Development of natural fibre reinforced polymer composites and

value added products using bauxite residue

Mohini Saxena
Former Scientist, Advanced Materials and Processes Research Institute (CSIR), Bhopal

Abstract
Bauxite residue (red mud) produced from aluminium industries is one of the major pollution
hazards for the surrounding environment. To address this problem, number of researchers all
over the world showed their serious concern by way of characterization and utilization of red
mud in value added products. In the present study red mud from National Aluminium
Company, India was initially characterized for its physical, chemical and mineralogical
properties and then used in various formulations with binders like polymer, along with sisal
and jute plant fibers, to intensify the physical as well as mechanical properties of the
resultant innovative composite. Bauxite residue polymer composite reinforced with natural
fibre is found to be a versatile material for its application in doors, partitions, flooring tiles,
furniture, instant houses and other similar mouldable products. Major contributions in this
area relates to processing of natural fibre reinforced polymer composites along with
industrial waste red mud in order to ensure uniform properties according to specification and
imparting excellent surface finish, durability, corrosion resistance and fire retardancy
characteristics. So developed value added composite materials has superior physical,
chemical mechanical properties and durability than teakwood, medium density fibre board,
rice husk board, particleboard, plywood etc. The environmental friendly and non polluting
features of these composite are the main attractions for overseas buyers.
The study gains significance from the fact that earlier investigators have focused their
attention mainly towards exploring the use of chopped (sisal) and textile (jute) composites
for different engineering applications including building while the present study examines
the suitability of abundantly available plant fibers such as sisal and jute in the presence of
otherwise harmful industrial waste like red mud for synthesizing polymer based composites.
Keywords : bauxite residue; plant fibre; polymer composites; engineering applications; sisal
and jute

1. Introduction
Alumina is produced worldwide from bauxite using the Bayer process. After digestion in
alkali, bauxite residue also known as red mud is separated as alkaline waste. The annual
production of the waste in Indian Alumina Plant is about 6 million tonnes per annum, while
the corresponding figure for world is ~120 million tonnes (Red mud project
http//www.redmud.org). The disposal of red mud requires large areas of land which may add
up in the cost of production of aluminum by 2-5%. Bauxite residue is the mixture of oxides
of iron, silicon, titanium, vanadium, calcium, and other minor metals. The current practice is
to store on land for future rehabilitation or use. The main environmental implications
associated with bauxite residue are high pH, minor and trace amount of heavy metals and
radio nuclides.
In the past decades, significant research in the world has been reported to utilized bauxite
244 TRAVAUX Vol. 36 (2011) No. 40

residue for environment benign applications such as building materials and for metal
recovery [Xu, 1996; Thakur and Sant, 1983; Tsakiridis et.al., 2004; Pontikes and
Angelopoulos, 2009]. In recent years, red mud has also been explored for gas cleaning,
waste water treatment and novel applications as a coagulant and adsorbent for water and gas
treatment as well as catalyst for some industrial processes. Red mud presents a promising
application in water treatment for removal of toxic heavy metals and metalloid ions,
inorganic anions such as nitrate, fluoride, phosphate and organics including dyes, phenolic
compounds and bacteria. In addition red mud can also be employed as catalysts for
hydrogenation, hydro dechlorination and hydrocarbon oxidation. Moreover, leaching and
eco-toxicological test indicate that red mud does not present high toxicity to the environment
before and after reuse [Wang et.al, 2008]. Following years of diligent research, scientists at
Alcoa Western Australia have developed an effective way to reduce the alkalinity of the
waste mud by capturing simultaneously carbon dioxide that would otherwise contribute to
global warming. Also, potential uses for the red mud residue, including brick and tile
making, in fertilizer, as a filler in plastics or concrete and as a replacement for construction
sand. The waste might even find a role as a soil amendment to help retain nutrients [Cooling,
2005]. A novel process has been reported for making radio opaque materials using bauxite
red mud and barium compound by ceramic processing route using phosphate bonding
[Amritphale et.al., 2007].
Plasma sprayed coatings of red mud have been developed at different operating power levels
of the plasma gun on aluminium and copper substrate as a value added utilization of this
industrial waste may be suitable for wear resistant applications [Satapathy et.al., 2006].
Reviews on this subject have also been published. (http://www.redmud.org/Applications
.html). Leading research organizations of world are putting extensive efforts for development
of techno-economical viable processes for utilization of bauxite residue
(http://bauxite2aluminium.blogspot.com/). The use of red mud in making value added
products by developing red mud polymer composites with an objective of waste to wealth
is discussed in the present paper.
The synthesis and use of composites usually prepared using glass, carbon and other synthetic
fibres are considered critical because of the environmental consciousness. Benefits of plant
fibres over synthetic reinforcing fibres are low cost, low density, acceptable specific
strength, easy extraction, carbon dioxide sequestration and bio-degradability [Bledzki and
Gassan, 1999; Mohanty et.al., 2000; Mohanty et.al., 2001]. The major drawback associated
with the plant fibers is their hydrophilic property and lack of good interfacial adhesion
between the fibre and polymer matrix (hydrophobic). However to improve interfacial
bonding between the fibre and matrix many efforts have been made by modifying the fibre
surface either by physical or chemical treatments and gained considerable success [Li
et.al.,2000; Rong et.al., 2001; Singh et.al., 1996; Nair and Thomas, 2003; Joseph et.al., 1996;
Saxena et.al., 2011]. The plant fibres such as jute, sisal, coir, banana, flax and ramie are
available in different parts of the world. Physico-chemical, mechanical and structural
properties of these plant fibres depend on the source and age of the plant, cellulose content
and microfibriller angle [Bledzki et.al., 1999; Pavithran et.al.,1991].
Also, it is reported that use of plant fibre reinforced composites as reinforcement in polymer
Mohini Saxena : Development of natural fibre reinforced polymer composites 245

