Preparation and characterization of composite polyester

Prepared by: Mahmoud Mohamed

ID: 141761
ABSTRACT
In this experiment it was required perform mechanical tests on three samples of polyester. Three
samples of composite polyester were prepared in which the first sample consists of pure polyester
without filler while the second sample is a composite polyester based on calcium carbonate as a
filler, and finally the third sample is also a composite polyester, however, the filler of this sample
was sand. Moreover, the composite polyester samples were left for curing and hardening as well
as pouring the samples in the moulds for the mechanical testing. The samples were subjected for
the hardness, tension, compression, and bending tests and the results showed some variations as
well as unexpected values.

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CONTENTS
Abstract ........................................................................................................................................... 2

1 introduction ............................................................................................................................. 5

1.1 thermosets......................................................................................................................... 5

1.2 Thermoplastics ................................................................................................................. 5

1.3 Thermoplastics vs thermosets .......................................................................................... 6

1.4 Composite polymers ......................................................................................................... 7

1.4.1 Compositions ............................................................................................................ 7

1.4.2 Polymer composites .................................................................................................. 7

1.5 Fillers ................................................................................................................................ 8

2 Procedures and provided materials ......................................................................................... 9

2.1 Procedures ........................................................................................................................ 9

2.1.1 chemicals provided ................................................................................................... 9

2.1.2 Equipment provided .................................................................................................. 9

3 Results ................................................................................................................................... 10

3.1 Tension test .................................................................................................................... 10

3.2 Compression test ............................................................................................................ 12

3.3 Bending test .................................................................................................................... 15

3.4 Hardness test .................................................................................................................. 18

4 Discussion ............................................................................................................................. 19

4.1 Sources of error .............................................................................................................. 20

5 Conclusion ............................................................................................................................ 21

6 Bibliography ......................................................................................................................... 22

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List of figures

Figure 1 Thermoplastic and Thermoset models.............................................................................. 7

Figure 2 Stress vs Strain plot of pure sample ............................................................................... 10
Figure 3 Pure sample .................................................................................................................... 10
Figure 4 Stress vs strain plot for silica sample ............................................................................. 11
Figure 5 Silica Sample .................................................................................................................. 11
Figure 6 Stress-Strain plot pure sample (compression) ................................................................ 12
Figure 7 pure sample (compression) ............................................................................................. 12
Figure 8 Stress-Strain plot (Compression) .................................................................................... 13
Figure 9 Calcium Carbonate sample (compression) ..................................................................... 13
Figure 10 Stress-Strain plot (compression)................................................................................... 14
Figure 11 Silica Sample (Compression) ....................................................................................... 14

List of tables

Table 1 Thermoplastics vs Thermosets........................................................................................... 6

Table 2 Hardness test results......................................................................................................... 18
Table 3 Results summary .............................................................................................................. 19

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1 INTRODUCTION

1.1 THERMOSETS

Thermoplastics are used in many applications because of their lightweight, economic fabrication
and good chemical resistance. The dependence of the specific volume of thermoplastics on the
temperature and on the pressure results in significant local volumetric changes in the thermoplastic
as it cools during processing. The most important property of a thermoplastic with regard to
specification of the processing conditions is its viscosity. The viscosity of even a thermoplastic
varies with temperature and may also vary with the feed rate and local flow geometry.
(Subramanian, 2013)

Thermoplastics are classified into three major classes:

1. Those with carbon chain as skeleton. Examples are polyethylene (PE), polypropylene (PP),
polystyrene (PS), PMMA, PVC, etc.
2. Those containing hetero atoms such as nitrogen, sulfur, oxygen, etc., in addition to carbon
atoms. Examples are polyether, polyester, polyamide, etc.
3. Those with double bonds—plastics composed of higher molecular compounds. Examples are
polyacetylene, polyphenylene.

