratory or in the finishing plant.
This involved impregnating the fabric with the reactive
dye solution, containing 20 g/L Na2CO3 and 20 g/L NaCl,
and storing the fabric, wrapped in plastic film to avoid
evaporation, for 24 h at room temperature and finally
washing and drying.
Success in continuous dyeing on the pilot scale led to
full-scale continuous dyeing trials in the finishing mill.
The latter were only carried out for the burgundy and
forest green shades. This involved dyeing of 400 m rolls
of the same cotton/polyester fabrics, both of which gave
a dye solution pickup of 58%. The impregnated fabric
passed through the infrared oven and then through a
conventional gas-fired hot air drying frame at about 19-
20 m/min. The infrared unit consisted of 6 banks each
with 8 tubular emitters (7 kW each). The fabric tem-
perature at the exit to the infrared oven, registered with
a manual pyrometer, was 120-140 °C, with most
variations across the fabric width. The motion of the
fabric made precise temperature measurements dif-
ficult. The dyed fabric was washed at the mill in an
eight-box continuous washing unit, numerous samples
being cut along the 400 m length before and after
washing.
All of the dyes used in the project have been used in
cold pad-batch dyeing and have the low to moderate
substantivity required by this process. The pad bath
solution was always at ambient temperature but, unlike
that used in cold pad-batch dyeing, contained no added
salt. Bath solution replacement times were about 14 and
16 min for pilot- and industrial-scale continuous dyeing
trials, respectively, so the processes never attained a
3956 Ind. Eng. Chem. Res., Vol. 44, No. 11, 2005
true equilibrium. Thus, neither type of trial would reach
a true equilibrium in the pad bath but any tailing
caused by dye substantivity would have been visible
over the 2-3 bath replacements involved in the overall
trials.
Dye Fixation Yields. Measurements of the reflec-
tance spectra of the dyeings (380-700 nm with a 10 nm
wavelength interval) were performed using a Diano
Match Scan II double-beam recording spectrophotom-
eter. This allowed calculation of the absorption spectra
of the dyeings (Kubelka-Munk K/S values as a function
of wavelength) and the CIELAB color coordinates for
CIE D65 Illuminant and the CIE 1964 supplementary
standard observer.4 In almost all cases, measurement
of the CIELAB color difference was with respect to the
appropriate commercial product obtained by jet dyeing
of the polyester and subsequent cold pad-batch dyeing
of the cotton, using identical recipes to those given in
this paper.
Because a mixture of reactive dyes was used, and
because the polyester component was already colored
in two of the cases, the following equation was used to
evaluate the degree of reactive dye fixation,
700 700
(∑
380
K/S(λ))W - (∑K/S(λ))P
380
% fixation ) × 100
700 700
( ∑ K/S(λ))U - (∑K/S(λ))P
380 380
where the subscripts W, U, and P refer to dry samples
of the washed dyeing, the unwashed dyeing, and the
dyed polyester of the initial fabric, respectively. For
determining the dye fixation on fabrics of 100% cotton,
the summations for the polyester component were
ignored. This is only an approximate measure and its
validity is dependent upon the absence of ring-dyed
yarns that would produce a stronger absorption of light
by the fabric.5,6 However, fixation yields for the reactive
dyes were also measured by extracting the unfixed dyes
from the fabric before and after heating and determi-
nation of the concentrations of the solutions and the
amounts of dye was done by spectrophotometry.1,2 The
fixation yields determined by extraction were within 2%
of those obtained using the above equation.
Dyeing Quality Evaluation. The degree of dye
bleeding during subsequent washing of the final dyed
samples from the infrared process was compared to that
from samples dyed by the cold pad-batch procedure in
the laboratory. Samples of the final dyeings (5.00 g)
were washed at 50 °C for 30 min in a dilute aqueous
detergent solution (50 mL of 0.5 mL/L of Sandoclean
PCL (Sandoz)) and the absorption spectrum of the
washing solution determined (380-700 nm with a 10
nm wavelength interval). The degree of unfixed dye
desorption was evaluated by summation of the absorb-
ance values for the 33 wavelengths. In addition, the
CIELAB color differences4 between the initial and tested
samples were measured.
Samples dyed using the thermal process and ap-
propriate comparison standards, dyed by a cold pad-
batch procedure, were inclined at 45° to the horizontal
and exposed to daylight under glass with half of each
sample covered to prevent fading. The sum of the K/S
values at 33 wavelengths was recorded each week and
the color loss of the dyed fabric compared to that of the
Table 2. Dye Fixation Yields for the Navy Blue Dyeing of
100% Cotton with Solutions Containing Various Alkalis
at Different Concentrations
dye fixation yields %
type and concentration of alkali
temp at the 20 g/L 1.0 g/L 20 g/L Na2CO3 5.0 g/L
IR oven exit, °C Na2CO3 NaOH 2.5 g/L NaOH NaOH
90 66.7 77.2 80.1 88.6
105 76.8 81.7 87.9 92.2
120 81.7 83.8 93.6 96.5
unexposed half of the sample. Despite the obvious
variations in daylight intensity, this comparison of
identically exposed samples provided information on any
effect of the thermal dyeing process on the light fastness
of the dyeings.
