PREPARATION OF LDPE-BLEACHED & GRAFTED PULQUE

FIBER COMPOSITE AND ITS PHYSICOCHEMICAL

PROPERTIES

Shamim-Ara Pervin, Ayesha Akther Zaman and M. Maniruzzaman

Department Applied Chemistry and Chemical Technology
Islamic University, Kushtia # 7003, Bangladesh

Submitted to Indian Journal of Fibre and Textile Research

Manuscript: Regular Articles

*To whom correspondence should be addressed.

Dr. M. Maniruzzaman

Associate Professor
Department Applied Chemistry and Chemical Technology
Islamic University, Kushtia # 7003, Bangladesh
Tel: +880-71-53029 Ext. 2455 Fax: +880-71-54400 e-mail:manir@kushtia.com
 PREPARATION OF LDPE-BLEACHED & GRAFTED PULQUE FIBER
COMPOSITE AND DEETEMINATION OF ITS PHYSICOCHEMICAL
PROPERTIES

SHAMIM-ARA PERVIN, M. MANIRUZZAMAN,

Department of Applied Chemistry and Chemical Technology, Islamic
University, Kushtia-7003, Bangladesh

ABSTRACT

A simple hot press molding process was used to produce LDPE-Pulque

fiber reinforced composites using LDPE (Low density polyethylene) and
Pulque fiber (raw, bleached and grafted with HEMA) varying the amount
of fiber and LDPE. Various physical and mechanical properties were
measured. The physical properties i.e., density is higher for composites of
grafted fiber than that of raw and bleached fiber. Water absorption and
moisture content are higher for composites of bleached fiber. The tensile
properties i.e., stress-strain curve and UTS are high for composites of
bleached fiber and increase with fiber addition to a maximum then
decreases or remains more or less constant. The flexural properties (
flexural strength, tangent modulus and flexural strain) of composites of
bleached fiber is higher than that of raw and grafted fiber composites and
these properties increase with the increase of fiber content to a maximum
and then decrease or remains fairly constant.
INTRODUCTION

Materials property combinations and ranges have been, and are being,
extended by the development of composite materials. . Composite
materials represent nothing but a giant step in the ever-constant endeavor
of optimization in materials. Strictly speaking, the idea of the composite
is not a new or recent one. Nature is full of example wherein the idea of
composite is used. The coconut, plum leaf is nothing but a cantilever
using the concept of fiber reinforcement. Wood is fibrous composite;
cellulose fiber in lignin matrix. The cellulose fibers have high tensile
strength but are very flexible. While the lignin matrix joins the fiber
furnishes the stiffness. Natural fibers are a promising reinforcement to
use in thermoplastic composites due to their low density and excellent
mechanical properties. Further more the natural fibers such as sisal, jute
hemp and flax are relatively cheap and obtained from renewable
resources.1

For the manufacturing of reinforced composite materials, factors such as

fiber content, fiber diameter, fiber length, void content matrix properties,
fiber-matrix bonding, fiber orientation and fiber properties are very
important as they determine the final properties of the natural fiber
reinforced composite components.2Composite is used to facilitate the use
of its constituent materials. Main constituent of our composite is LDPE
(Low density polyethylene) with the addition of chemically modified
sisal fiber composite, which is strong and improved in quality than
LDPE. The composite may be used as roofing materials, as well as for
partition and other commercial and domestic uses.2

Incorporation with a natural fiber (sisal fiber), the polymeric matrix

LDPE made our sample product. Heat and press molding process was
used which is a very low cost process than the other process for
fabrication of composite. Here the temperature and pressure are the two
main parameters for the fabrication and the others are cooling time,
additional pressure and retention time. Here the main drawback is
consumption of long time. The density of sisal fiber is greater than
matrix. Through changing the parameters of the fabrication, optimum
condition for operation was decided, for the desired composite product.
The intention of this thesis work is to achieve a natural fiber reinforced
composite with high mechanical properties using chemically modified
short Agave Atroverance fiber as reinforcement and a Low density Poly
Ethylene (LDPE) as a polymer matrix.3

