Journal of Industrial Textiles

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Paraffin Wax Emulsion as Water Repellent for Cotton/Polyester Blended

Fabric
M.H. Abo-Shosha, Z.H. El-Hilw, A.A. Aly, A. Amr and Al Said I. El. Nagdy
Journal of Industrial Textiles 2008 37: 315
DOI: 10.1177/1528083707083793

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 Paraffin Wax Emulsion as Water
Repellent for Cotton/Polyester
Blended Fabric
M. H. ABO-SHOSHA,* Z. H. EL-HILW,
A. A. ALY AND A. AMR
Textile Research Division, NRC, Dokki, Cairo

AL SAID I. EL. NAGDY

Faculty of Science, Ain Shams Un., Cairo

ABSTRACT: Paraffin wax emulsion is prepared by emulsifying paraffin wax (PW)

in water using stearic acid (SA) and triethanolamine (TEA) emulsifying system. A
mother emulsion is prepared at different concentrations of PW (10.519.1%w/w)
and SA (4.513%w/w) neutralized to different extents by TEA (25100% degree of
neutralization). Upon treating 50/50 cotton/polyester fabric with a padding solution
containing 50 g/L of different mother emulsions, its water repellency does not exceed
the value of 50. Aluminum chloride proves to be the best deactivating agent of the
hydrophilicity of the emulsifying agent among other salts including barium chloride,
zinc sulfate, and aluminum sulfate. Optimum emulsion ingredients are found to be
PW (10.5%w/w), SA (4.5% w/w), TEA (2.4% w/w, to attain full neutralization of
SA), and SA/AlCl3 molar ratio (1/1). Treating the fabric with the deactivated
emulsion results in enhancing its water repellency rating (up to 80), decreasing its
surface roughness, and increasing its stiffness. A scanning electron micrograph of the
treated fabric shows the deposition of the emulsified wax on the fabric surface.
Treating the fabric with the emulsion in the presence of a fluorochemical finish,
namely Nuva FB of Clariant, proves that the first can be used as an extender for the
second. Raising the drying temperature to 160 C gives rise to a water-repellency
rating of 100.

KEY WORDS: paraffin wax emulsion, stearic acid, water repellent, hydrophilicity
deactivating agents, extender.

*Author to whom correspondence should be addressed.

E-mail: mshosha1@yahoo.com

JOURNAL OF INDUSTRIAL TEXTILES, Vol. 37, No. 4April 2008 315

1528-0837/08/04 031511 $10.00/0 DOI: 10.1177/1528083707083793
SAGE Publications 2008
Los Angeles, London, New Delhi and Singapore
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316 M. H. ABO-SHOSHA ET AL.

INTRODUCTION

can be broadly divided into three groups

T EXTILE WATER REPELLENTS
[14]. The first comprises hydrocarbon hydrophobes which includes
paraffin wax (PW) emulsions and fiber reactive hydrocarbon hydrophobes
(e.g., N-methylol stearamide melamine wax type water repellents, metal
complexes). The second and the third are silicones and fluorochemicals.
PW emulsions are the most economical water repellents for textiles. They
acquire the fabric good water repellency, however, they are not durable to
repeated laundering [1,4]. Accordingly, they can be applied onto fabrics that
are not subjected to laundering, such as tent fabrics, upholstery, and fabrics
used for covering goods in transport and storage.
The present work is undertaken with a view of preparing a PW
emulsion suitable to impart 50/50 cotton/polyester fabric good water
repellency. PW is emulsified in water using stearic acid triethanolamine
emulsifying system.

EXPERIMENTAL DETAILS

Materials

Mill scoured and bleached 50/50 cotton/polyester fabric (145 g/m2)

supplied by Misr Spinning and Weaving Co., Mehalla el Kobra, Egypt,
was used. PW supplied by Al Amirya Petroleum Co., Alexandria, Egypt was
used. Stearic acid (SA), triethanolamine (TEA), barium chloride, zinc
sulfate, aluminum chloride, and aluminum sulfate, reagent grades, were
used.