Finally, because a high-energy infrared heating pro-
cess involves possible thermal damage to both the cotton
and polyester fibers, the handle of the fabric was
evaluated manually by comparing it with the handle of
standard fabrics dyed by the cold pad-batch procedure.
Results
Preliminary Trials. The initial work involved opti-
mizing both the physical and chemical variables used
in the thermal dyeing operation so as to maximize the
reactive dye fixation (maximum K/S values). The key
physical operational variables were the fabric speed (2.3
m/min) that determined the residence time in the
infrared oven (36 s), the voltage supplied to the electri-
cally heated tubular infrared sources (around 400 V),
and the length of fabric in the hot air oven operating at
150 °C (2.3 m). The only important chemical variable
was the strength and concentration of the alkali added
to the reactive dye solution just prior to impregnation.
This phase of the work, for each of the recipes, quickly
confirmed what had been established previously.1,2
Optimum fixation required a relatively high concentra-
tion of a strong alkali (5 g/L NaOH) in the dye bath.
This concentration is a compromise between maximizing
activation of the cotton toward reaction with the dyes
and minimizing hydrolysis of the reactive groups of the
dyes during their residence in the dye bath. In addition,
high levels of dye fixation required heating the fabric
in the infrared oven so that drying was complete and
the fabric temperature increased to 110 °C for the
cotton/polyester and cotton fabrics, respectively. Heating
to higher exit temperatures than these caused increased
fabric stiffness and a deterioration of the fabric handle.
Table 2 shows data for the navy blue dyeing of the 100%
cotton fabric illustrating the effects of alkali type and
concentration, and of heating to higher temperatures,
on the dye fixation yields.
Similarly, for the burgundy dyeing on cotton/polyester
using dye baths containing 20 g/L NaHCO3, 20 g/L
Na2CO3, 1.0 g/L NaOH, or 5.0 g/L NaOH, and with a
fabric temperature at the infrared oven exit of 110 °C,
the dye fixation yields were 10, 65, 62, and 72%,
respectively. For the burgundy dyeing using 5.0 g/L
NaOH in the dye bath, the CIELAB color difference was
1.85 (slightly yellower) with respect to the production
standard for this shade obtained from the mill. This was
a most satisfactory result. This dyeing was barely
influenced by the presence of salt in the dye bath, the
dye fixation yield only increasing from 72 to 75% with
an addition of 50.0 g/L of anhydrous Na2SO4. The

Table 3. Continuous Dyeing Trials on the Pilot and
Industrial Scale
burgundy forest green
navy blue on on cotton/ on cotton/
100% cotton polyester polyester
Pilot-Scale Dyeings
dye fixation yield % 94.1 ( 0.8 72.0 ( 3.5 74.0 ( 5.0
integrated K/S values 302.1 ( 1.6 295.8 ( 5.4 293.4 ( 6.0
CIELAB color 6.05 ( 0.11 a 2.87 ( 0.38 2.84 ( 0.49
difference 1.60 ( 0.32a
Mill Dyeings
dye fixation yield % 72.0 ( 1.4 65.7 ( 3.5
integrated K/S values 293.7 ( 4.06 305.3 ( 5.95
CIELAB color 2.00 ( 0.05a 2.19 ( 0.20
difference
a Measured with respect to a sample dyed in the laboratory by
the cold pad-batch process.
reactive dyes in the burgundy recipe are less reactive
than those in the navy blue recipe.
The high concentration of NaOH required to obtain
maximum dye fixation was of concern because the pH
value of the bath was high enough to possibly cause
rapid hydrolysis of the reactive groups of the dyes. Trials
carried out over a period of time with the same alkaline
dye solution (5.0 g/L NaOH) showed that there was no
significant loss of color strength of any of the dyeings
provided that the solution was not used for a period
exceeding 20 min.
One striking result of the optimization study was that
the hot air oven played almost no role in dye fixation.
We had initially assumed that 40-45 s of infrared
heating would not be sufficient to drive the fixation to
its optimum value and therefore chose to follow the
infrared heating with hot air at a safe, constant high
temperature. The optimum dye fixation depended only
on how high a temperature the cotton fabric reached in
the infrared oven. Even for dyeings where the fixation
yield at the infrared oven exit was lower, as when using
20 g/L Na2CO3 in the dye bath, further heating for 1
min at 150 °C in the hot air oven did not increase the
yield by more than about 2%.