Experimental

For composite preparation the chief raw materials used are LDPE,
collected from local market and Agave Atroverance, are collected from
rural area.Untreated (raw) light brown Agave Atroverance fiber,
bleached pulque fiber and 2-Hydroxy ethylmethacrylate (HEMA)
modified or grafted pulque fibers were used as reinforcement agent. In
the thesis work no coupling agent is used.
The samples were prepared by several steps such as pulque fiber cutting
(to get sized pulque bundles were cut into different length of 2-3 mm,
average, with its help of a knife) the sized pulque were manually agitated
to make the pulque fiber loose with each other. This pulque kept at a dry
environment for seven days for the partial removal of moisture. The
samples were prepared by mixing, casting, curing and controlling,
cooling and demolding.
To evaluate the properties of prepared composite the following tests are
performed –
1. Measurement of bulk density
2. Water intake/Water absorption
 3. Tensile strength testing
4. Flexural testing
The samples were prepared by Weber Pressen Hydraulic Press Machine
and the samples were tested by UTM Machine (Hounsfield test
equipment).

Bulk Density Calculation:4

D = Ws / V

Where, D = Density of the specimen, Kg/m3

Ws = Weight of the specimen, Kg, and
V = Volume of the specimen, m3.
Water absorption /Water in take:5 The total water absorption was
calculated following the rules given below.
1. Increase in weight, %Wi = Ww-Wc ÷Wc×100
2. Soluble matter lost, %Ws = Wc-Wrc ÷Wc×100
3. % water absorbed, W= Wi + Ws
In all cases a protective gel coat (araldite) was applied on the cut sides to
prevent penetretion of water from cut sides.
Tensile Strength (i):
Tensile specimen was prepared according to ASTM Method.
The test speed was 1mm/min.
Applied load
Tensile Strength6 = Cross sectional area of the load bearing area

P
6 = A

P KN
= A . mm2
P N
= 103 A . mm2

P N
= 103 A . 10-6m2

P N
= 103 A . m2 X 106

P
= 103 A . Pa X 106
 P
= 103 A . M Pa

Tensile strain (ii): Tensile strain is calculated according to

ASTM D-638M - 91a.

Tensile strain = Extension

25

Flexural Strength7 (i):

Flexural specimen was prepared according to ASTM D790M, 3 point
loading. The specimen dimension was 125 x 10 x 6-8 mm and support
span was 96 mm. The test speed was taken as 2 mm/min. The strength
may be calculated for any point of the load deflection by means of the
following equation-

S = 3PL / 2BD2
Where,
S = stress in the outer fibers at midspan, MPa,
P = load at a given point on the load – deflection curve, N,
L = support span, mm,
B = width of specimen tested, mm,
D = depth of tested specimen, mm.

In this way the flexural strength of each sample is measured

Flexural Strain (ii):

Flexural specimen was prepared according to ASTM D790M, 3 point loading. The
specimen dimension was 125 x 10 x 6-8 mm and support span was 96 mm. The test
speed was taken as 2 mm/min. It may be able to be calculated for any deflection using
the following equation-
εf = 6Dd / L2
Where,
εf = Main strain in the outer surface, mm/mm
D = Maximum deflection of the center of the beam, mm
L = Support span, mm.
d = Depth, mm.
Tangent Modulus (iii): To determine the Tangent Modulus at first the slope is
calculated from the load deflection curve. If
Sloe = K
 Span = L
Width = b
Thickness =D
Tangent Modulus = KL3/4bD3

Results and Discussion

Physical Properties:

1
0.98
0.96
0.94
Density/gm/cc

0.92
0.9
0.88
Grafted
0.86 Bleached
0.84 Raw
0.82
0.8
0 5 10 15 20 25
Fiber Content/%

Fig. 1: Effect of fiber addition on density for LDPE-pulque or Agave atroverance

fiber composite for raw, bleached and grafted fiber.
Figure 1 shows the effect of fiber addition on density for LDPE-pulque fiber
composite for different types of fiber as mentioned above. The curve shows that the
density increases with the fiber addition and it increases up to 20% of fiber addition. It
is seen that the density is high for grafted fiber and lower for raw fiber and the
bleached fiber attain the medium value.
The relationships derived for different fiber are:
Density = 0.92+0.0001(% of raw fiber),
Density = 0.92+0.0002(% of bleached fiber)
Density = 0.92+0.0014 (% of grafted fiber)

Grafted fiber shows highest slope and raw fiber shows the lowest slope. From the data
it is concluded that the slope is high for grafted fiber than for bleached and raw fiber.
 15

