Journal of Natural Fibers

ISSN: 1544-0478 (Print) 1544-046X (Online) Journal homepage: https://www.tandfonline.com/loi/wjnf20

Surface Modification of Jute Fabric by Treating

with Silane Coupling Agent for Reducing Its
Moisture Regain Characteristics

Runumi Gogoi & Ajay Kumar Tyagi

To cite this article: Runumi Gogoi & Ajay Kumar Tyagi (2019): Surface Modification of Jute Fabric
by Treating with Silane Coupling Agent for Reducing Its Moisture Regain Characteristics, Journal of
Natural Fibers, DOI: 10.1080/15440478.2019.1658252

To link to this article: https://doi.org/10.1080/15440478.2019.1658252

Published online: 27 Aug 2019.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2019.1658252

Surface Modification of Jute Fabric by Treating with Silane

Coupling Agent for Reducing Its Moisture Regain Characteristics
Runumi Gogoi and Ajay Kumar Tyagi
Material Science Division, Shriram Institute for Industrial Research, Delhi, India

ABSTRACT KEYWORDS
In the present study, the effect of silane treatment method on reducing the Jute fabric; silane treatment;
moisture regain of the jute fabric was investigated. Triethoxyvinylsilane, moisture regain;
hydrophobic; surface
a widely used hydrophobic silane is used as the silane coupling agent. modification
The treated fabrics were characterized by Fourier transform infrared spec-
troscopy (FTIR), Scanning electron microscopy/Electron dispersive spectro- 关键词
scopy (SEM/EDS) and for contact angle, moisture regain etc. It was observed 黄麻织物; 硅烷处理; 回潮
that the moisture regain of the jute fabric reduced significantly by this 率; 疏水性; 表面改性
treatment. The contact angle measurement showed that after silane treat-
ment, the surface of the jute fabric became exclusively hydrophobic in
nature with a contact angle of 111°. FTIR analysis of the treated fabric
showed the presence of Si-O-C linkage on the surface which confirms that
the hydroxyl groups of the jute fabric react with the silanol molecules
forming Si-O-C linkages. The grafting of silane molecules onto the surface
of jute fabric was further confirmed by the presence of silicone atoms
detected by electron dispersive spectroscopy. It is expected that the find-
ings of the work will open up new horizons for utilization of jute fabric in
the area of healthcare, oil absorbent mat, composites and geo-textiles.

摘要
研究了硅烷处理对黄麻织物回潮率的影响. 三乙氧基乙烯基硅烷是一种广
泛使用的疏水性硅烷，用作硅烷偶联剂.用傅立叶变换红外光谱（FTIR）、
扫描电子显微镜/电子分散光谱（SEM/EDS）对织物进行了表征，并对织
物的接触角、回潮率等进行了表征. 结果表明，处理后黄麻织物的回潮率
明显降低。接触角测量结果表明，经硅烷处理后，黄麻织物的表面呈完
全疏水性，接触角为111°. 对处理后的织物进行FTIR分析，发现表面存在
Si-O-C键，这证实了黄麻织物的羟基与硅醇分子反应形成Si-O-C键. 通过电
子分散光谱检测硅原子的存在进一步证实了硅烷分子在黄麻织物表面的
接枝. 预计这项研究成果将为黄麻织物在保健、吸油垫、复合材料和土工
织物领域的应用开辟新的天地。

Introduction
Jute is an abundantly available natural biodegradable fiber, which occupies the second position in
terms of world production levels after cotton (Jan 2009; Teli et al. 2013). Among all the natural
fibers, jute fiber is gaining prominence on account of its low cost, low density, high specific strength
and modulus, no health risk, easy availability, biodegradability and much lower energy requirement
for processing. The constituents of jute fibers are mainly cellulose (60–62%), hemicellulose (22–24%)
and lignin (12–14%). In addition, it contains other minor constituents (1–2%) of fats, waxes,