Continuous Dyeing Trials on a Pilot and Indus-
trial Scale. For the pilot-scale and industrial-scale
continuous dyeing trials, we measured the dye fixation
yield, the integrated K/S values determined from the
reflection spectrum, and the CIELAB color difference
with respect to a cold pad-batch dyeing from the
finishing mill, unless otherwise indicated. Measure-
ments were taken at frequent intervals along the length
of dyed fabric, and also across the fabric width for
dyeings conducted at the mill. The results in Table 3
give the average values and the standard deviations of
each measured quantity over all the samples of a
particular dyeing. They show that the process was well-
controlled and that, in all cases, any variations of the
color difference along the fabric were negligible, a
conclusion confirmed by detailed visual inspection by
our industrial partner. Note that the standard devia-
tions of the CIELAB color differences are all below 0.5.
Despite some temperature variations across the fabric
width at the exit of the infrared dryer at the mill, there
was no measurable or visible color variations across the
fabric width. The CIELAB color differences were deter-
mined with respect to the appropriate industrial dyeings
provided by our partner that were prepared by jet
pressure dyeing of the polyester with disperse dyes
followed by cold pad-batch dyeing of the cotton with
Ind. Eng. Chem. Res., Vol. 44, No. 11, 2005 3957
reactive dyes, using exactly the same recipes as given
in this paper. For the navy blue dyeing, the average
CIELAB color difference with respect to the laboratory
cold pad-batch dyeing was quite high because of the
much lower dye fixation in the latter case (68%). The
dyeings on the pilot scale in the laboratory and those
at the mill were carried out under different conditions.
The solution pickup at the mill (58%) was lower than
that in the laboratory (72%), but despite this, the dyed
fabrics produced at the mill had colors only slightly
different than those of the standard shades.
Washing and Light Fading Tests. The bleeding of
residual unfixed dyes during subsequent washing and
the light stability of the dyed samples were examined
and compared to those of identically treated samples
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
dyeing obtained by the infrared process, the values of
the integrated absorbance values for the washing solu-
tions were 7.30 ( 0.97, 2.61 ( 0.06, and 2.74 ( 0.27,
respectively. Both the sample dyed using infrared
radiation and the laboratory-scale cold-pad batch dyeing
contained slightly more than a third of the amount of
unfixed dyes as the sample produced by our industrial
partner. They also had much smaller variations in the
amounts of residual unfixed dyes among the samples.
For the navy blue shade on the 100% cotton fabric dyed
using the infrared procedure or by a cold pad-batch
method, the values of the integrated absorbance values
were 7.2 and 28.9 (single test of each sample). The very
high value for the cold pad-batch sample is a conse-
quence of the much lower fixation yield for this dyeing
(62%) and the inadequacy of the post-dyeing washing
procedure in removing the large amounts of residual
unfixed dyes in this case. Color measurements and
visual inspections on the washed and unwashed samples
showed that the washing test did not result in any color
difference.
Exposure to daylight over periods of 3-6 weeks
showed no decrease in the integrated K/S values for
either infrared or cold pad-batch dyeings. The thermal
process thus had no influence on the color stability of
the dyed fabrics to light exposure.
At each stage in the project, fabric samples were
examined to evaluate their handle. Provided that the
maximum temperatures at the infrared oven exit were
not exceeded, the dyeings produced by the thermal
process were of identical handle to those produced by
the cold pad-batch method.
Conclusion
The use of infrared radiation for drying and heating
fabrics containing cotton and impregnated with a strongly
alkaline solution of reactive dyes gave effective fixation
and less residual unfixed dye in the final fabric. The
thermal continuous dyeing process was well-controlled,
did not result in end-to-end or side-to-side color varia-
tions, and had no influence on color fading in daylight.
The absence of electrolyte and urea from the reactive
dye solution gave washing liquors with a much reduced
pollution load.
Acknowledgment
This project was funded by a Co-operative R&D grant
from the University-Industry program of the Natural
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
also gratefully acknowledge the collaboration of the
Bureau de Liaison Entreprise-Université de Sherbrooke.
Literature Cited
(1) Broadbent, A. D.; Thérien, N.; Zhao, Y. Effects of Process
Variables on the Fixation of Reactive Dyes to Cotton Using
Infrared Radiation. Ind. Eng. Chem. Res. 1995, 34, 943.
(2) Broadbent, A. D.; Thérien, N.; Zhao, Y. Comparison of
Thermal Fixation of Reactive Dyes on Cotton Using Infrared
Radiation or Hot Air. Ind. Eng. Chem. Res. 1998, 37, 1781.
(3) Broadbent, A. D. Basic Principles of Textile Coloration;
Society of Dyers and Colourists: Bradford, UK, 2001.
(4) McDonald, R. Colour Physics for Industry, 2nd ed.; Society
of Dyers and Colourists: Bradford, UK, 1997.
(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.
(6) Motamedian, F.; Broadbent, A. D. Modeling the Influence
of Dye Distribution on the Perceived Color Depth of a Filament
Array. Textile Res. J. 2003, 73, 124.
Received for review December 6, 2004
Revised manuscript received March 30, 2005
Accepted March 30, 2005
IE040288R