Grafted
Bleached
Water Absorption/%
Raw
10

0
0 100 200 300 400
Time/hrs

Fig. 2 : Effect of immersion time on Water Absorption (WA) of LDPE-various

types of such as raw, bleached and grafted Agave atroverance (pulque) fiber
reinforced composites for 20 % of fiber addition.
Fig. 2 shows the effect of immersion time on water absorption of raw, bleached and
grafted or 2-Hydroxy ethyl methacrylate(HEMA) modified fiber reinforced LDPE
composites for 20% of fiber addition. It reveals that the water absorption depends on
fiber addition and immersion of time. It can be seen that the percentage of water
absorption for all percent of fiber addition increases with time as it is a diffusion
phenomenon. Water absorption is responsible only for fiber addition and higher the
fiber addition higher will be the water intake .The figure shows that the % of water
absorption increases initially slowly and with increases of time it increases rapidly.
The figure shows that the % of water absorption is high for grafted fiber, medium for
bleached fiber and low for raw fiber.

Mechanical properties :
Tensile Properties:
The tensile properties of a material shown by the stress-strain curve.
 14 5% fiber
10% fiber
12
20% fiber
10
Stress/Mpa

0
0 0.2 0.4 0.6
Strain/mm/mm

Fig.1: Stress-strain curve(Tensile) for LDPE-raw Agave atroverance (pulque)

fiber composite (% of fiber loading).

14

12

10
Stress/Mpa

6 5% fiber
10% fiber
4
20% fiber
2
15% fiber
0
0 0.1 0.2 0.3 0.4 0.5
Strain/mm/mm

Fig.2: Stress-strain curve for LDPE-bleached Agave Atroverance (pulque) fiber

composite (% of fiber loading).
 14 5% fiber

12 10% fiber

10 15% fiber
Stress/Mpa

0
0 0.1 0.2 0.3 0.4 0.5
Strain/mm/mm

Fig.3: Stress-strain curve(Tensile) for LDPE- grafted or 2-Hydroxy ethyl

methacrylate (HEMA) modified Agave atroverance (pulque) fiber composite (%
of fiber loading).

Figure 1,2 and 3 shows the Stress-strain curve(Tensile) for LDPE-raw, bleached and
grafted pulque fiber composite (% of fiber loading). The tensile properties of a
material are shown by stress-strain curve. Here stress increases with the increase of
strain. It reaches maximum and after that the stress falls down. The curves have two
regions- one is the elastic region and another is plastic region. Initial region is the
elastic region and after that samples deform plastic area. The figure shows that higher
the percentages of fiber loading higher the maximum stresses (UTS) and lower the
strain. That is with the increase of fiber addition the maximum stress (UTS) increases
but ductility of composite decreases.

UTS (Ultimate Tensile Strength):The strength of a material is the tensile stress

under which it ruptures.
 12

10

8
UTS(MPa)

6
Raw
4
Bleached
Grafted
2

0
0% 5% 10% 15% 20% 25%
Fiber Content/%
Fig.4: Effect of fiber addition on Ultimate Tensile Strength for LDPE- raw,
bleached and grafted Agave atroverance (pulque) fiber reinforced composite.

Figure 4 shows the effect of fiber addition on Ultimate Tensile Strength for LDPE-
raw, bleached and grafted pulque fiber reinforced composite. Here the curves shows
that the tensile strength is maximum at every treatment for 10% loaded fiber
composite. But untreated fiber shows that the tensile strength decreases with the fiber
loading. Ultimate tensile strength is higher for LDPE-bleached pulque fiber reinforced
composite because of better bonding between fiber and matrix. For grafted fiber
composite the strength is less than bleached fiber but higher than raw fiber. It means
that the fiber matrix bonding increases for bleached fiber and simultaneously for
grafted fiber and treated fiber matrix bonding is much better than raw one.

Flexural Properties:
The stress required to rupture a material under flexure is its flexural strength.
 10

8
Flexural Strength/MPa

4
Grafted

2 Bleached
Raw

0
0% 5% 10% 15% 20% 25%
Fiber Content/%

Fig.1: Effect of fiber addition on Flexural Strength for LDPE-raw, bleaced and
grafted Agave atroverance fiber reinforced composite.