CONTACT Runumi Gogoi Runumi@shriraminstitute.org Material Science Division, Shriram Institute for Industrial Research,
19 university road, Delhi 7, India
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/WJNF.
© 2019 Taylor & Francis
2 R. GOGOI AND A. K. TYAGI

inorganic matter, nitrogenous matter and traces of pigments like b-carotene and xanthophylls
(Chattopadhyay et al. 2010).
The jute fibers possess many positive attributes, however its inherent property of attaining
moisture in its surface is limiting its use for many applications. The moisture regain of jute fibers
varies between 5% and 12% (Ali et al. 2016). The presence of large number of hydroxyl groups in the
cellulose makes the jute fiber hydrophilic in nature and sensitive to regain moisture present in the
atmosphere (Erdogan et al. 2016).
The use of jute fabric is limited to packaging materials like grocery bags, shopping bags, floor
mats, ropes, canvas, etc. (Teli et al. 2013). The jute fiber, if made less moisture sensitive, i.e.,
hydrophobic, will find wide applications in the areas of composites, healthcare, geo-textiles, oil
absorbent, etc. In areas of composites, its high moisture regain affinity cause weak bonding between
fiber and the matrix causing dimensional instability, matrix cracking and poor mechanical properties
of the composites (Celino et al. 2014; Singhal et al. 2014).
In the current work, the silane treatment of the jute fabric was carried out with the aim to make it
appropriate for being used in medical bandage. The medical bandage is used to immobilize body
parts during fracture or injury. The bandage was prepared by coating moisture curable polymeric
resin onto the surface of jute fabric. The moisture absorption affinity of the jute fabric cause
premature hardening of the bandage and reduces its shelf life. Thus, a continuous scientific
investigation is needed to reduce the moisture regain property of jute fiber for opening new avenues
in the area of innovative healthcare and modern day’s industrial need while fulfilling market
demand.
A silane treatment of jute fabric is considered as one of the step forward toward reducing the
hydrophilic character of the jute fabric. The use of silane coupling agents is gaining a lot of interest
because of their availability, low cost and ease of grafting. The hydroxyl groups of the jute fabric
which are responsible for its high moisture uptake can be blocked by hydrophobic moieties present
in silane coupling agents (Ramamoorthy, Rissanen, and Skrifvars 2014).
Recent works suggested that silane treatment is a most popular approach used for modifying
cellulosic materials. Koga, Kitaoka, and Isogai (2011) used a silane compound to modify cellulosic
surfaces with amine groups. Rouabhia et al. (2014) used aminosilane treatment as the first step in
preparing antibacterial surfaces. Abidi, Hequet, and Tarimal (2006) used vinyltrimethoxysilane to
functionalized cotton fabric to impart water repellency and wrinkle recovery property. Ali et al.
(2016) used silane treatment to improve the hydrophobic nature of flax fibers with improved
mechanical properties. Arbelaiz et al. (2005) reported in their work surface treatment of flax fibers
by using vinyltrimethoxysilane for improving the compatibility between flax fiber bundles and
polypropylene matrix. It has been observed that the polar component of the fabric was reduced
significantly by silane treatment; however, slight decrease in tensile strength of treated fabric was
observed. Another work reported by Fathi et al. (2019) has revealed that the fiber/matrix adhesion
was improved and water absorption was reduced significantly by silane treatment. They modify the
flax fibers by first oxidising it through 2,2,6,6, tetramethyl piperidine-1-oxy radical (TEMPO)
followed by direct application of aminosilane.
In the past, a lot of work has been reported on modification of natural fibers by treating them
with silane compound; however much limited work has been done on silane treatment of jute fabric
for making it useful for medical product. Thus, in the current paper, a very simple method was
explained for reducing moisture regain of jute fabric by treating them with triethoxyvinylsilane,
a silane coupling agent. Vinyl functionality of triethoxyvinylsilane is expected to increases the
hydrophobicity of the modified material. The silane treated jute fabric was characterized for Si-O
linkages by Fourier transform infrared spectroscopy (FTIR), presence of silicone by Scanning
electron microscopy/Electron dispersive spectroscopy (SEM/EDS), hydrophobicity through contact
angle measurement and change in moisture regain property. The tensile strength of the treated fabric
was also determined to observe any change in mechanical properties after the treatment. It is
 JOURNAL OF NATURAL FIBERS 3

expected that the findings of the work will open up new areas of utilization of jute fabric in the
market of healthcare, oil absorbent and composites.

