RJTA Vol. 10 No.

1 2006

The Durable Press Finishing of Silk Fabrics by Using

1,2,3,4-Butanetetracarboxylic Acid
Zhuohong Yang1, 2 and Jinlian Hu2
1
College of Science, South China Agriculture University, Guangzhou, P. R. China
2
Institute of Textiles and Clothing, The Hong Kong Polytechnic University,
Hung Hom, Kowloon, Hong Kong

ABSTRACT

In this paper, the nonformaldehyde agent 1,2,3,4-butanetetracarboxylic acid was used for
durable press finishing of silk fabric. To optimize the finishing, the effects of the amount of
sodium hypophosphite, 1,2,3,4-butanetetracarboxylic acid and citric acid, curing temperature
and curing time were examined. It was found that the wet wrinkle recovery angle had an
obvious improvement from 179° to 273°, and that the finishing had a very small effect to the
breaking strength.

Keywords: Silk, Durable Press Finishing, Butanetetracarboxylic Acid

1. Introduction prepared according to the literature (Toshihiro et

To the present, 1,2,3,4-butanetetracarboxylic acid
(BTCA) was found to be the most effective
nonformaldehyde durable press finishing reagent
[1-4]. It has been considered that the
polycarboxylic acid reacted with cotton to form
crosslinks through ester linkages between the
cellulose and the agent (Schramm et al., 1998; Xu
et al., 2001). Recently, much research work has
been done on the Durable Press (DP) finishing of
cotton (Blanchard and Graves, 2002; Zhou et al.,
2002; Yang et al., 2001; Yang, 2001). While silk
as very exalted fabrics originated from China and
has similar structure compared with cotton
because both of which have many hydroxy
groups, little attention has been given. Since the
DP finishing is also very important to silk, the
BTCA was chosen for the DP finishing of silk
fabrics in this paper. Moreover, the relation
among each finishing variable, the amount of
sodium hypophosphite (SHP), BTCA and Citric
acid (CA), curing temperature, curing time and
the finished fabric’s properties, including
breaking strength and wet wrinkle recovery angle
were also investigated.
2. Experimental
2.1 Materials
al.). Citric acid, SHP, triethanolamine (TEA) and
Boric acid were purchased from Beijing Chemical
Company and were analytical grade. Softener
(SG-6) and permeate agent (JFC) were purchased
from Jiangsu Hai’an Chemistry Company.
2.2 Silk Durable Press Treatment
The silk was immersed in the aqueous treating
solution containing BTCA, CA, SHP and other
reagents of different amounts. The fabric was then
passed through squeeze rolls and immersed in the
treating solution, and was then passed through
squeeze rolls again to give a specified wet pick-up
of ca.100%. The fabric was pre-dried at 80°C, and
cured in a second oven for 2 minutes at 170°C
~175°C.
2.3 Testing Methods
Mechanical properties were measured on an
Instron tester (model 3410) at a 50 mm gauge
length and with a crosshead speed of 100
mm/min. The width of the sample was 15 mm. As
the silk has a good dry wrinkle recovery angle,
only the wet wrinkle recovery angle was
measured in this paper. Standard methods were
used to measure the wet wrinkle recovery angle
(AATCC 66-1996).

Undyed 100% silk was purchased from WuXi

Silk Factory. 1,2,3,4-butanecarboxylic acid was
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RJTA Vol. 10 No. 1 2006

