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Preparation and characterization of ink formulations based on sod. alginate

and natrosol as thickeners for jet printing on nylon carpet

Article · January 2010

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RJTA Vol. 16 No. 1 2012

Preparation and Characterisation of Ink Formulations for

Jet Printing on Nylon Carpet
H. Abd El-Wahab1, M.M. El-Molla2* and L. Lin3
1
Department of Chemistry, Faculty of Science, Al-azhr University, Egypt, hamada19982000@hotmail.com
2
Textile Research Division, National Research Centre, Dokki, Cairo, Egypt, melmolla@yahoo.com
3
Department of Colour and Polymer Chemistry, School of Chemistry, University of Leeds, Leeds LS2 9JT,
UK, l.lin@leeds.ac.uk

ABSTRACT

Various ink formulations for inkjet printing on nylon66 carpet are prepared by using CI Acid
Red 57, Natrosol and sodium alginate thickeners, ethylene glycol, diethylene glycol, and
isopropanol with auxiliaries. The inks are characterised for their rheological, wetting, and
storage stability properties. They were jetted by using a Printos P16 drop-on-demand jet
print-head onto the nylon66 carpet materials, and the printed images were characterised by
using an Image Xpert system.

The inks that contained the synthetic thickeners at the optimum ratio provide good printing
and imaging properties, such as optical density, drop size, and depth of penetration into the
substrate at pH 4-5. The optimised ink formulation is found to have good storage stability.
The study has focused on ink formulations based on CI Acid Red 57. Ink formulations
based on other colorants could also be studied in order to assess the applicability of the ink
formulation system found for other colorants. The ink formulations developed could find
both uses in industrial scale printing and low cost ink formulations for printing of nylon66
carpets.

Keywords: Ink Formulations, Textile Printing, Nylon Carpet, Inkjet Printing, Thickener

1. Introduction Samah, 2004; Sostar & Sehneider, 2000; Zahran,

Sodium alginate is an anionic polysaccharide that
is composed of 1.4-linked β-D-mannuronic acid
and 1.4-linked α -L-guluronic acid. Sodium
alginate is one of the most important thickening
agents. It is possible to list over 300 known
commercial applications of alginates1 in areas as
widespread as textile printing, paper sizing, and
welding rod extrusion, and in food industries, such
as ice cream, salad dressings, beer foam
stabilization, restructured vegetables and fruits,
jellies, pet foods, etc. ( El-Molla & El-Sayad, 2001,
Whistler et al., 1993).
Mohmoud, & El-Rafie, 2007).
Thickeners are used in textile printing to modulate
the rheological properties of the printing pastes
during application and obtain sharp and clean
drawing patterns by preventing dye migration.
Alginates, guar gum and its derivatives, methyl
and carboxymethyl cellulose, some exudate gums
and xanthan are excellent thickeners for this
application, since they can impart high viscosities
at low concentrations and possess adequate
rheological behaviours (Baranov, Dymnikova, &
ll'in, 2002; Fijan, Sostar- Turk, Lapasin, 2007).

Recently, there has been increasing research on the
preparation of thickeners from polysaccharides
and application of these thickeners in textile
printing (Barba, Montane, Rinaudo, & Farriol,
2002; El-Sherbiny, 2004; Oblosek et al., 2000;
* Corresponding author. Tel.:+ 20 123825747; fax:+ 20 23370931
E-mail address: melmolla@yahoo.com (M.M. El-Molla)
24
Alginates are the most widely used thickeners in
cellulosic fabric printing. (Oblosek et al., 2003).
Water is the best vehicle for jet inks because of its
viscosity, ionic nature, and conductivity. A
water-based ink has key advantages over an
RJTA Vol. 16 No. 1 2012

organic-based ink, as it is less toxic, and does not Scheme I Chemical structure of CI Acid Red 57
denature enzymes; this allows for a one-step dye
printing process which greatly reduces the cost of
production (Crouch, 2005).