Preparation of the Mother Wax Emulsion

Specified weights of PW (918 g) along with SA (3.7511.25 g) were

melted together in a 250 mL glass beaker in a thermostated water bath at
6570 C. To that mixture, 70 g of an aqueous solution of TEA (containing
520 g TEA) at 6570 C were gradually added with stirring, using a strong
homogenizer, within a period of 3 minutes. Stirring is continued for an extra
3 minutes to obtain a homogeneous oil in water mother emulsion. In case of
metal salt containing emulsion, the amount of TEA is dissolved in water to
50 g, and the emulsion is formed as usual. Then 20 g of an aqueous solution
of the salt are added with homogenizing to the wax emulsion to form the
metal salt containing mother wax emulsion.

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 Paraffin Wax Emulsion as Water Repellent for Blended Fabric 317

Fabric Treatment

Certain weight of the mother emulsion is diluted, with stirring, with water
to a specified concentration, in which the fabric is padded two dips and two
nips to a wet-pick up of 100%. Then it is dried at specified temperatures and
times.

Testing

Water repellency was performed using the spray test as described by

AATCC Test Method 22-1989. Oil repellency rating was measured as
described in AATCC Test Method 118-1992. Stiffness was determined
according to ASTM Test Method D 1388-96 using the cantilever apparatus.
Roughness was measured using a surfacoder 1700a. Scanning electron
microscopy was conducted on S 360 LEICA scanning electron microscope.

RESULTS AND DISCUSSION

Ingredients of the Mother Emulsion

In this paper, the impact of changing the concentration of the ingredients

of the mother emulsion (i.e., PW, SA, and TEA) on water repellency rating
of the fabric is studied. In each run, the fabric is treated with a bath
containing 50 g/L of the mother emulsion.

Paraffin wax concentration

Table 1 shows the effect of the concentration of PW in the mother

emulsion on water repellency rating of the treated fabric. It is clear that the

Table 1. Effect of paraffin wax concentration in the mother emulsion

on water repellency rating of the treated fabric.

Paraffin wax concentration (wt/wt) Water repellency rating

Blank, untreated 0
10.5 50
15.1 50
19.1 50

Other ingredients of mother wax emulsion: stearic acid (4.5%); triethanolamine (2.4%).
The fabric is padded in 50 g/L of mother emulsion to a wet pick up of 100%; dried at 100 C/5
minutes.

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318 M. H. ABO-SHOSHA ET AL.

Table 2. Effect of stearic acid (SA) concentration in the mother

emulsion on water repellency rating of the treated fabric.

SA concentration (%) (wt/wt) Water repellency rating

Blank, untreated 0
4.5 50
9 50
13.5 50

Other ingredients of mother emulsion: paraffin wax (10.5%); triethanolamine

(equivalent amount of SA).
The fabric is padded in 50 g/L of mother emulsion to a wet pick up of 100%; dried at
100 C/5 minutes.

treatment imparted the fabric water repellency, compared to the untreated

sample. This is a direct consequence of coating the fabric with a low surface
energy film of PW. However the rating, which is 50, is the lowest in the scale
of the test, whatever the wax concentration used in the mother emulsion.
This can be associated with the hydrophilic nature of the emulsifying
agent (SA salt of TEA) that impairs the hydrophobic character of PW [1].

Stearic acid Concentration

Table 2 shows the effect of SA concentration on water repellency rating of

the treated fabric. Obviously, increasing the concentration from 4.5 to
13.5% has no effect on water repellency rating of the fabric. Once more, the
rating is still at its minimum level of the scale of the test.

Degree of neutralization of SA

The presence of TEA is important as it neutralizes SA to form the

emulsifier. However, it has the drawback of being hydrophilic, which
detracts from the hydrophobicity of PW [1]. In the previous run the amount
of TEA used was sufficient to induce full neutralization SA. It was thought
that if TEA was added to attain partial neutralization of SA it would be
helpful for promoting the emulsion hydrophobicity. Table 3 shows the effect
of the degree of neutralization of SA on water repellency rating of the
treated fabric. It is seen that: (a) the mother emulsion is not formed up till a
degree of neutralization of 50%, (b) at a degree of neutralization of 75%, the
emulsion is formed, however upon dilution relatively large particles appear
resulting in non-homogeneous treatment, and (c) a successful emulsion is
formed at a degree of neutralization of 100%. Nevertheless, the last
emulsion gives rise also to a very low water repellency rating, which is 50.