Experimental
Materials
Knitted Jute fabric (GSM: 255 g/m2 at 65%RH & 27°C) was procured from P K Astir Ltd, New Delhi,
India (Figure 1(a)). It was used in raw form without any pretreatment. Triethoxyvinylsilane was
procured from Sigma Aldrich (Figure 1(b)). Acetone and Hydrochloric acid were procured from
sdFine Chem Ltd, Mumbai. All the chemicals used were of analytical grade.

Methods
Silane treatment of jute fabric
Triethoxyvinylsilane was hydrolyzed in acetone/water solution (80/20 v/v) with the addition of conc
HCl to adjust pH 3.5 to 4 and continuously stirred for 30 min. Five different concentrations (5, 10,
15, 20, 25 wt % of fabric) were made for the study. Pre-dried jute fabrics were then immersed in the
treatment solution for 2 h at ambient temperature. After the treatment, the fabric was taken out and
dried at room temperature for 1hr followed by oven drying at 110 ± 2°C till constant weight was
obtained. The treated fabrics were then used for further analysis. The possible reaction of silane
treatment method is given in Figure 2.

Characterization of untreated and treated jute fabric

Moisture regain analysis. The moisture regain is a property to evaluate the moisture absorption
capacity of a fabric. The moisture regain of the jute fabric was determined according to ASTM
D2654 89a. This method makes use of the oven-dry technique to calculate the moisture regain of the
fabric at standard atmospheric conditions (21 ± 1°C and 65 ± 2% relative humidity). The fabrics are
weighed after conditioning under standard atmosphere until moisture equilibrium is established. In
the next step, the fabrics were dried to constant mass in an oven maintained at 105 ± 2°C. The
difference between the mass of sample at moisture equilibrium and the oven dried mass is used to
calculate the moisture regain of the fabric.

Figure 1. a)Knitted jute fabric and b)Chemical structure of Triethoxyvinylsilane.

4 R. GOGOI AND A. K. TYAGI

Figure 2. Mechanism of silane treatment method.

Tensile strength analysis. The tensile strength of the fabric was determined in a universal tensile
machine following ISO 13934 − 1: 1999 (E). The width of the fabric was taken as 50 mm with
a gauge length of 200 mm and crosshead speed of 100 mm/min. A total number of five samples were
tested and their mean value was reported. All tests were conditioned at 20 ± 2°C and relative
humidity in the range of 65 ± 2%.

Water contact angle analysis. The hydrophobic property was evaluated by measuring water contact
angle. The contact angle was measured using a drop shape analyzer (DSA100) (JAS-ANZ make)
using the sessile drop method. The contact angle is measured using the image of a drop at the point
of intersection between the drop contour and the projection of the surface (baseline). The contact
angle is a measure of the wettability of the solid by the liquid. In the case of complete wetting, the
contact angle is 0°. Between 0° and 90°, the solid is wettable and above 90°, it is not wettable. In
the case of ultra hydrophobic material, with the so-called lotus effect, the contact angle approaches
the theoretical limit of 180°C.

Fourier transform infrared spectrometer analysis. Fourier transform infrared spectrometer (FTIR)
spectra of raw and treated fabrics were recorded in a FTIR spectrophotometer (Nicolet Corporation
USA). The fabric was dried in an oven at 105 ± 2°C prior to use. The dried fabric piece was then
analyzed in an attenuated total reflectance (ATR) detector over a range of 400 to 4000 cm−1 at
a resolution of 4 cm−1/min.

Scanning electron microscopy observation. The surface topography of the fabric was analyzed using
a scanning electron microscope (SEM) (SNE – 4500 M Plus, make SEC). Since the fabric is non-
conducting, it was gold-plated prior to analysis. The analysis was carried out with an acceleration
voltage of 15 kV at a working distance of 11 mm with 2.0 k magnification.