The balance of the inkjet ink composition may be

water; at least 80% of the ink composition is water.
Inkjet inks may also include a pigment. Generally,
the amount of pigment ranges from about 2 wt%
to about 6 wt% (Rolly, 2008).
In spite of the superior thickening properties of
kerosene/water emulsions which also contribute
towards a soft hand of the print and good fastness
properties, environmental and economical factors
have compelled the search to replace kerosene
(El-Molla & Schneider, 2006).
Also, thickeners and binders play a paramount role
in pigment printing and rheological properties of
printing pastes during application and the
obtaining of sharp and clean drawing patterns by
preventing dye migration (Zahran et al., 2007;
Baranov et al., 2002; Fijan et al., 2009).
The synthesis and application of thermally stable
dyes for ink-jet printed colour filters was
investigated Kim et al. (2009).
Thickeners
Two thickeners were used in the preparation of
various ink formulations. These were Natrosol
and sodium alginate, which are briefly described
as follows.
Natrosol
The Natrosol used was supplied by Sigma-Aldrich,
UK. Modified hydroxyl ethyl cellulose is a
non-ionic, water-soluble polymer that can thicken
and form films. Its structure is shown in Scheme
II.
Scheme II Structure of Natrosol thickener
(hydroxyethyl cellulose).
[C6H7O2 (OH)x (OC2H5)y [O(CH2CH2O)m
H ]z]n.

The work reported in this paper is based on the

preparation of various modified ink formulations
for inkjet printing on nylon66 carpet materials. A
comparison is made between ink formulations
with and without thickeners, in terms of jetting
properties, storage stability and quality of the
printed images on nylon66 carpet materials, such
as optical density, drop size, and penetration Sodium Alginate
properties.
The sodium alginate used was also supplied by
2. Experimental Sigma-Aldrich, UK. It was designed for the
rheological control of aqueous and water soluble
2.1 Materials resin systems that provide pseudo plastic flow
behaviour. The viscosity increase improves the
Dye sag resistance properties. Its structure is shown in
Scheme III.
The dye used was CI Acid Red 57 dye (Nylosan
Red E-BNL) supplied by Clariant, Switzerland, Scheme III Structure of sodium alginate
with its structure shown in Scheme I.

25
RJTA Vol. 16 No. 1 2012

Auxiliaries mentioned materials were prepared. The

Various other auxiliaries were used to improve the
penetration of the ink, reduce the droplet size on
fibre and regulate viscosity and wetting
characteristics of the inks prepared. These
included diethylene glycol (DEG), ethylene glycol
(EG), glycerol, BYK-800 (an alkoholalkoxylate
antifoam), isopropanol (co-solvent), and acetic
acid (for pH adjustment to pH 4~5), all supplied
by Sigma-Aldrich, UK. In-house made deionised
water was used as the main solvent.
Urea, supplied by Avocado Research Chemicals
Ltd., was used as a swelling agent for the nylon
fibres. Sandogen NH Liquid, an anionic
levelling agent supplied by Clariant, Switzerland,
was employed as a levelling agent to achieve level
dyeing in textured nylon yarns and fabrics.
Polyamide Fabrics and Carpets
Fabrics and carpets made of 100% nylon66 were
obtained from a local supplier.
2.2 Preparation of Ink Formulations
Water-based inks that consist of the above
formulations contained 3% Nylosan Red E-BNL
mixed with either Natrosol or sodium alginate,
various other auxiliaries, and deionised water as
the solvent. Each of the formulations was prepared
by mixing the relevant ingredients under stirring
for 2 hours. The ink formulations were designed
by using Minitab 14 (supplied by Minitab Ltd.,
UK) following the factorial experimental design
principle, in order to evaluate the effects of
different binders on the properties of the inks and
obtain optimised ink formulations. The ink
formulations prepared are shown in Tables 1 and
2.
2.3 Method for Inkjet Printing onto Nylon66
Fabrics and Carpet Materials
The Printos P16 drop-on-demand jet printing
machine was used to print the inks prepared onto
the nylon66 carpet materials. Samples printed
with the prepared inks that contained Acid Red
dye B-NBL and Natrosol and other inks that
contained sodium alginate were first air-dried
followed by steaming at 110°C for 15 min. at an
atmospheric pressure for the fixation of dye onto
the fabrics and carpet materials. These samples
were subsequently subjected to various analyses.