matrix with a view to replace more expensive and non-renewable synthetic fibres, such as
glass, can reduce the material cost and at the same time yield high strength- to- weight ratio.
[Bledzki et.al., 1999; Bledzki et.al., 2001; Munikenche et.al., 1999; Lim et.al., 2003; Mathur,
2006]. The scope for substituting jute and sisal fibres in place of glass fibres as
reinforcement in composites is due to the higher specific modulus and lower specific gravity
of jute and sisal [Roe and Ansell, 1985]. Besides, much lower cost and renewable nature of
jute and sisal, requirement of less energy for their production and processing make them
more attractive as reinforcement in polyester based composites [Bowen, I981].
Available information indicates that limited work has been carried out to synthesize polymer
matrix composite materials and value added products thereafter using the industrial wastes
like red mud (bauxite residue) and plant fibres [Saxena et.al., 2008]. Moreover, the related
information exists in scattered form and a systematic study is yet to be carried out in order to
assess the properties and the performance capability of the synthesized material systems.
In view of the above, polymer based composites have been synthesized with different
combinations of the pre-characterised red mud and/or the plant fibres (as fillers/
reinforcements). Relevant engineering properties of the composites have also been
characterised with a view to use them as alternative to glass fibre reinforced composite, as
value added products in building construction, such as doors, roofing sheets, partition walls,
tiles to reduce environmental pollution and deforestation. Relevant characteristics of
conventionally used building materials have also been compared in order to assess the
application potential of the developed composites.

2. Experimental Methodology
Characterization of polymer matrix and the reinforcements
Indigenously available sisal and jute fibres were reinforced with a thermoset polyester
polymer matrix in the woven form along with red mud particles. The red mud was
characterised using wet chemical analysis to determine its chemical composition. Phase
identification was carried out by X-ray diffraction technique using a Philips diffractometer
(PW 1710). Jute fibres were extracted from the stem of Corchorus capsularis plant by water
retting method. Sisal fibre was mechanically extracted from the leaves of the sisal plant
(Agave sisalana). In this study, jute and sisal woven clothes with fibre contents of 300g/m2
and 204g/m2 respectively were used after treating with fire retardant materials. In the present
study, polyester resin (Acrolite 572) of fire retardant grade was used for preparing the
composites. In order to accelerate the polymerisation process, cobalt naphthonate (2-5%) and
methyl ethyl ketone peroxide (mekp) (2-5%) as catalyst was used.
Composite preparation
The composite materials were synthesised by mixing the red mud dispersoid phase in the
(liquid) polymer with the help of a mechanical stirrer. The composites in sheet form were
prepared using jute and sisal cloth after fire retardant treatment as reinforcement in polymer
matrix along with curing catalysts. The laminates were prepared in suitable moulds and
pressed at a pressure of 0.5 MPa for one hour at room temperature and post cured in an oven
at 80 C for 24 hours. A schematic representation of different steps involved in synthesising
246 TRAVAUX Vol. 36 (2011) No. 40