Energy dispersive spectroscopy analysis. Energy dispersive spectroscopy (EDS) analysis of the raw
and silane treated jute fabric was carried out in an energy dispersive spectrometer (make Bruker) to
determine the elemental composition of the fabric. The specimen is subjected to an electron beam of
accelerating voltage 15 kV of energy. The X-rays emitted from the element present in the fabric was
detected in a back scatter detector.
 JOURNAL OF NATURAL FIBERS 5

Preparation of medical bandage using silane-treated jute fabric

The bandage was prepared by coating moisture curable polymeric resin onto the surface of jute fabric.
The workroom was maintained at 25–30°C and the relative humidity of 35–40% during the coating
process. The coated fabric was then sealed under vacuum in a multilayer packet for shelf life analysis. The
shelf life analysis of the bandage was carried out by accelerated aging test. The sealed packet was put in an
oven maintained at 40°C and checked for any premature hardening of the bandage inside the packet. The
storage at 40°C for 124 days without any hardening amount to 2-year shelf life of the bandage at 20°C.

Results and discussion

Moisture regain
Moisture regain is an amount of water absorbed by a dried material at under standard conditions of
temperature and humidity compared to the mass of dried material. Figure 3 shows the change in
moisture regain from untreated to treated jute fabric. It can be seen that the moisture regain of the
jute fabric decreases sharply on silane treatment. The moisture regain of the jute fabric comes down
to 4.5% on 15wt% silane treatment. Further increase of silane concentration does not affect much on
moisture regain property of jute fabric.

Water contact angle

The extent of hydrophobization of the jute fabric was evaluated by determining the water contact
angle. The jute fabric treated with 15wt% triethoxyvinylsilane was used to determine the water
contact angle. As expected, before treatment the jute fabric was highly polar and hydrophilic. The
untreated jute fabric shows a water contact angle of 106° at the beginning but the droplet collapse
within 5–7 s, whereas the treated fabric gives a water contact angle of 111° and it remains as such up
to 60 s. The contact angle of a water droplet with time on both untreated as well as treated jute fabric
is shown in Figure 4. This clearly showed that the inherent hydrophilicity of the jute fabric get
reduced with silane treatment. The OH groups of the jute fabric get blocked by the silane molecules,
limiting its affinity toward water.
The water absorption behavior/surface hydrophobicity of the treated fabric was further confirmed
by the absorption of colored water droplets by the surface of the untreated jute fabric within 5 s and
non-absorption of water droplet by the silane treated fabric upto 4 h. After 4 h, the water droplet
slowly begins to loose its spherical shape and within 20–30 min it completely collapse (Figure 5).

10
Moisture regain (%)

9
8
7
6
5
4
3
2
0 5 10 15 20 25
Triethoxyvinyl silane (wt%)
Figure 3. Moisture regain of treated jute fabric as a function of silane concentration.
6 R. GOGOI AND A. K. TYAGI

Untreated Treated
120
100

Contact angle (o)

80
60
40
20
0
0 10 20 30 40 50 60
Time (sec)

Figure 4. Contact angles over time for the untreated and silane treated jute fabric.

Figure 5. Digital photographs of water droplets captured on the surface of (a) untreated jute fabric after 5 s and (b) treated jute
fabric after 60 s.

FTIR analysis
The FTIR analysis of the treated jute fabric clearly indicates that silanization has taken place at the
surface of the jute fabric (Figure 6). The treated jute fabric showed the presence of Si-O-Si peak (at
1032 cm−1), Si-O-C peak (at 1205 cm−1) and Si-O peak (at 777 cm−1). This confirms the chemical
reaction between hydrolyzed silane and the hydroxyl groups of the jute fabric forming Si-
O-C linkages creating polysiloxane network. The schematic representation of the probable reactions
of jute fabric with silane is depicted in Figure 2.