(Subramanian, 2013)

1.2 THERMOPLASTICS
Thermoset plastics contain polymers that cross-link together during the curing process to form an
irreversible chemical bond. The cross-linking process eliminates the risk of the product remelting
when heat is applied, making thermosets ideal for high-heat applications such as electronics and
appliances. Thermoset plastics significantly improve the material’s mechanical properties,
providing enhances chemical resistance, heat resistance and structural integrity. Thermoset plastics
are often used for sealed products due to their resistance to deformation. (Dasari, 2013)

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1.3 THERMOPLASTICS VS THERMOSETS
Table 1 Thermoplastics vs Thermosets

Thermoplastics Thermosets
soft Rigid
clear Opaque
High volume Low volume
Ease of productions Difficult processing
Higher temperature processing Lower temperature processing
Low production scrap High production scrap
Higher initial material cost Lower initial material cost
Lower total parts cost Higher total parts cost
High flow Low flow
Insulator Conductive
Higher impact strength Lower impact strength
Lower heat resistance Higher heat resistance
Higher creep Lower creep
Recyclable Not recyclable
Good electrical properties Excellent electrical properties
Examples: polyesters, polyurethanes, Examples: epoxies, unsaturated polyesters,
polyamides, polyethers aminoplastics

(Sastri, 2010)

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 Figure 1 Thermoplastic and Thermoset models
(Bobo, 2013)

1.4 COMPOSITE POLYMERS

Composites can be defined as materials that consist of two or more chemically and physically
different phases separated by a distinct interface. The different systems are combined judiciously
to achieve a system with more useful structural or functional properties non-attainable by any of
the constituent alone. (Jose, 2012)

1.4.1 Compositions
Composite material is a material composed of two or more distinct phases (matrix phase and
dispersed phase) and having bulk properties significantly different from those of any of the
constituents. Matrix phase is the primary phase having a continuous character. Matrix is usually
more ductile and less hard phase. It holds the dispersed phase and shares a load with it. Dispersed
(reinforcing) phase is embedded in the matrix in a discontinuous form. This secondary phase is
called the dispersed phase. Dispersed phase is usually stronger than the matrix, therefore, it is
sometimes called reinforcing phase. (Jose, 2012)

1.4.2 Polymer composites

Most commercially produced composites use a polymer matrix material often called a resin
solution. There are many different polymers available depending upon the starting raw ingredients.
There are several broad categories, each with numerous variations. The most common are known

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as polyester, vinyl ester, epoxy, phenolic, polyimide, polyamide, polypropylene, polyether ether
ketone (PEEK), and others. (Jose, 2012)

1.4.2.1 Characteristics of polymer composites

PMCs are very popular due to their low cost and simple fabrication methods. Use of nonreinforced
polymers as structure materials is limited by low level of their mechanical properties, namely
strength, modulus, and impact resistance. Reinforcement of polymers by strong fibrous network
permits fabrication of PMCs, which is characterized by high specific strength, high specific
stiffness, high fracture resistance, good abrasion resistance, good impact resistance, good corrosion
resistance, good fatigue resistance, low cost. On the other hand, the disadvantages of composite
polymers are, low thermal resistance, and high coefficient of thermal expansion. (Jose, 2012)

1.5 FILLERS
Fillers are solid inorganic or organic, natural or synthetic materials that are dispersed in polymers.
The shape of filler particles may be spheroidal, fibrous, or platelet-like. The chemical structure of
fillers is usually not important except for so-called active ones. Fillers are used in considerable
proportions in plastics, elastomers, fibers, papers, coatings, adhesives, etc. In thermoplastics, fillers
are used mainly in poly(vinyl chloride), it-poly(propylene), poly(ethylene), and polyamides and in
thermosetting polymers such as phenolic resins and unsaturated polyester resins. Inactive fillers
dilute expensive polymers without significantly changing their use properties. They reduce costs
and are therefore also called extenders. Active fillers improve certain mechanical properties. They
are therefore also known as reinforcing fillers, and for molding materials (compounds) as resin
binders. The activity of such fillers depends on the concentration and chemical structure of atomic
groups on particle surfaces. "Reinforcement" is not well defined: it may denote the in- crease of
tensile strength, notched impact strength, or flexural strength, or the decrease of abrasion. (Elias,
2009)