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 Paraffin Wax Emulsion as Water Repellent for Blended Fabric 319

Table 3. Effect of degree of neutralization of stearic acid (SA) by

triethanolamine on water repellency rating of the treated fabric.

Degree of neutralization Water repellency rating

Blank, untreated 0
0a
25a
50a
75b 50
100c 50

Other ingredients of mother wax emulsion: paraffin wax (10.5%) SA (4.5%)

a
: no stable emulsion is formed, b:emulsion with large particles, and
c
: homogeneous soft emulsion.

Deactivating the Emulsifying Agent

The reason behind impairing the hydrophobicity of the treated fabric, as

has already been mentioned before, is the emulsifying agent [1], i.e., SA salt
of TEA. To deactivate the emulsifying agent when the fabric is heated, some
salts of polyvalent metals, such as barium chloride, zinc sulfate, aluminum
chloride, and aluminum sulfate, were added to a mother emulsion
(containing PW (10.55 w/w), SA (4.5% w/w), and TEA (2.4% w/w)).
These salts were added in an equimolar ratio of that of stearic acid.
Addition of either barium chloride or zinc sulfate resulted in precipitating
the emulsion immediately. Aluminum sulfate gave rise to an emulsion with
two layers, the upper one contained the emulsified phase and the lower one
was an aqueous clear solution. Addition of aluminum chloride brought
about neither precipitation nor separation. So aluminum chloride was
selected as a deactivating agent.
The effect of changing aluminum chloride-to-SA molar ratio on the
physical nature of the mother emulsion and water repellency rating of the
treated fabric is shown in Table 4. It is clear that increasing the ratio from
0/1 to 1/1 is accompanied by an increase in water repellency rating from 50
to 80, a result that signifies the importance of aluminum chloride in
deactivating the emulsifying agent. Increasing the ratio in the range of
15/12/1 results in changing the emulsion from the liquid state to a paste
form. Upon dilution the paste (for fabric treatment) precipitated.
Accordingly, a ratio of 1/1 is considered as an optimum ratio.
The effect of treating the fabric with different concentrations of the
deactivated emulsion on the water repellency rating, surface roughness, and
stiffness is shown in Table 5. It is evident that increasing the concentration
from 25 to 50 g/L is accompanied by increasing water repellency rating from

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320 M. H. ABO-SHOSHA ET AL.

Table 4. Effect of AlCl3/stearic acid (SA) molar ratio on the physical appearance of
the mother emulsion and water repellency rating of the treated fabric.

AlCl3/SA Physical appearance Water repellency

molar ratio of the mother emulsion rating of the treated fabrica

0/1 Liquid emulsion 50

0.5/1 Liquid emulsion 70
1/1 Liquid emulsion 80
105/1 Pasteb b
2/1 Pasteb b
Ingredients of mother emulsion: paraffin wax (10.5%); SA (4.5%); triethanolamine (2.4%). a: the fabric was
padded in 50 g/L of the mother emulsion, dried at 100 C/5 minutes and b: upon dilution of the paste to 50 g/
L, it was precipitated, and hence no treatment was carried out.

Table 5. Effect of AlCl3 containing wax emulsion concentration on water

repellency, roughness, and stiffness of the treated fabric.

Stiffness (mg
cm)

Emulsion Water Surface

concentration (g/L) repellency rating roughness (mm) Warp Weft

Blank, untreated 0 12.96 10607 3694

25 70 11.34 12047 4349
50 80 9.39 15280 5349
75 80 8.52 16599 5856
Ingredients of mother emulsion: paraffin wax (10.5%); stearic acid (SA) (4.5%); triethanolamine (2.4%),
Al2Cl2/SA (1 mole/1 mole). Wet pick up 100%; drying at 100 C/5 minutes.

70 to 80 along with promoting surface smoothening (or decreasing the

roughness) while increasing the fabric stiffness. Further increase in
concentration up to 75 g/L results in no change in water repellency.
However, both the surface smoothness and the fabric stiffness increase.
Increasing the surface smoothness can be attributed to the deposition of a
smooth film of the solid ingredients of the emulsion (PW and deactivated SA/
TEA) on the fabric surface that reduces friction. Promoting the stiffness of
the fabric suggests that the emulsion can be used to acquire body to fabric.
Figure 1 is a scanning electron micrograph of the fabric before (a) and
after treatment with 50 g/L (b) and 75 g/L (c) of AlCl3 containing emulsion.
It is seen that the film deposited in the case of a concentration of 50 g/L is
more homogeneous than that in the case of 75 g/L. Moreover, the
depositions acquired the yarns more thickness as can be seen in (b) and
(c) compared to the blank sample in (a).

