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Temperature–Alkaline Conditions
ABSTRACT: The factors affecting the dyeability of poly- that is, EDTA ⬎ Diaserver威 AD-95 ⬎ Tinoclorite威 CBB
ester-based textiles with disperse dyes in an alkaline me- ⬎ citric acid ⬎ none, as well as kind of the disperse dye; (e)
dium were studied. It was found, for a given set of dyeing direct reuse of the disperse dyebaths, without reconstitution,
conditions, that (a) the appropriate conditions for attaining a in the dyeing of the used substrates was shown to be feasible
higher color yield were 45 min at 130oC with pH 9 using a in a single shade and in the reverse-order dyeings (dark 3
material-to-liquor ratio of 1/10; (b) increasing the Diaser- light); (f) one-bath, one-step exhaust dyeing of polyester/
ver威 AD-95 concentration to 2% ows (based on weight of cotton-knitted fabric using selected disperse reactive dyes
substrate) as well as including triethanolamine to 2% ows in combinations under high-temperature alkaline conditions is
the dyeing formulations bring about a significant improve- feasible; and (g) the color and fastness properties of the
ment in the dye uptake; (c) both a preheat setting from 160 resultant dyeings depend on the type of the used auxiliaries,
to 200oC/30 s and an alkaline weight reduction have a in addition to the nature of disperse/reactive dyes combi-
positive impact on postdyeing with the used disperse dye; nations as well as compatibility with other ingredients. ©
(d) the extent of dye uptake as well as the color strength are 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 3563–3573, 2003
governed by the type of substrate, that is, knitted fabric
⬎ spun yarn ⬎ woven fabric, nature of the dye stabilizer, Key words: blends; dyes; polyester
Methods
Alkali dyeing process
Samples of polyester substrates were dyed at a mate- Figure 1 Dyeing cycle used in the present study.
rial-to-liquor ratio (LR) of 1/10, with a 2% ows (based
on weight of the substrate) commercial disperse dye
solution. The standard dyeing profile is shown in Fig- Dyebath reuse
ure 1.16 Washing-off was carried out according to the
manufacturer’s instructions to remove unfixed dis- The exhausted hot dyebaths were reused to dye a
solved oligomers as well as residual auxiliaries. number of batches of material, without analysis, to
determine the concentrations of residual dyestuffs and
auxiliaries, that is, without reconstitution, keeping the
Heat setting LR fixed to obtain lighter shades for economical and
ecological reasons.
Heat setting of the polyester fabric samples were car-
ried out in a hot-air curing oven in a taut condition for
30 s at 160 –200oC. Disperse/reactive dyeing of polyester/cotton knitted
fabric
The standard dyeing profile is shown in Figure 2.
Weight reduction Washing-off was carried out according to the manu-
Woven fabric samples were treated at 80oC for 30 min facturer’s instructions to remove unfixed and/or hy-
with a liquor ratio of 20:1, including small quantities drolyzed dyes as well as residual salts, fixing agents,
of Dodigen威 226 (0 –1 g/L) as an accelerant, in an and other auxiliaries.
aqueous sodium hydroxide solution (10 g/L). The
treated samples were then rinsed in water to remove
Testing
any residual (alkali, accelerator, as well as hydrolysis
products), neutralized with acetic acid, then thor- The color intensity, expressed as the K/S value, of the
oughly rinsed again with distilled water until the rinse dyed substrate was measured at the wavelength of
water was neutral, and, finally, dried under standard maximum absorbance using an automatic filter spec-
conditions. Weight loss was determined gravimetri- trophotometer and calculated by the Kubelka–Munk
cally.5,6,25 equation26:
EXHAUST DYEING OF POLYESTER-BASED TEXTILES 3565
Figure 2 Dyeing cycle used in the present study (rapid dyeing/one bath). Chemical/auxiliaries: borax (2 g/L); Disperso-
gen威 P (0.5 g/L); Eganal威 PSN (2 g/L); Diaserver威 AD-95 (2% owf, based on weight of fabric), unless otherwise notified; with
a liquor ratio of 10:1, in presence or absence of TEOHA (0.5% owf). Dyestuffs: The disperse/reactive dyes combination (2%
owf), pH 9.