Table 1. Ink formulations containing Natrosol 3% gel

Compositions (%)
Ink sample code
DEG EG IPA Water Natrosol 3%gel Acid red dye
A1 10 5 5 27 0 3
A2 10 5 5 17 10 3
A3 0 5 0 42 0 3
A4 0 5 0 32 10 3
A5 10 0 0 37 0 3
A6 10 0 0 27 10 3
A7 0 0 0 47 0 3
A8 0 0 0 37 10 3
A9 0 0 5 42 0 3
A10 0 0 5 32 10 3
A11 0 5 5 37 0 3
A12 0 5 5 27 10 3
A13 10 5 0 32 0 3
A14 10 5 0 22 10 3
A15 10 0 5 32 0 3
A16 10 0 0 27 10 3
Using Glycerol (G), levelling agent, antifoam, Acetic acid (A.A) to adjust pH , Sodium Chloride
(NaCl), and Urea, as 1.78g ,0.59g, 0.3g, 0.59g, 0.03g, and 2.96g respectively.

26
RJTA Vol. 16 No. 1 2012

Table 2. Ink formulations containing Sod.alginate 2% gel.

Compositions (%)
Ink sample code Sodium alginate
DEG EG IPA Water Acid red dye
Gel. 2%
B1 10 5 5 27 3 0
B2 10 5 5 17 3 10
B3 0 5 0 42 3 0
B4 0 5 0 32 3 10
B5 10 0 0 37 3 0
B6 10 0 0 27 3 10
B7 0 0 0 47 3 0
B8 0 0 0 37 3 10
B9 0 0 5 42 3 0
B10 0 0 5 32 3 10
B11 0 5 5 37 3 0
B12 0 5 5 27 3 10
B13 10 5 0 32 3 0
B14 10 5 0 22 3 10
B15 10 0 5 32 3 0
B16 10 0 0 27 3 10
Using Glycerol (G), levelling agent, antifoam, Acetic acid (A.A) to adjust pH , Sodium Chloride
(NaCl), and Urea, as 1.78g, 0.59g, 0.3g, 0.59g, 0.03g, and 2.96g respectively

3. Methods for the Characterisation of (CCD) cameras and a Power Macintosh G3

Ink Formulations computer, in which the analysis software was
integrated.
3.1 Rheological Analysis
3.4 Optical Density
Rheological properties of the water-based ink
formulations prepared were analysed (at 25°C and The optical density of each printed sample was
different shear rates) by using an RFS II measured by using a GRETAG D183
(Rheometrics CO 1483) fluid spectrometer. densitometer.

3.2 Measurement of Surface Tension 3.5 Drop Size

The surface tension of the inks prepared was
measured by using a torsion balance (Torsion
Balance Supplies, UK). This instrument
determines the force required to detach a platinum
ring from the surface of the ink. The measurement
procedure was repeated six times to obtain an
average value of the detaching force. Before
each measurement, the platinum ring was
thoroughly rinsed in distilled water and flamed
with a Bunsen burner to remove any residues.
The diameter of the printed circles on the surface
of the fabrics/carpet materials was measured by
using a ruler.
3.6 Penetration
The depth (in percentage) of ink penetration into
the printed fabrics/carpet materials was measured
on the cross section of the printed fabrics/carpet
materials.

3.3 Image Qualities 4. Results and Discussion

An Image Xpert stationary system, supplied by
Image Xpert Inc., USA, was used in this study to
analyse the quality of images that the inkjet
printed onto the nylon fabrics and carpet materials.
The system consisted of charge-coupled device
27
Two families of ink formulation were prepared;
namely, Group A inks which contained Natrosol as
a thickener while Group B inks contained a
sodium alginate as the thickener. The relevant test
results are shown in Tables 3-4 and Figures 1-11.
RJTA Vol. 16 No. 1 2012