3. Results and Discussion In the DP finishing of cotton with BTCA, SHP is

a very important factor as a catalyst. In addition,
3.1 The Effect of BTCA Amount to the DP the amount of SHP is even more critical to the
Finishing finishing. Therefore, we also investigated the
effect of the SHP amount and the results are
Table 1. The relation of BTCA amount with wet shown in Table 2. From the results, we found that
WRA and breaking strength retention the wet WRA was markedly influenced by the
of silk fabric amount of SHP. When the fabric was treated with
4% SHP and 2% TEA, the wet WRA greater than
BTCA Wet Breaking Strength 270° was obtained with 85.8% breaking strength
(%) WRA Retention (%) reserved.
3 244.7° 103.6
4 248.0° 97.0 3.3 The Choice of Curing Temperature and
6 255.7° 85.3 Time
7 255.7° 101.5
8 236.0° 107.0 It is reasonable to try to decrease the curing time
Untreated 179.0° 100 by using a relatively high temperature. However,
sample higher temperature leads to the breaking-down of
Note. The durable press finishing also contained the fabric polymer and the decrease of strength,
3.0% SHP, 2.0% triethanolamine, 1.0% SG-6, 0.5% which can be seen from the results in Table 3.
JFC, 0.5% Boric acid, followed by predrying at When the finished fabric was cured at 170°C for 2
80°C for 5 minutes, curing in a second oven at minutes, the best finishing result was obtained
170°C for 2 minutes. with 273° of wet WRA and 87.5% of breaking
strength retention.
At first, the effect of BTCA amount was
investigated and the results are summarized in Table 3. The DP finishing with different
Table 1. We found that the BTCA amount had an curing temperature and time
obvious influence on the properties of finished
fabrics: With the increase of BTCA to 7%, the T. Time Wet Breaking Strength
(°C) (min) WRA Retention (%)
wet WRA increased up to 255.7°; while the use of
170 1.5 253.3° 88.3
8% only led to the wet WRA of 236°. We
170 2.0 273.0° 87.5
consider that the elasticity of fabric would
170 3.0 255.7° 85.3
decrease when the fabric had an exceeded
175 1.5 264.6° 105.6
crosslinking with BTCA, which led to the
175 2.0 254.0° 95.5
decrease of wet WRA. With the breaking strength
175 3.0 258.7° 71.6
considered, 7% of BTCA seemed to have the best
result of WRA for the experiments reported here. Note. The durable press finishing also contained
7.0% BTCA, 4.0% SHP, 2.0% triethanolamine,
3.2 The Effect of the Amount of SHP to the 1.0% SG-6, 0.5% JFC, 0.5% Boric acid, followed
DP Finishing by predrying at 80°C for 5 minutes.