Dyeing time
Figure 4 shows the effect of the dyeing time on the Figure 4 Variation of the K/S values with the dyeing time.
Dyeing bath constituents: Dianix威 Navy Blue AD-G (2%
extent of dye uptake, expressed as the K/S value, of the ows); Diaserver威 AD-95 (2% ows); Eganal威 PSN (2 g/L);
dyed polyester substrates. As is evident, prolonging Dispersogen威 P (0.5 g/L); borax (2 g/L); pH 9; LR, 1/10;
the dyeing duration to 45 min at 130oC brings about a dyeing temperature, 130°C.
EXHAUST DYEING OF POLYESTER-BASED TEXTILES 3567
LR
Figure 5 shows the change in the K/S values as a
function of the LR ranging from 1/10 to 1/30 at 130oC
for 45 min. It is clear that decreasing the LR to 1/10 is
accompanied by a gradual increase in the K/S value
regardless of the used substrate, that is, the lower the
LR, the higher is the dye uptake. The enhancement in
the K/S value of the dyed polyester substrates as the
LR decreases could be attributed to the greater
swellability and accessibility of the polymer structure
along with a greater availability of dye molecules and
active ingredients in the vicinity of the so-called amor-
phous regions of the polyester polymer.
Dyebath pH
It is evident (Fig. 7) that, within the range examined,
increasing the pH to 9 at 130oC for 45 min in the
presence of Diaserver威 AD-95 (2% ows) along with
other additives brings about a noticeable increase in
the K/S values of the dyed samples, then it levels off
with a further increase in pH to 10, reflecting the
favorable impact of a proper dyebath pH on (i) loos-
ening the fiber structure, (ii) releasing and dissolution Figure 7 Variation of the K/S values with the dyebath pH.
Dyeing bath constituents: Dianix威 Navy Blue AD-G (2%
of oligomers, and (iii) enhancing and facilitating easy ows); Diaserver威 AD-95 (2% ows); Eganal威 PSN (2 g/L);
penetration of dye molecules into the polymer struc- Dispersogen威 P (0.5 g/L); borax (2 g/L); LR, 1/10; dyeing at
ture, thereby giving rise to higher dye uptake.13,34 130°C for 45 min.
EXHAUST DYEING OF POLYESTER-BASED TEXTILES 3569
Heat-setting temperature
Figure 9 shows the relationship between the Dianix威
Navy Blue AD-G disperse dye (2% ows) uptake on the
woven and knitted polyester fabrics and heat-setting
temperature. It is evident that, for a given dyeing
condition, increasing the thermosetting temperature
from 160 to 200oC for 30 s gives rise to a gradual
increase in the dye uptake, regardless of the used
substrate, which is a direct consequence of the (i)
formation of larger crystals, (ii) reduction in the chain
molecules’ orientation, as well as (iii) increasing the
free volume available to each crystal. The net effect of
the aforementioned changes in the polymer structure
is a gradual increase in dye uptake with increase in the
heat-setting temperature.28,37
Alkaline weight reduction Figure 9 Variation of the K/S values with the heat-setting
temperature. Dyeing bath constituents: Dianix威 Navy Blue
Figure 10 shows the effect of alkaline hydrolysis of AD-G (2% ows); Diaserver威 AD-95 (2% ows); Eganal威 PSN
polyester woven fabric in the presence and absence of (2 g/L); Dispersogen威 P (0.5 g/L); borax (2 g/L); pH 9; LR,
a quaternary ammonium compound (Dodigen威 226) 1/10; dyeing at 130°C for 45 min; heat-setting time, 30 s.