the composites is discussed in detail elsewhere [Saxena and Mishra, 2004]. Table 1 shows
the composition of the composites.
Table 1. Composition (wt %) of the Composites
Composite Material Matrix Reinforcement
Polyester resin Red mud Sisal fabric
Red mud-sisal fabric-polymer
35 50 15
Polyester resin Red mud Jute fabric
Red mud-jute fabric-polymer
35 50 15
3. Property characterization of the composites
Physical and mechanical properties
Physical and mechanical property characterisation of the composite materials was done
according to ASTM D792-91 (Density), ASTM D571-88 (Water absorption), ASTM D790-
92 (Flexural strength), ASTM D638-91 (Tensile strength). The tensile and flexural strengths
of the specimens were measured at a cross head speed of 5mm /min using universal testing
machine (Instron 1185, England).
Abrasion resistance
Abrasion tests were conducted using Suga Abrasion Tester, Japan following procedures
given in ASTM D 1242-92. All the tests were carried out at a fixed load (650gms) and
sliding distance (25.6 meters). Water proof emery paper containing 50 micron SiC particles
was used as the abrasive medium.
Impact strength
Various samples of the matrix polymer and composites were prepared in required size
(10mm x 10mm x 65mm) and their impact strength was measured using an impact tester
(CEAST, Italy). This test (IZOD -type) was conducted on notched samples following ASTM
D256-92.
Weathering
Accelerated weathering studies were carried out as per ASTM G-26-92 using a
Weatherometer (Atlas, ES 25, US). The composites reinforced with sisal/jute fibres were
exposed to ultra violet radiation, water spray and humidity.
Fire behaviour characteristics
Fire retardance/ resistance tests were conducted to measure various properties like non-
combustibility (IS: 3808 1979), Ignitibility (BS 476 : part 5-1968), fire propagation index
(BS 476: part 6-1981), surface spread of flame (BS 476: part 7-1981), and maximum specific
optical density (flaming and non flaming) as per procedures given in ASTM E 662-79.
Microstructure
Microstructural studies and analysis of dispersoid phase particles were carried out using
scanning electron microscope (JEOL 35, Japan). The samples were cold mounted in
Mohini Saxena : Development of natural fibre reinforced polymer composites 247

polyester resin and polished according to standard metallographic techniques. Morphology

of the red mud particles and interfacial bonding of jute/ sisal fibres with the polymer matrix
were studied. The fractured surfaces were also examined to understand the fibre fracture and
interfacial adhesion.

4. Results and discussion

The chemical composition and phases present in the red mud is shown in Table 2
respectively. X-ray diffraction of red mud showed the presence of Gibbsite [Al(OH3)],
Haematite (Fe2O3), Anatase (TiO2) and Calcite (CaCO3) as the major phases. Additionally, it
contains boehmite (AlO.OH), goethite [-FeO(OH)], Acmite/ Calcian [(NaCa) FeSiO2 O6]
[Saxena et.al.2008].
Table 2. Chemical Composition (wt.%) of Plant Fibre (Jute & Sisal) and
Industrial Waste (Red mud) Reinforcements
S.No Constituent Jute Sisal Constituents Red Mud
1. Cellulose 82.50 78 Fe2O3 62.7
2. Hemicelluloses - 10 Al2O3 15.0
3. Lignin 11.30 8 TiO2 3.0
4. Fat & Wax 0.64 2 SiO2 6.50
5. Pectin - 0.9 Na2O 4.80
6. Nitrogenous substances 1.50 - CaO 0.20
7. Ash 1.20 1 MgO -
8. Miscellaneous 2.86 - K2O -
9. Moisture absorption 6-9 3-7 Loss on ignition 7.10
SEM micrograph of as received red mud powder is shown in Fig. 2(a,b). The figures reveal
that in general the particles were of size less than 60 microns. The shape of the reinforcement
particles varied from spherical (Fig.2a) to angular (Fig.2b). The chemical composition and
properties of both the fibres are shown in Table-2. Cellulose and lignin were noted to be the
main constituents present in jute and sisal fibre. The cellular structure of jute and sisal fibre
can be seen in Fig. 2(c) & (d) respectively.
The microstructural features of the polymer composites reinforced with red mud particles are
revealed in Fig.3. The red mud particles were observed to be uniformly distributed in the
polymer matrix as shown in Fig.3(a). The cross section of red mud polymer composites
reinforced with jute fabric is shown in Fig.3(b)&(c). The presence of red mud particles along
with cellular structure of the fibres can be seen in the Fig.3(c) (regions marked by double
arrow and C respectively). The dispersoid / matrix interface was sound.
Properties of the red mud polymer composites reinforced with jute/ sisal fibre are shown in
Table-3. It is noticed that the developed composite materials showed significantly improved
mechanical strength. Moreover, the degree of water absorption and (adverse) effect of
weathering has been minimal in the case of the developed composites.
248 TRAVAUX Vol. 36 (2011) No. 40