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 Paraffin Wax Emulsion as Water Repellent for Blended Fabric 321
(a)

(b)

(c)

FIGURE 1. A scanning electron micrograph of the fabric before (a) and after
treatment with 50 g/L (b) and 75 g/L (c) of AlCl3 containing emulsion.

Emulsion as an Extender for a Fluorochemical Finish

It is known that commercial wax emulsions can be used as extenders for

fluorochemical finish [5]. That is, they can replace some of the expensive

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322 M. H. ABO-SHOSHA ET AL.

Table 6. Water repellency rating of the fabric treated with the emulsion in
conjunction with Nuva FB.

Nauva FB Wax emulsion Water Oil repellency

concentration (g/L) concentration (g/L) repellency rating rating

Blank, untreated 0 0
0 25 70 0
50 80 0
70 80 0
20 0 80 7
25 90 7
50 90 7
75 90 7
30 0 90 7
25 90 7
50 100 7
75 100 7
Ingredients of mother emulsion: paraffin wax (10.5%); stearic acid (SA) (4.5%); triethanolamine
(2.4%), Al2Cl2/SA (1 mole/1 mole). Wet pick up 100%; drying at 100 C/5 minutes.

fluorochemical finish to attain the same performance properties of the

finished fabric with a less expensive formulation. To check the validity of
using the prepared wax emulsion as an extender of a fluorochemical finish of
textiles, for example Nuva FB of Clariant, the emulsion was used in
combination with different concentrations of the latter and the performance
properties of the finished fabric were measured and tabulated as shown in
Table 6. It can be seen that the fabric treated with Nuva FB in the absence of
the emulsion acquired both hydrophilicity and oleophobicity, a character-
istic of fluorochemical finish [610]. Addition of the emulsion in the presence
of Nuva FB has no effect on oil repellency rating. However, some changes
occurred regarding water repellency rating. At a concentration of 20 g/L of
Nuva FB, addition of the emulsion at a concentration of 25 g/L raised
the water repellency rating from 80 to 90. Further increase in emulsion
concentration up to 75 g/L has no effect on water repellency rating. At a
Nuva FB concentration of 30 g/L, water repellency rating increased only in
the concentration range of 5075 g/L of the emulsion. It can be concluded
from Table 6 that the emulsion can be used as an extender for a
fluorochemical finish in virtue of the facts that: (a) the fabric properties at
a Nuva FB concentration of 30 g/L can be attained at a lower concentration
of 20 g/L along with the emulsion at a concentration of 2575 g/L, and (b)
addition of the emulsion to Nuva FB enhances, in general, the water
repellency rating of the fabric under the conditions employed.

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 Paraffin Wax Emulsion as Water Repellent for Blended Fabric 323

Table 7. Effect of drying temperature on water repellency rating of treated fabrics.

Drying temperature ( C) 100 120 140 160

Water repellency rating 80 80 90 100
Ingredients of mother emulsion: paraffin wax (10.5%); stearic acid (SA) (4.5%); triethanolamine (2.4%),
Al2Cl2/SA (1 mole/1 mole). Wet pick up 100%.

Drying Temperature

Fabric samples were padded in a finishing bath containing 50 g/L of

mother emulsion, then dried at different temperatures (120160 C) for
5 minutes. The results of water repellency ratings are shown in Table 7. It
can be seen that (a) water repellency ratings of samples dried at 120 C is the
same as that dried at 100 C, and (b) higher drying temperatures result in
promoting water repellency ratings, i.e., a rating of 90 is attained at 140 C
and a rating of 100 is obtained at 160 C. It seems that at such elevated
temperatures, the waxy layer gets more uniform distribution on the fabric
surface, which results in higher water repellency rating. Furthermore, it is
probable that SA/TEA salt orient itself, under the action of heat energy,
in such a manner that the hydrophilic heads (carboxyl-amine moieties) are
adsorbed on the fiber surface and the hydrophobic tails are oriented
outwards, giving rise to extra hydrophobic layers on the fabric surface.