3570 IBRAHIM ET AL.
TABLE II
Color and Fastness Properties of Polyester Dyeings
CF
Disperse dye Substrate K/S WF (CC) LF d w
TABLE IV
Feasibility of Reusing the Dyebath Without Reconstitution
Polyester substrate Disperse dye K/S K/S1 K/S2
Woven fabric Dianix威 Yellow AD-G (max: 420 nm) 14.977 0.269 0.011
Dianix威 Orange AD-R (max: 440 nm) 12.206 0.366 0.014
Dianix威 Red AD-2B (max: 520 nm) 14.960 0.371 0.015
Dianix威 Rubbin AD-B (max: 540 nm) 16.062 0.503 0.020
Dianix威 Blue AD-R (max: 600 nm) 21.162 0.366 0.014
Dianix威 Navy Blue AD-G (max: 600 nm) 18.001 0.809 0.032
Knitted fabric Dianix威 Yellow AD-G 16.007 0.295 0.012
Dianix威 Red AD-2B 15.980 0.430 0.017
Dianix威 Navy Blue AD-G 23.010 1.038 0.041
Spun yarn Dianix威 Yellow AD-G 15.263 0.148 0.006
Dianix威 Red AD-2B 14.530 0.437 0.017
Dianix威 Navy Blue AD-G 21.750 0.773 0.031
Initial dyebath components: disperse dye (2% ows); Diaserver威 AD-95 (2% ows); Eganal威 PSN (2 g/L); Dispersogen威 P (0.5
g/L); borax (2 g/L); pH 9; LR (1/10); dyeing at 130°C for 45 min. K/S: color strength (before reusing); K/S1: color strength (first
run); K/S2: color strength (second run). Reusing of the dyebath was carried out without reconstitution.
3572 IBRAHIM ET AL.
TABLE V
Color and Fastness Properties of Dyed Samples Using Dianix威 Blue AD-R/Procion威 Saphire HEXL Combination
K/S* CF
Increase in K/S WF
Dye stabilizer Without With (%) (CC) d W LF
3. The K/S values of the resultant dyeings, the per- 6. This dyeing procedure also produces level poly-
cent increase in the K/S values, as well as the ester/cotton dyeings.
fastness properties of these dyeings are deter-
mined by the nature of disperse/reactive combi-
CONCLUSIONS
nation, that is, the molecular weight, chemical
structure, extent of aggregation and agglomera- In this study, trials have been carried out to
tion, extent of solubility, diffusion and penetra-
tion, degree of stability, energy level of the dis- (a) Study factors governing the dyeability of poly-
perse dye, dye affinity, migration power, in addi- ester-based textiles with disperse dyes in an al-
tion to compatibility with each other as well as with kaline medium,
other ingredients in dyeing formulations.27,33,38,42,43 (b) Evaluate the feasibility of the reuse of the dye-
4. Generally speaking, the fastness properties’ rat- baths, as well as
ings of the dyed samples, in the presence of (c) Demonstrate the technical feasibility of dyeing
TEOHA (0.5 ows), are rated quite highly, espe- polyester/cotton blend with disperse/reactive
cially in the case of using Dianix威 Blue AD-R/ dyes at high-temperature alkaline conditions.
Procion威 Saphire HEXL and Dianix威 Yellow AD-
G/Procion威 Flavine HEXL combinations. The results obtained led to the following conclu-
5. Fabrics dyed with a Dianix威 Red AD-2B/Pro- sions:
cion威 Red HE3B combination resulted in a
slightly lower wash and light fastness properties • For a given set of dyeing conditions, dyeing at
ratings. 130oC for 45 min constitutes the optimal condi-
TABLE VI
Color and Fastness Properties of Dyed Samples Using Dianix威 Yellow AD-G/Procion威 Flavine HEXL Combination
K/S* CF
WF
Dye stabilizer Without With Increase in K/S (%) (CC) d w LF
TABLE VII
Color and Fastness Properties of Dyed Samples Using Dianix威 Red AD-2B/Procion威 Red HE3B Combination
K/S* CF
WF
Dye-stabilizer Without With Increase in K/S (%) (CC) d w LF
tions for attaining higher K/S values, regardless of 14. Hussamy, S. In Book of Papers, AATCC 1997 International,
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