Laundry Starch

Stefan Poowiski
Technical University of d
Department of Physical Chemistry of Polymers
ul. eromskiego 116, 90 543 d, Poland
Stiffening Agents Made from

Poly(Itaconic Acid)
Abstract
As a result of the matrix polymerisation of itaconic acid, a product was obtained that
was then used as a stiffener for cotton woven fabrics. It has been found that such fabrics impregnated with poly(itaconic acid) show considerable stiffness and have an
attractive sateen handle. The stiffening effect is not stable, and declines during an
intensive washing process.
Key words: stiffening agents, cotton fabrics, poly(itaconic acid).
reached after about 150 h at a temperature
of 60C [5], and after 720 h at 20C.
n Introduction
Nearly a hundred years ago (in 1908),
Eschalier proposed an improvement of
the properties of cellulose textiles by
cross-linking with formaldehyde. Since
then, numerous preparations and textile
treatment methods have been used to
improve fabric properties [1]. Various
technologies and agents have been developed for specific finishes. Depending on
the properties desired, filling, stiffening,
weighting, lustering, softening, hygroscopic and other agents are available.
In the case of stiffening agents, in addition to starch, the most commonly used
compounds include urea-formaldehyde
or melamine-formaldehyde resins, as
well as cross-linking agents such as
N,N-dimethyurea, derivatives of cyclic
amines and epichlorohydrin [2]. Some
of these compounds, when applied onto
fibres and during the use of those fabrics,
emit highly toxic substances, for instance
carcinogenic formaldehyde. Therefore,
intensive research is being carried out
to replace those toxic products, especially formaldehyde resins, with other
compounds more suitable to impart the
appropriate properties to woven fabrics.
Recently, poly(itaconic acid) and copolymers of maleic acid have been proposed
as cross-linking agents for cellulose to
increase fabric stiffness [3,4].
Both maleic and itaconic acids polymerise with great difficulty. In a conventional
polymerisation of itaconic acid initiated
with AIBN, a 50% yield of the process is
84
A characteristic feature of matrix polymerisation as a relatively new method of

radical polymerisation is that the polymeric matrix used in the system accelerates this process [6]. This method has not
as yet been used to polymerise itaconic
acid. On the other hand, numerous studies have dealt with the matrix polymerisation of methacrylic or acrylic acid [7,
8], using poly(ethylene glycol), among
other things, as a matrix. As is already
known, polyacids form complexes with
polyglycols, and so the polymerisation
results in a complex of polyacid with
polyglycol.
The aim of the present study was to
prepare poly(itaconic acid) by matrix
polymerisation, and to use the resultant
product for finishing cotton fabrics to
increase their stiffness.
n Experimental
Synthesis of poly(itaconic acid)
Materials used
Itaconic acid (Koch-Light Lab. Ltd, England); ammonium persulphate (pure for
analysis - FOCh, Poland); AIBN crystallised from ethanol; poly(ethylene glycol)
300 (Loba, Vienna, Austria) (PEG 300);
poly(ethylene glycol) 6000 (Fluka Ag,
Switzerland) (PEG 6000).
Poly(itaconic acid) was synthesised in
accordance with the following procedures:
A. 25 g of itaconic acid was dissolved in
150 ml of PEG 300. After dissolution
(at about 50C), 0.5 g of AIBN was
added and left at room temperature for
48 h. Anhydrous acetone was added
to a 2 ml sample of the solution to
precipitate the polymer, which was
then filtered off, dried and weighed,
obtaining 0.1185 g of PIA, i.e. about

41.5% of the polymer. The whole was
dissolved in 500 ml of distilled water
and used for fabric padding.
B. 25 g of itaconic acid and 8.46 g of
PEG 6000 was dissolved in 100 ml
of dioxane, and after dissolution 0.5 g
of AIBN was added. The solution was
heated for 8 h at a temperature of 50C
and then left for 48 h at room temperature. Anhydrous acetone was added to
a 1 ml sample to precipitate the polymer, obtaining 0.1383 g of PIA, i.e.
73.57%. The whole was dissolved in
500 ml of distilled water and used for
fabric padding.
C. 25 g of itaconic acid and 8.5 g of PEG
6000 was dissolved in 56 ml of water
and 1 ml of ammonium persulphate
solution (1g/50 ml water) was added
and left for 48 h at room temperature.
Then, another 1 ml of ammonium
persulphate solution was added. After
24 h, 5 ml of ammonium persulphate
solution was added and heated for 5 h
at 50C. The solution was completely
homogeneous. After another 24 h, anhydrous acetone was added to a 1 ml
sample in order to precipitate about
96% of PIA.
D. 25 g of itaconic acid and 8.5 g of PEG
6000 was dissolved in denaturated
ethyl alcohol and made up to 100 ml.
After dissolution (by warming), 0.5
g of AIBN was added and the whole
was heated at 70C for 13 h. The yield
was about 10%.
E. 25 g of itaconic acid and 8.5 g of
PEG 6000 was dissolved in 40 ml
of water, and after dissolution 1 g of
ammonium persulphate was added.
The whole was heated at 70C for 6 h
and diluted with water to 100 ml. The
yield was 77.6%.
Based on the above syntheses, it was
found that the polymerisation of itaconic
acid in the presence of ethanol (sample
D) takes place with a very low yield, and
FIBRES & TEXTILES in Eastern Europe April / June 2004, Vol. 12, No. 2 (46)
only samples A, B, C and E were selected