Storage Stability

A stoppered glass bottle, containing 500 mL of the mother emulsion was

stored for different periods of time, i.e., 3, 6, and 9 months. After each
period it was found that the emulsion separated into two layers. A clear
solution was in the bottom, and a somewhat thicker emulsion above it. The
height of the bottom layer is about one-fifth of that of the upper layer. Upon
shaking, the two layers disappear, and a homogeneous emulsion is formed.
Fifty grams of this emulsion, after each period, were used to treat fabric
samples, and then they were dried at 160 C/5 minutes. Water repellency
rating in each case was 100. This result indicates that the emulsion is stable
upon storing up to 9 months.

CONCLUSIONS

A PW emulsion was prepared by emulsifying the wax in water using

SA/TEA emulsifying system. The emulsion was used to impart 50/50

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324 M. H. ABO-SHOSHA ET AL.

cotton/polyester fabric water repellency at different concentrations of PW,

SA, and TEA. However, the water repellency rating did not exceed the value
of 50. Deactivating the emulsifier using aluminum chloride resulted in
enhancing the water repellency of the treated fabric. Optimum emulsion
ingredients were PW (10.5%), SA (4.5%), TEA (2.4%), and SA/aluminum
chloride molar ratio (1/1). This emulsion could be used as an extender for
fluorochemical finishes. Elevated drying temperature (160 C/5 minutes)
results in promoting its water repellency ratings to reach 100. The emulsion
is stable upon storing up to 9 months.

REFERENCES

1. Tomasino, C. (1993). Chemistry and Technology of Fabric Preparation and

Finishing, Chap 9, p. 154, College of Textile, NCSU, NC,USA.
2. Sadov, F., Korchongin, M. and Matcsky, A. (1978). Chemical Technology of
Fibrous Materials, Translated from Russian by Chernyshova, A., p. 651,
Mir Pub., Moscow.
3. Moilliet, J.L. (1963). Water Proofing Emulsions, In: Moilliet, J.L. (ed.), Water
Proofing and Water Repellency, Chap. 3, p. 52, Elsevier Pub. Co., New York.
4. Higgins, E.B. (1963). Water Repellency Treatment of Cellulosic Fibers, Ibid,
Chap. 6, p. 188.
5. Abo-Shosha, M.H. (1978). Finishing of Textile Materials to Obtain Water/Oil
Repellency and Soil Release Properties, MSc Thesis, Cairo University, Cairo.
6. Sato, Y. (1994). Effect of Crosslinking Agents on Water Repellency of Cotton
Fabrics Treated with Fluorocarbon Resin, Text. Res. J., 64(6): 316.
7. Achwal, W.B. (1991). Developments in Auxiliaries (Speciality Chemicals) for
Textile Processing, Colourage Annual, 133.
8. Gulf Coast Section (1997). Performance of Flame Retardant and Water
Repellent Finishes for Kenaf/Cotton Blend Fabrics, Text. Chem. Colorist,
29(12): 22.
9. Connick Jr, W.J. and Ellzey Jr, S.E. (1968). Emulsion Application of a Poly
(Perfluorooctanoyl) Ethylenimine to Cotton, Amer. Dyestuff. Rep., 29: 17.
10. Audenaert, F., Lens, H., Rolly, D. and Vander Elst, P. (1999). Fluorochemical
Textile Repellents-Synthesis and Applications: A3M Perspective, J. Text. Inst.,
90(3): 76.

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 Paraffin Wax Emulsion as Water Repellent for Blended Fabric 325

BIOGRAPHY

Professor Zeinab Haroun El-Hilw received her

BSc (1972), MSc (1982), and PhD (1994) in textile
printing, dyeing and finishing from the Helwan
University Faculty of Applied Arts. She joined the
Textile Research Division of the National
Research Center (Dokki, Cairo, Egypt) in 1974
and graduated in research positions from research
assistant to researcher to associate professor and
professor in the field of chemistry and technology
of carbohydrates. She supervised about two MSc
and PhD thesis in the field of textile wet
processing. She has over 20 scientific papers
published in international periodicals covering the field of textile wet
processing. She has participated in many industrial and environmental
projects in Egypt.

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