Figure 1 shows the effect of fiber addition on Flexural Strength for LDPE-raw,
bleached and grafted pulque fiber reinforced composite. It reveals that the flexural
strength increases with the increase of fiber addition up to certain percentage of
addition fiber (10%), the strength is always higher for bleached than that for raw and
grafted fiber.
For 0% fiber the polymer strength was obtained 6.92 MPa. Up to 10% fiber addition
both the fiber and matrix bear the load and make resistance to slip as in the case of
age hardening of metals. Up to 10% the short fibers are finely distributed and the
interfacial bonding between the fiber and matrix is high, after that fibers are present as
bundle of fibers and fiber-fiber bonding strength is lesser and the interfacial bonding
between the fiber and matrix is poor. After that the fiber are coagulated as bundle of
fibers, bundle of fibers fractured during load to slips and does not make resistance to
slips. Moreover, these also act as stress concentrator. Consequently, after 10% fiber
addition the flexural strength decreases. Similar effect was found by Rashed and
Rizvi8, Shabname Ele9,Bipasha Bose10 Asad 11.
 8

Flexural Strain/mm/mm
6

Raw
2
Bleached
Grafted
0
0% 5% 10% 15% 20% 25%
Fiber Content/%

Fig.2: Effect of fiber addition on flexural strain for LDPE-raw, bleached and
grafted Agave atroverance (pulque) fiber reinforced composite.

The effect of fiber addition on flexural strain of LDPE-raw, bleached and grafted
pulque fiber reinforced composites is shown in figure2. It reveals that the flexural
strain of fabricated product decreases continuously with the increase of fiber addition.

It is apparent that the elongation decreases very slightly with the increasing of fiber
content. The presence of fiber restricts the slip resulting in lesser ductility and
consequently the % of elongation decreases continuously with the increase of fiber
addition. Strain is lesser for bleached fiber than that for raw and grafted fiber. Similar
effect was found by Shabname Ele9, Asad 11.

Conclusions
Our research work was conducted to make this type of (house wares, toys, and
containers, lids, and closures, power coating, pipe, window and door, roofing in the
developing countries, automobiles body etc.) high performance application materials,
from low-density polyethylene and polypropylene reinforced with Agave Atroverance
fiber. One of the most important objectives of our research work is to use Agave
atroverance fibre, which is biodegradable. So, a definite amount of low-density
polyethylene and polypropylene could be replaced by the Agave Atroverance fiber,
which is very important to our environment. After use of the product manufacture by
LDPE and pp reinforced by natural fiber rotten a certain percentage when goes to the
environment. So, in the respect of our risky environment, it is suitable to use this type
of composite materials, produced with polymer, which is reinforced by natural fibers
such as Agave Atroverance. From this experiment it is concluded that the tensile and
flexural properties of bleached pulque fiber composite is higher than that of raw and
grafted fiber composite.
Reference:

1. Joseph, K.; Mattoso, L.H.C. et. al., Natural Fiber Reinforced Thermoplastic
Composites. Nat. Polymer Agro Fibers Based Composites. 159-20 (Eng), 2000.

2. http://as.wiley.com/WileyCDA/WileyTitle/productCd-0471873578.html

3. Joseph, K., Thomas, S., Pavithran C.; Composite Science and Technology; 53:99-110,
1995.

4. ASTM Designation; C 134-76, Standard Test Method for Size and Bulk Density of
Refractory Brick and Insulating Firebrick.

5. ASTM (Reapproved 1988) Designation; D 570-81; Standard Test Method for Water
Absorption of Plastic.

6. ASTM Designation; D 638-98, Standard Test Method for Tensile Properties of

Plastics.

7. ASTM (Reapproved 1991), Designation; F 417-78, Standard Test Method For Flexural
Strength (Modulus Of Rupture) Of Electronic- Grade Ceramics.

8. Lunt JM, Shortall JB "The Effect of Extrusion Compounding on Fiber Degradation&

Strength Properties in Short Glass Reinforced Nylon-66, Plastic & Rubber
Processing", 108-14, Sept 1979 .

9. Castle JE, Watts JF The Study of Interfaces in Composite Materials by Surface

Analytical Techniques, In Brewis DM, Briggs D (Eds) Industrial Adhesion Problems,
Orbital Press, Oxford, 1985.

10. TheMetal Cladding & Roofing Manufacturers Association.The Steel Construction

Institute 2003 MCRMA Technical Paper No. 15,SCI Publication No. P327,

11. Baer, M., Composites obtained by encapsulation and collimation of glass fibers within
a thermoplastic matrix by means of polymerization, J Appl. Polymer Sci , 19:
1323-36, 1975 .