4.1 Effects of Binders on the Viscosities of experienced by the inks at a low Natrosol
Inks concentration range.

The viscosities of various inks prepared are shown The relationship between the surface tension and
in Tables 3 and 4. The effects of the binders on the binder concentration of the Group B inks was
the viscosities of the inks are shown in Figures 1 relatively complex, possibly due to the opposing
and 2. It can be seen from Figure 1 that the effects of the binders and the various solvents and
viscosities increase with an increase in the additives. (Figure 4) However, as the
concentration of Natrosol for Group A inks. The concentration of the binder increased, the surface
viscosities of Group B inks also increase as the tensions of the inks generally increased, resulting
concentration of sodium alginate increases (Figure in reduced ability of the resulting inks to spread.
2). Such effects are expected, due to the
thickening effect of Natrosol and sodium alginate. Table 4. Properties of the inks containing
However, an interesting observation was that the Sod.alginate.gel2%.
viscosities of the Group A inks experienced a peak Ink sample Viscosity Surface tension
value before the concentration of Natrosol in the code (cP) (mN/M)
ink formulation reached the maximum. A1 5.7 35
A2 25 32.2
Table 3. Properties of the inks containing A3 4 35.3
Natrosol.gel 3%. A4 20 32
Ink sample Viscosity Surface tension A5 3 36
code (cP) (mN/M) A6 23 31
A1 5.7 35 A7 3 36
A2 19 32 A8 15 32.6
A3 4 35.3 A9 3.5 36
A4 15 32.5 A10 12 32.8
A5 3 36 A11 5 35.2
A6 20 32 A12 15 32.5
A7 3 36 A13 4 35.6
A8 10 34 A14 28 30.8
A9 3 36.3 A15 4.5 35.4
A10 8 34.3 A16 20 32
A11 5 35.2
A12 10 34
A13 4 35.6
A14 20 31.9
A15 4.5 35.4
75
A16 15 32.5
50 DEG
Viscosty 30.00
4.2 Effects of Binders on the Surface Tensions
25
of the Inks 20.00

0.00
0
The surface tensions of the inks in Groups A and B Natr olsol gel
30.00 0.00
are shown in Tables 3 and 4. The effects of the 50.00
binders on surface tension are shown in Figures 3 water
and 4. It can be seen from Figure 3 that the surface Fig. 1. Correlation of viscosity of ink to Natrosol
tension of Group A inks decreases as the 3% gel, water and DEG
concentration of Natrosol increases. This is likely
due to the contribution of sodium alginate for the
improved spreading ability of the resulting inks.
There was a peak value of surface tension

28
RJTA Vol. 16 No. 1 2012

density for Group A inks decreases as the content

of Natrosol in the inks increases, possibly due to
the dilution effect. However, the situation for the
60
carpet materials is reversed, which is possibly due
to the reduced amount of ink penetration as the
40
DEG binder content increased. Similar effects
viscosity 30.00 occurred for the Group B inks, as evident in
20 Figure 7.
25.00

0.00
0 Table 5. Effect of Natrosol 3% gel on optical
SOD.A
30.00 0.00 density of print at different ratios of
55.00
DEG, EG and IPA
WA TER

Fig.2. Correlation of viscosity to Sod.alginate Ink Optical density Optical density on

2%gel, water and DEG sample code on fabrics carpet materials
A1 1.3 1.9
IP A A2 2.2 2.5
30 A3 1.7 1.9
A4 2.4 2.5
A5 1.3 1.8
A6 2.4 2.5
A7 1.5 1.9
0 20 A8 2.2 2.4
A9 1.4 2.1
A10 2.3 2.6
A11 1.3 2
A12 2.1 2.6
50 0 30 A13 1.4 1.9
water Na t r o ls o l g e l
A14 2.3 2.5
Fig.3. Correlation of surface tension to Natrosol
A15 1.4 1.8
3%gel, water and IPA
A16 2.4 2.3

Table 6. Effect of Sod.alginate 2% gel on optical

density of print at different ratios of DEG,
34
EG and IPA
Ink Optical density Optical density on
IP A
s u e f a ce .te n
32
30.00
sample code on fabrics carpet materials
25.00
A1 1.3 1.8
30 0.00
A2 1.8 2.2
A3 1.7 1.9
SO D .A
30.00 0.00 A4 2 2.3
55.00
WA T E R
A5 1.3 1.8
Fig.4. Correlation of surface tension to A6 2 2.3
Sod.alginate 2%gel, water and IPA A7 1.3 1.9
A8 1.7 2.3
4.3 Effects Of Binders on Optical Density of A9 1.4 2
Prints A10 2 2.3
A11 1.3 2
The optical density of the prints on the fabrics and A12 1.9 2.3
carpet materials are shown in Tables 5 and 6 and A13 1.3 1.8
Figures 5 and 6. A14 1.9 2.5
A15 1.3 1.9
It can be seen from Figure 5 that the optical A16 2 2

29
RJTA Vol. 16 No. 1 2012

4.4 Effects Of Binder Content on Ink

Spreading

The measured diameters of the circles printed on

the carpet materials are shown in Tables 7 and 8
and Figures 8 and 9.