Table 2. The effect of the amount of SHP 3.4 The Mixed Finishing of BTCA with CA

SHP TEA Wet Breaking Strength Table 4. The wet WRA and breaking strength
(%) (%) WRA Retention (%) retention of the fabric treated by BTCA
2 2 227.3° 87.0 mixed with CA.
3 2 255.7° 85.3
BTCA CA Wet Breaking Strength
4 2 270.4° 85.8
(%) (%) WRA Retention (%)
5 2 264.6° 87.4
4 3 229.7° 110.7
3 3 254.7° 93.2
4.5 2.5 238.4° 105.7
Note. The durable press finishing also contained
5 2 242.7° 96.4
7.0% BTCA, 1.0% SG-6, 0.5% JFC, 0.5% Boric
acid, followed by predrying at 80°C for 5 minutes, 5.5 1.5 222.6° 103.1
curing in a second oven at 170°C for 2 minutes. 6 1 249.0° 87.6
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RJTA Vol. 10 No. 1 2006
Note. The durable press finishing also contained
4.0% SHP, 2.0% triethanolamine, 1.0% SG-6, 0.5%
JFC, 0.5% Boric acid, followed by predrying at
80°C for 5 minutes, curing in a second oven at
170°C for 2 minutes.
Although BTCA has a good finishing result, the
high cost of BTCA is an obstacle to mills’
decisions to use BTCA. As mixed polycarboxylic
acids has been an interesting research area for
decreasing the expense of using BTCA by
reducing the required amount of BTCA in DP
finishing, the finishing of BTCA mixed with CA
was also investigated in this paper. The results
are shown in Table 4. It is evident that the wet
WRA decreased when smaller amount of BTCA
mixed with CA was used in the DP finishing,
although the breaking strength retention did not
vary too much. As CA was considered to have
lower activity than BTCA (Xu and Shyr, 2000), in
the same condition, CA could not have a complete
crosslink with silk fabrics. To obtain better
finishing results with CA, other methods should
be considered.
3.5 FTIR Analysis
FTIR analysis is a very important analysis method
in the DP finishing (Yang, 2001). In this paper,
the FTIR was also used to study the crosslink of
BTCA with silk fabrics. Compared with the FTIR
of silk structure, the finished fabric appeared an
obvious absorption at 1700~1750 cm-1, which was
usually considered the feature of ester and could
be proved that BTCA has successfully crosslinked
with the silk fabric.
4. Conclusion
This paper reported the durable press finishing of
silk fabrics with BTCA. The effect of the
finishing variables, SHP, BTCA and CA amounts,
curing temperature and curing time were
investigated. The results showed that BTCA is a
very effective reagent to the DP finishing of silk
fabrics. The optimized finishing variables were
given and up to 273° of wet WRA was obtained
with 87.5% breaking strength retention reserved.
In addition, the effects of different processing
conditions on DP of silk fabrics have been
studied.
48
REFERENCE
[1] Blanchard, E.J. & Graves, E.E. 2002,
‘Polycarboxylic acids for flame resistant
cotton/polyester carpeting’, Textile Research
Journal, vol. 72, no. 1, pp. 39-43.
[2] Choi, H.M., Welch, C.M. & Morris, N. 1993,
‘Non-phosphorus catalysts of formaldehyde-
free DP finishing of cotton with 1,2,3,4-
butanetetracarboxylic acid. I. Aromatic
N-heterocyclic Compounds’, Textile Research
Journal, vol. 63, no. 11, pp. 650-657.
[3] Hyung, M.C. & Welch, C.M. 1994,
‘Saturated and unsaturated carboxylic acid
salts as curing additives for BTCA treatment
of cotton’, Textile-Chemist-&-Colorist, vol.
26, no. 6, pp. 23-27.
[4] Schramm, C., Rinderer, B. & Bobleter, O.
1998, ‘Quantitative determination of BTCA
bound to cellulosic material by means of
isocratic HPLC’, Textile Research Journal,
vol. 68, no. 11, pp. 821-827.
[5] Toshihiro, T., Yoshiro, F., Hydeo, Y. &
Noriyuki, H., ‘Preparation of 1,2,3,4-butan-
etetracarboxylic Acid’, JP Patent 53-060579.
[6] Xu, W.L. & Shyr, T.W. 2000, ‘Durable press
finishing of cotton fabrics by polycarboxylic
acids after graft copolymerization with
hydroxyethyl methacrylate’, Textile Research
Journal, vol. 70, no. 1, pp. 8-10.
[7] Xu, W.L., Cui, W.G., Li, W.B. & Guo, W.Q.
2001, ‘Two-step durable press treatment of
cotton fabric’, Color.Technol, vol. 117,
pp. 352-355.
[8] Yang, C.Q. 2001, ‘FTIR Spectroscopy Study
of Ester Crosslinking of Cotton Cellulose
Catalyzed by Sodium Hypophosphite’, Textile
Research Journal, vol. 71, no. 3, pp. 201-206.
[9] Yang, C.Q., Qian, L. & Lickfield, G.C. 2001,
‘Mechanical strength of durable press finished
cotton fabric part IV: Abrasion resistance’,
Textile Research Journal, vol. 71, no. 6,
pp. 543-548.
[10] Yang, C.Q., Wang, X.L. & Kang, I.S. 1997,
‘Ester crosslinking of cotton fabric by
polymeric carboxylic acids and citric acid’,
Textile Research Journal, vol. 67, no. 5,
pp. 334-342.
[11] Zhou, L.M., Yeung, K.W. & Yuen, C.W.M.
2002, ‘Treating cotton fabric with cellulase
and BTCA in one bath’, AATAA-Review,
vol. 2, no. 1, pp. 29-33.