for further examination. At room temperature, the process (synthesis C) proceeds
very slowly and requires an additional
quantity of the initiator. Despite the high
yield, the process is inconvenient from a
practical point of view.
The best conditions for synthesis seem to
exist in procedure E because of the rather
short time of the reaction and the satisfactory yield. In addition to poly(itaconic
acid), the product obtained also contained poly(ethylene glycol) which was
not removed from the mixture used for
padding.
Padding procedure
The padding of cotton woven fabric with
a surface weight of 1.4 g/dcm2 was carried out in a laboratory Ernest Benz padding machine with a roller load of 45 kG
per 1 cm of roller length, at a speed of 2
m/min. Each fabric sample was padded
three times, and then dried in an Ernest
Benz drier at a speed of 0.5 m/min at
a temperature of 100C, followed by
reheating (setting) at the same rate at
150C.
Hand washing with soap
Fabric samples were immersed in a
beaker containing 500 ml of water, 10 g
of Na2CO3 and 5 g of soap at 60C for 10
min. During the next 30 min, the whole
content was sporadically stirred. Then,
the samples were rinsed four times with
distilled water and dried.
Washing in a washing machine
Table 1. Flexural rigidity, mN.m.

Sample
Before washing
After hand washing

with soap
After washing
in washing machine
Treated with CaCl2

and washed with soap
0.019
0.007
0.036
0.022
0.010
0.165
0.026
0.006
0.452
0.050
0.009
0.201
0.413
0.053
0.009
0.287
Table 2. Results of measurements of opening angle.

Sample Before washing,
deg.
After hand washing

After washing
Treated with CaCl2
with soap,
in washing machine, and washed with soap,
deg.
deg.
deg.
30.3
43.0
40.0
37.7
45.2
30.4
37.8
44.4
23.8
35.9
47.8
31.2
20.3
39.4
49.4
25.9
G = mF . c3 . g . 10-9, mN . m
where:
mF - the fabric surface weight,
g - the acceleration of gravity
(9.806 m/s),
c - the average bending length.
The results of calculation are listed in
Table 1, which shows that a very high
rigidity was obtained when using concentrated solutions of C and E products;
on the other hand, considerably lower
figures are obtained when compounds A
and B were used. The rigidity is considerably decreased after washing with soap,
and effectively declines after intensive
washing in a washing machine. The samples additionally treated with calcium
salt maintain a higher rigidity even after
washing with soap.
Fabric samples were washed in a domestic washing machine at a temperature of

40C for 30 min, using Vizir washing
powder (10g /L), and then rinsed three
times with water. Samples C and E were
additionally treated with calcium salt solution. They were immersed for 10 min
in a solution containing 60 g/L of CaCl2,
rinsed in distilled water and dried.
Crease resistance
The crease resistance of the woven fabrics under examination was determined
according to Polish standard PN-63/P04737. The results were calculated in
the form of an average angle of sample
arms opening in per cent in relation to
180. The results obtained are given in
Table 2.
Determination of flexural rigidity
As is seen from Table 2, the fabric

samples impregnated with a diluted solution of PIA (A and B) show a rather
insignificant stiffness that declines after
washing. On the other hand, the samples
impregnated with concentrated solutions
(C and E) show considerable stiffness
as well as an attractive sateen handle.
This stiffness is considerably decreased
after washing in a soap solution, and totally disappears after washing in a washing machine. The stiffness effect can be
The unitary flexural rigidity was determined by the constant deflection angle
method [9]. The measurement consists
in finding the length of a sample strip (L)
hanging down to contact a surface positioned at an angle of 4030. The average
bending length c=L/2 calculated from 5
measurements was used to calculate the
unitary flexural rigidity G according to
the following formula:
FIBRES & TEXTILES in Eastern Europe April / June 2004, Vol. 12, No. 2 (46)
made slightly more resistant to washing

with soap by additional treatment with a
calcium salt solution.
n Conclusions
Polymerisation of itaconic acid in
the presence of poly(ethylene glycol)
proceeds faster than polymerisation in
conventional conditions. The product
obtained can be used as a stiffening
agent, similar to a new type of proposed
cross-linked agents for cellulose which
does not emit toxic substances. The stiffness effect is rather high, but the effect
decreases after washing. The addition of
divalent ions slightly improves the effect.
However, at present the method can be
used only for products not intended to be
washed.
References
1. L. Jackiewicz-Kozanecka, Chemiczne
podstawy apretur szlachetnych, p. 251,
WNT Warszawa, 1985.
2. Poradnik Inyniera - Wkiennictwo T. 2,
p. 156, WNT Warszawa 1988.
3. C.Q. Yang, X. Wang, Y. Lu, J. Appl.
Polym. Sci. &%, 327 (2000).
4. Z. Mao, C.Q. Wang, Appl. Polym Sci., 79,
319 (2001).
5. D. Braun, I.A. Aziz EL Sayed, Macromol.
Chem., 96, 100 (1966).
6. S. Poowiski, Prog. Polym. Sci., 27, 537
(2002).
7. S. Poowiski, J. Polym. Sci., Polym.
Chem. Ed., 22, 2887 (1984).
8. S. Poowiski, Europ. Polym J., 19, 679
(1983).
9. W. Konecki, Metrologia Surowcw i Wyrobw Wkienniczych; ed.: Technical
University of d, P. 2, p. 54.
Received 24.08.2003
Reviewed 07.04.2004
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Stefan Poowiski

Stiffening Agents Made from

A characteristic feature of matrix polymerisation as a relatively new method of

obtaining 0.1185 g of PIA, i.e. about

only samples A, B, C and E were selected

Table 1. Flexural rigidity, mN.m.

After hand washing

Treated with CaCl2

Table 2. Results of measurements of opening angle.

After hand washing

Fabric samples were washed in a domestic washing machine at a temperature of

Determination of flexural rigidity

As is seen from Table 2, the fabric

made slightly more resistant to washing

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