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2 PROCEDURES AND PROVIDED MATERIALS

2.1 PROCEDURES
1. Weigh 100gm of unsaturated polyester and place it in a 250ml beaker.
2. Add 1% of initiator benzoyl peroxide ,and stir precisely.
3. After all the benzoyl peroxide dissolves, add 0.2g of activator cobalt octoate and stir the
contents of the beaker.
4. Fill a dog-bone mould, a petri dish, full test tube, and one third of another test tube with
pure polyester.
5. Repeat steps 1-4 with 1% filler calcium carbonate added to the polyester.
6. Again, repeat steps 1-4 with 1% filler silica.
7. Leave the samples for about 1-5 hours for hardening
8. Perform mechanical tests
- Tension for dog-bone shaped samples.
- Compression for samples 1/3 of test tube shaped
- Bending for the sample shaped as full test tube.
- Hardness for petri dishes samples.

2.1.1 chemicals provided

1. Commercial unsaturated polyester.
2. Benzoyl peroxide initiator.
3. Cobalt octoate activator.
4. Calcium carbonate powder.
5. Silica.

2.1.2 Equipment provided

1. 3 250ml beakers.
2. 6 test tubes.
3. Sensitive balance.
4. Glass rods.
5. 3 Petri dishes.
6. Dog-bone moulds.
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3 RESULTS

3.1 TENSION TEST

Pure polyester results

Stress at which failure occurred = 15.91 𝑀𝑃𝑎

Force required for failure = 1.40 𝑘𝑁

Figure 2 Stress vs Strain plot of pure sample

Figure 3 Pure sample

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Polyester + silica results

Stress at which failure occurs = 31.50 𝑀𝑃𝑎

Force required for failure = 2.52 𝑘𝑁

Figure 4 Stress vs strain plot for silica sample

Figure 5 Silica Sample

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3.2 COMPRESSION TEST
Pure polyester results

Force required for failure =8.61 kN

Stress at which failure occurred = 48.6 𝑀𝑃𝑎

Figure 6 Stress-Strain plot of pure polyester (compression)

Figure 7 Pure polyester (compression)

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Calcium carbonate polyester results

Force required for failure = 4.05 𝑘𝑁

Stress at which failure occurred = 22.9 𝑀𝑃𝑎

Figure 8 Stress-Strain plot of calcium carbonate polyester (Compression)

Figure 9 Calcium Carbonate polyester (compression)

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Silica polyester results

Force required for failure = 6.82𝑘𝑁

Stress at which failure occurred = 38.5𝑀𝑃𝑎

Figure 10 Stress-Strain plot of silica polyester (compression)

Figure 11 Silica polyester (Compression)

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3.3 BENDING TEST
Pure polyester results

Force required for failure = 1.3 𝑘𝑁

Stress at which failure occurred = 12.9 𝑀𝑃𝑎

Energy needed for failure = 5.804 𝐽

Figure 12 Stress-Strain plot pure polyester (bending)

Figure 13 Pure polyester (bending)

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Calcium carbonate polyester results

Stress at which failure occurred = 11.750 𝑀𝑃𝑎

Force required for failure = 1.18𝑘𝑁

Energy needed for failure= 3.920 𝐽

Figure 14 Stress-Strain plot of calcium carbonate polyester (bending)

Figure 15 Calcium Carbonate polyester (Bending)

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Silica polyester results

Stress at which failure occurred = 6.3 𝑀𝑃𝑎

Force required for failure = 0.63 𝑘𝑁

Energy needed for failure = 0.957 𝐽

Figure 16 Stress-Strain plot of Silica polyester (bending)

Figure 17 Silica Sample (Bending)

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3.4 HARDNESS TEST
Samples were tested at different regions and the average of the outputs was taken.