SEM and EDS analysis

The SEM images of the untreated and treated jute fabric surface are shown in Figure 7. The
untreated jute fabric has a characteristics straight configuration of jute fibers having rough surface
with impurities, whereas treated fabric has a smoother surface probably due to homogenous
deposition of silane compound on its surface.
The deposition of silane compound on the surface of jute fabric is further confirmed by the EDS
analysis (Figure 8 and Table 1). It can be seen from the table that the untreated jute fabric showed
the presence of only carbon and oxygen atom, whereas the treated fabric indicated the presence of Si
atom on the surface along with C and O. Also, the percentage of O in treated jute fabric gets reduced
which may be attributed to the bonding of OH groups in the form of Si-O linkages. Thus, it can be
 JOURNAL OF NATURAL FIBERS 7

-1
32 untreated 777cm
30
treated (Si-O)

28
26
24
-1
Transmittance(%)
1205 cm
22
(Si-O-C)
20
18
16
14
12
-1
1032 cm
10
(Si-O-Si)
8
6

1400 1200 1000 800 600 400

-1
Wavenumber (cm )

Figure 6. FTIR spectra of untreated and treated jute fabric.

Figure 7. SEM images of untreated and treated jute fiber.

inferred that the silane treatment is quite effective for blocking the hydroxyl groups of the jute fabric
for making it hydrophobic.

Tensile strength
While doing any treatment, it is also desirable that the jute fabric doesn’t loose its initial physical
properties. It was observed that the tensile strength of the jute fabric doesn’t get affected by the
treatment (Figure 9). In fact, a little bit improvement in tensile strength was observed after the silane
treatment. Initially, the tensile strength of the jute fabric was 25.45 Kgf/cm2, which after silane
treatment increased a little bit to 26.44 Kgf/cm2. This could be due to the fact that the fibers become
physically strong and rigid on silane treatment. With the increase in concentration over 15wt%, no
significant change was observed.
8 R. GOGOI AND A. K. TYAGI

Figure 8. EDS spectra of untreated and treated jute fabric.

Table 1. Elemental composition of untreated and treated jute fabric.

Element (wt %)
Sample C O Si
Untreated jute fabric 57.19 42.81 0
Treated jute fabric 72.60 26.14 1.27

Shelf life analysis of the medical bandage

Silane treatment of the jute fabric enhances the shelf life of the bandage significantly as is evident
from Table 2. The shelf life of the bandage was increased from 1 day (in case of untreated fabric) to
365 days (in case of treated fabric). The silane treatment of jute fabric blocks the hydroxyl groups of
the jute fabric by forming Si-O-Si linkages, thus prohibiting it from reaction with moisture sensitive
group of the polymeric resin and ultimately increasing the shelf life of the bandage.

Conclusion
It can be concluded that the surface treatment of jute fabric with triethoxyvinylsilane can be an
effective method for reducing surface hydrophilicity of the jute fabric. The moisture regain of the
 JOURNAL OF NATURAL FIBERS 9

27

Tensile strength (Kgf/cm2)

26.5
26
25.5
25
24.5
24
0 5 10 15 20 25
Triethoxyvinyl silane (wt%)

Figure 9. Tensile strength of treated jute fabric as a function of silane concentration.

Table 2. Shelf life of medical bandage prepared using untreated vs silane-

treated jute fabric.
Material Shelf life (in days)
Bandage – Untreated jute fabric 1
Bandage – Silane treated jute fabric (15wt %) 365

jute fabric is decreased significantly by silane treatment with a reduction of 48.2%. The increase in
contact angle to 111° clearly showed that after silane treatment, the surface of the jute fabric becomes
hydrophobic in nature. FTIR analysis of the treated fabric showed the presence of Si-O linkage,
confirming the fact that silanization of the jute fabric has taken place. The grafting of silane
molecules on the surface of the fabric is further affirmed by EDS analysis which shows the presence
of Si atoms in addition to C and O atoms. The tensile strength of the treated fabric exhibited no
significant changes in its values which confirm that the treatment method doesn’t affect the inherent
mechanical property of the fabric. Further, the treatment method is eco-friendly and cost-effective,
thus providing an attractive method for improving the surface hydrophobicity of the jute fabric
useful in varied applications.

Acknowledgments
The authors wish to thank Department of Science and Technology, Ministry of Science and Technology, Govt of India
for providing financial support and management of Shriram Institute for Industrial Research, India for their
encouragement in carrying out the study.

Funding
The authors funding by Department of Science and Technology, Ministry of Science and Technology, Govt of India
under grants number SP/YO/014/2016 (G).

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