(a)
(b)

(c) (d)
Fig 2. SEM micrographs of (a&b) red mud particles, (c) sisal and (d) jute fibre before
reinforcement in the polymer
Table 3. Properties of the red mud polymer composites reinforced with jute/ sisal fibre
Red mud jute fibre Red mud sisal fibre
S.No. Properties Unit
polymer composite polymer composite
1. Density gm/cm3 1.72-1.76 1.60-1.64
2. Moisture content % 0.20-0.38 0.48-0.56
3. Modulus of rupture N/mm2 85.00-95.00 78.00-88.00
4. Tensile strength N/mm2 22.00-24.00 18.00-23.00
Compressive strength
5. N/mm2 78.48-101.00 70.00-95.00
perpendicular to surface
Compressive strength parallel
6. N/mm2 44.00-51.00 42.00-50.00
to surface
Water absorption
7. 2 hours % 0.15-0.40 0.20-0.35
24 hours % 1.10-1.50 1.15-1.40
Swelling water
Length % 0.00-0.36 0.00-0.48
8.
Width % 0.00-0.47 0.00-0.62
Thickness % 0.00-1.38 0.00-1.30
Self extinguishing Self extinguishing
9. Fire retardency Second
within 15 second within 20 second
Mohini Saxena : Development of natural fibre reinforced polymer composites 249

(a)

(b) (c)

Fig 3. SEM micrographs of the polymer composites containing (a) red mud (b&c) jute
fibre + red mud particles [ : Red mud particles, C : Jute fibre]
Table-4 shows a comparison of typical properties of the developed composites vis--vis their
conventional (wood) counterparts. It may be noted that the density of the composites varied
over a (narrow) range of 1.60 to 1.76 gm/cc as compared to 0.50 to 0.62 gm/cc of the wood
(like teak) and its products such as partitions, boards, (made of ply board, rice husk board,
medium density fibre board etc.) [Sood et.al., 1994]. The moisture content of the composites
was noted to be 0.20 to 0.50% as against 5 to 15% in the case of wood and its products.
Similarly, water absorption was found to lie in the range of 1.10 to 1.50% after 24hrs of
soaking in water. The extent of absorption of water in the wood was much higher (12-20%)
than that of the composites making the so developed composites more durable. The extent of
swelling in water of the composites varied between 0.36 to 1.78%. Out of this little amount
of water absorption, the maximum share is contributed by the jute and sisal fibres because
polyester reinforced only with red mud showed very little water absorption as reported
elsewhere [Saxena and Khazanchi, 1992; Saxena and Morchhale, 1993; Mayer, 1993]. The
range of the swelling for the woods was significantly higher than the composites. Resistance
of the composites to burning (firing) was also much improved over the conventional wood
material. Interestingly, the composites were observed to be self extinguishing (within 1522
second) in nature. Fire ignitability behaviour of red mud polymer composites indicate that
these are not easily ignitable. The fire propagation index shows that red mud composites are
250 TRAVAUX Vol. 36 (2011) No. 40