Table 2 Hardness test results

MEASUREMENT’S 1 2 3 4 5 AVERAGE
NUMBER
PURE SAMPLE 96 90 94 94 93 93.4
CALCIUM- 92.5 93 91 92 91 91.9
CARBONATE SAMPLE
SILICA SAMPLE 94 92 90 94 90 92

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4 DISCUSSION
The results of the mechanical tests showed some variations in the properties of the prepared
samples of polyesters. Starting with the tensile test, the silica filled polyseter required higher stress
for failure while the pure polyester needed only half of the value of the silica polyster. On the other
hand, the failure of carbonate occurred at a distance very near to the upper end of the specimen,
and not at the centre as expected. As for the compression test the results arranged from highest to
the lowest stress, pure, silica, and calcium carbonate respectively. The arrangement should have
been silica, calcium carbonate, and pure polyester, however, some error may have produced these
results. Bending test results showed that the pure polyester required the highest stress for failure
followed the calcium carbonate sample then the silica polyester and these results also were affected
by the errors occurred in the experiment in which the silica should have attained highest failure
stress followed by the calcium carbonate, and pure polyester. Finally, the same problem was
observed in which the pure polyester was the hardest sample then silica and the calcium carbonate.
When adding a filler, it is expected to improve the proprieties of the pure polymer which is not
logical in which the pure polyester showed better mechanical properties than the composite
polyester. The composite silica polyester should have had the highest values of the mechanical
tests. Moreover, the amount of fillers added are very little to show touchable variations from the
pure polyester.

Table 3 Results summary

SAMPLE TENSION COMPRESSION BENDING HARDNESS
TEST TEST (MPA) TEST
STRESS (MPA)
(MPA)
1 Pure 15.91 48.6 12.9 93.4
2 Calcium 4.05 11.75 91.9
carbonate
3 Silica 31.5 6.82 6.3 92

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4.1 SOURCES OF ERROR
- Inaccuracy in weighing the required masses of initiator, activator, and fillers.
- Amounts of fillers are very small.
- Stirring was not efficient enough thus results were affected.
- Dimensions of the samples were not measured accurately which could affect the
results.

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5 CONCLUSION
The aim of the experiment is to perform four mechanical tests on three samples of polyesters. The
tests are tension, compression, bending, and hardness while sample of polyester are pure sample,
calcium carbonate polyester, and silica polyester. Using an unsaturated commercial polyester,
samples were prepared by adding initiator benzoyl peroxide then the activator cobalt octoate. In
addition, silica and calcium carbonate are added in which one pure sample and two composite
polyester sample are obtained. Samples are then poured into the provided moulds and left for
some time in order to attain curing and hardening. Sample are then subjected to mechanical tests
in which tensile, compression, and bending tests are based on stress-strain plots that shows the
stress at which the failure of the material occurred. The results were not as the expected in which
by addition of filler the tensile strength and resistance to deformation in compression and bending
should be improved (increased) as well as the hardness.

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6 BIBLIOGRAPHY
Bobo, E. (2013). Development of a controllable polymer system using interpenetrating networks.
Researchgate.

Dasari, A. (2013). Structural Materials and Processes in Transportation. Wiley.

Elias, H.-G. (2009). Macromolecules. Wiley.

Jose, J. P. (2012). Advances in Polymer Composites: Macro- and. In S. Thomas, Polymer

composites . John Wiley and Sons Inc.

Sastri, V. R. (2010). PLASTICS IN MEDICAL DEVICES: PROPERTIES, REQUIREMENTS,

AND APPLICATIONS. Elsevier Inc.

Subramanian, M. N. (2013). Plastics Additives and Testing . John Wiley & Sons, Inc.

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