Table 7. Effect of Natrosol 3%gel on circle size

and depth of penetration at different ratios
of DEG, EG and IPA
Ink sample Circle size on Depth of
code fibre (cm) penetration %
A1 2 100
Fig. 5. Correlation of optical density of print on A2 1.9 100
fabrics to Natrosol 3% gel, water and A3 2 90
DEG A4 1.7 100
A5 2.5 100
DEG A6 1.9 100
50 A7 2.4 100
A8 1.8 100
A9 2.5 100
A10 1.8 80
A11 2.3 60
A12 1.8 100
0 0 A13 2.2 100
A14 1.9 100
A15 2.4 100
A16 1.9 100

Table 8. Effect of Sod. alginate 2%gel on circle

50 0 50 size and depth of penetration at different
water Natrolsol gel ratios of DEG, EG and IPA
Fig. 6. Correlation of optical density of print on Ink sample Circle size on fibre Depth of
carpet to Natrosol 3% gel, water and DEG code (cm) penetration %
A1 2.2 90
A2 1.8 100
A3 2.1 60
A4 1.6 100
2.0 A5 2.3 100
A6 1.7 100
1.5 DEG A7 2.4 100
O.D.on fiber 30.00 A8 1.6 100
1.0 A9 2.4 60
25.00
A10 1.6 100
0.5 0.00
A11 2.3 100
SOD.A
30.00
A12 1.6 80
0.00
55.00 A13 2.2 90
WA TER A14 1.8 100
Fig. 7. Correlation of optical density of print on A15 2.4 100
fabrics to Sod.alginate 2% gel, water and A16 1.7 100
DEG

30
RJTA Vol. 16 No. 1 2012

IP A 4.5 Effects of Binder Content on Ink

30
Penetration

The depth of ink penetration on the carpet

materials is shown in Tables 7 and 8, Figure 10,
and Plates 1 and 2.
0 20

DEG
50

50 0 30
water Na t r o ls o l g e l
Fig. 8. Correlation of circle size of print on fabrics
to Natrosol 3% gel, water and IPA.
0 0
It can be seen from Figures 8 and 9 that the
diameter of the printed circles decreases as the
binder content increases, most likely due to the
reduced spreading of the inks on the carpet
materials, resulting from increased viscosity and
surface tension of the relevant inks.
50 0 50
water Natrolsol gel
Fig.10. Correlation of depth of penetration of ink
on carpet to Natrosol, water and EG
2.25
It can be seen from Figure 10 that the relationship
2.00
EG
between the depth of ink penetration and binder
D.Size on fiber 30.00 content is a complex one. This is likely due to
1.75
25. 00
the fact that both viscosity and surface tension
1.50
0.00
affect the depth of penetration. It is the balance
between the opposing effects of viscosity increase
SO D.A
30.00 0.00 and surface tension increase that determines the
55.00
depth of penetration, which depends on the
WA T ER
structure of the substrate (e.g. porosity).
Fig. 9. Correlation of circle size of print on fabrics
to Sod.alginate 2% gel, water and EG.

(a) (b)
By Natrosol thickener by Sodium alginate
Plate 1. Image of the circles printed on carpet materials

31
RJTA Vol. 16 No. 1 2012
(a)
Plate 2. Cross section of printed carpet material showing penetration of ink
Plate 3. Images printed on fabrics
4.6 Stability of Inks
All of the prepared ink formulations were stored in
glass sample bottles for six months at ambient
temperatures. Their viscosities, surface tensions
and extent of precipitation were observed at
regular intervals. It was found that all of the inks
have relatively constant viscosities and surface
tensions, and that there is no precipitation.
5. Conclusion
Based on the findings described above, the
following are the conclusions.
Natural thickeners, Natrosol and sodium alginate,
could be used to successfully regulate the
viscosities and surface tensions of ink
formulations for printing onto nylon carpet
materials.
All of the fabrics and carpet materials printed with
inks that contained Natrosol and sodium alginate
have higher optical densities than those with inks
that did not contain binders.
Highly reproducible prints could be created by
jet-printing through the use of inks that contain a
natural thickener on polyamide fabrics and nylon
carpet materials which give high quality prints
(Plate 3).All of the ink formulations prepared have
good storage stability.
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(b)
Plate 4. Images printed on carpet
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