better in comparison with medium density fibre board (MDF), expanded polystyrene (EPS)
and wood. It is due to the combined effect of fire retardant additives and industrial wastes
such as red mud [Saxena and Asokan, 2010 ].
Resistance to chemical attack and weathering was much better in the case of the composites
than the wood. Mechanical properties of the developed composite materials were
significantly superior to wood wherein nearly 6-9 time improvement in the modulus of
rupture, 5-40 times increase in tensile strength and 8-10 times higher compressive strength
was exhibited by the composites over wood and wood products (Table 4). The fractured
surface of red mud polymer composite reinforced with jute shows particles and fibres in
position {Fig.4 (a&b)}. This is an indication of good wetting and adhesion between
reinforcement phases (jute and red mud and polyester resin matrix. Instead of pull out of
fibres, broken ends of fibres are seen in the micrographs affirms a better interfacial bond
(Fig.4 a). Good bonding was also found in the case of red mud containing composites
reinforced with either jute or sisal as well (Fig. 3 b&c). Here the red mud particles occupied
the micro pores of the cellular structure of jute and sisal thereby preventing void formation.
Thus the composites developed in this study attained much improved physical and
mechanical properties (except density) as compared to those of their conventional (wood)
counterparts. However, the specific strength was still better than teak and other agro-waste
materials.
Table 4. Comparison of typical properties of the developed Composites with
conventional building materials
Conventional materials
S. Developed
Test Conducted MDF MDF Particle Teak
No composites PVC
(EG) (IG) Board Wood
1.30- 0.50-
1. Density, gm/cm3 1.60-1.76 0.5-0.9 0.5-0.9 0.62
1.58 0.90
0.50-
2. Moisture content, % 0.20-0.56 - 5-25 5-25 11.00
15.0
Modulus of rupture, 68- 12.50- 12.50- 12.50- 13.00
3. 78.00-95.00
N/mm2 110 15.50 15.50 15.00
Tensile strength, 0.60- 0.60- 0.40- 4.00
4. 18-24 -
N/mm2 0.70 0.70 0.45
Compressive Strength
5. perpendicular to 70-101 55.90 - - - 8.80
surface, N/mm2
Compressive Strength
6. parallel to surface, 40-51 55.90 - - - -
N/mm2
Water Absorption 0.04- 12.00- 17.00- 17.00- 10.0-
7. 1.10-1.50
24 hours, % 0.4 13.00 18.00 20.00 20.0
Mohini Saxena : Development of natural fibre reinforced polymer composites 251

(a) (b)
Fig 4. SEM micrographs of fractured surfaces of polymer composites
containing (a&b) red mud particles reinforced with sisal fibres
Abrasive wear rate and impact strength of various combinations of polyester, red mud,
chopped and woven sisal fabric are studied. The addition of red mud reduced the abrasion
rate of polyester matrix. Better abrasion resistance of red mud composite than the polymer
alone could be attributed to the protection offered to the softer matrix by the hard red mud
particles [Nielson, 1974; Saxena et.al., 2008].
The accelerated weathering studies showed better performance of red mud polymer
composites as compared to the composites without red mud. Visually no change was
observed even after a period of 1500hrs exposure. The improved behaviour may be due to
the highly stabilising ceramic oxides present in red mud. The oxides restricted the
disintegration due to ultraviolet radiation.
An appraisal of the above clearly suggests that polymer matrix composites so developed in
the present study by using industrial wastes bauxite residue (red mud) and (abundantly
available) plant fibres as reinforcement/ fillers are potential value added products for
building applications. This becomes beneficial from two stand points, namely, environmental
protection through the meaningful use of the largely accumulating industrial wastes and
development of value added products using naturally available fibres (jute and sisal) and
industrial wastes like red mud. A few prototype alternative building products (i.e. door
shutters, roofing sheets, tiles, partition walls etc.) were developed in order to assess their
performance in service.

5. Conclusion
Plant fibre composites with industrial wastes present immense opportunities to play an
increasing role as alternative engineering materials. Jute/ sisal reinforced polymer
composites with red mud show better physical, chemical, mechanical, weathering and fire
resistance properties than conventional materials including wood and wood substitutes. Their
durability and strength make them a more promising value added building products. The
developed red mud- plant fibre reinforced polymer is a versatile material and can be used for
applications like partitioning, false ceiling, roofings, panels, floorings, wall tiles, furnitures
252 TRAVAUX Vol. 36 (2011) No. 40

etc. It can also be used in prefabricated housing, shades/ shelter, instant houses. There is a
growing global demand for products such as composite doors and panels. So, while the
forest cover is limited, the potential for composite doors and panels is virtually unlimited.
This composite is an ecofriendly material because it helps environment in two ways: firstly
by helping to prevent further deforestation and secondly by effectively using waste products
and in the process reducing pollution hazards.

6. Acknowledgements
The author is grateful to all the scientific and technical staff of AMPRI, Bhopal for rendering
necessary technical support in the present study. The most of the research work was carried
out with the support of BMTPC, MOEF, NALCO, TIFAC, DST and CSIR is thankfully
acknowledged.

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