EXPERIMENT 2

GELLING TIME AND CASTING TECHNIQUE OF THERMOSET SAMPLE

1. OBJECTIVE
1.1 To produce polymer product using gelling and casting technique.
1.2 To investigate the effect of cure temperature to the cast polymer product.
1.3 To determine gel time dependence of resin epoxy on hardener, catalyst and
accelerator concentration.
2. INTRODUCTION
Casting processes are characterized by the use of liquid or powder starting
material that is shaped without the application of significant pressure. In other words,
casting resins are pourable plastic or thermoset compounds that are used to cast parts,
make molds, or form structures in place. Casting are operations carried out on polymeric
materials to increase their utility. The conversion of polymeric raw materials into useful
finished products. Mold making applications for these resins include their use with
semiconductors; generators and motors; coils and transformers; and switches and circuit
breakers [1].
Thermoplastic are polymers that turn to liquid when heated and turn solid when
cooled. They can be repeatedly remelted and remolded, allowing parts and scraps to be
reprocessed. In most cases they are also very recyclable. Casting resin are mixed with a
hardener, catalyst, or activator and then poured into the sprue of open molds.
Polyester resin is an unsaturated, thermosetting resin produced by a reaction
between several organic acids and polyhydric alcohols. It is most commonly used in the
construction of molded reinforced fiber and composite products. The polyester resin used
in most molding applications is a viscous liquid requiring the addition of catalysts and
accelerators to complete the curing process. Polyester resins are contact products which
require no pressure to cure and can be cured from a fluid or solid state. Although these
products have several distinct disadvantages when compared to other commonly used
composite resins, they still offer an attractive balance of ease of use, low cost, and
positive physical characteristics. MEKP (Methyl Ethyl Ketone Peroxide) is the hardener
added to polyester resins. As the catalyst mixes with the resin, a chemical reaction occurs,

creating heat which cures (hardens) the resin. The reaction is highly exothermic so care
should be taken not to allow excessive heat build up in the part. This is best done by
limiting the thickness of the part to be cured, by minimizing the amount of heat applied to
initiate the peroxide reaction, and by reducing as much as possible the amount of
accelerator used. If the concentration of hardener reactive group matches the
concentration of polyester, a well cross-linked structure with maximum properties will
result [2].
Choose the polyester resin is better than epoxy resin because it lower cost, cure
time can be controlled by catalyst ratio, no sanding between layers, and UV resistant
(Surfboard resin) .
Polymer composite materials often are a combination of small fibers (glass, carbon,
aramid) and a thermosetting resin such as unsaturated polyester, epoxy, phenolic,
polyimide, polyurethane and others being used for specialty composites. All
thermosetting resins must undergo a cure. Cure is a time-dependent, exothermic,
irreversible chemical reaction in which the low molecular weight liquid converts to a
high molecular weight, cross linked solid that serves as a matrix for the fibers.
An important change during cure is gelation, when the reaction has proceeded
sufficiently so that the resin has achieved a flexible but non-flowing three dimensional
molecular structure. Gelation is accompanied by a release of heat resulting in a
temperature rise. Gelation marks the end of the working time of the resin and fiber.
Resin is no longer liquid and attempts to work it and the fiber shape and smooth them
are ineffective and may compromise the properties of the composite. Thus, gel time is an
important factor in the manufacture of all composites and gel temperature is important for
thick or large cross section composites [3].

3. COMPONENT AND EQUIPMENTS

3.1 Plastic cup

3.2 Glass rode

3.3 Dropper

3.4 Timing watch

3.5 Electronic weight balance

3.6 Polyester resin and Methyl Ethyl Ketone Peroxide

4. METHODOLOGY
4.1 Gel Time of Thermoset Sample
4.1.1 All chemicals are moved out from refrigerator and it allowed for 20 minutes at
room temperature.
4.1.2 Polyester resin was weighted for 50g and pour it into plastic glass.
4.1.3 1% (0.5g) of methyl ethyl ketone peroxide was added into epoxy resin and stir
it firmly.

4.1.4 Timing watch was started when these two epoxy were mixed.
4.1.5 Polyester mixer was stirred until it change from liquid to become
agglomerate(crumbly consistency).At the same time, most of the epoxy mixers
will stick at glass rod. Timing watch was stopped and the time was recorded.
4.1.6 Procedure 4.1.1 - 4.1.5was repeated with increases the percentage of methyl
ethyl ketone peroxide with 2%, 3%,4% and 5%.
4.2 Casting Technique
4.2.1 Polyester resin was prepared according to the formulation given by instructor.
4.2.2 Casting make sure was from any dust or scrap.
4.2.3 Spray, pour or brush release agent onto a mold. Release agent help harden or
cure polyester to be easily remove from the mould.
4.2.4 Polyester resin was pour into casting unit slowly to avoid air trapped that can
caused defects to harden polyester.
4.2.5 Polyester resin was allowed dried in room temperature and without pressure for
4 hours.
4.2.6 Hardened polyester was removed from cast unit carefully.

5. RESULT AND DISCUSSION

Table 1 : Result of gel time and cure time of epoxy resin
Group

Polyester resin, g

Methyl ethyl

Gel time (min)

ketone peroxide, g
1

50

0.5

10.03

50

1.0

7.58

50

1.5

7.00

50

2.0

7.35

12
10
8
Gel time, min

6
4
2
0
0.5

1.5

Methyl ethyl ketone peroxide, g

Figure1: Graph of gel time versus the epoxy hardener

From this experiment, it shown that the methyl ethyl ketone peroxide act as
accelerator used to reduce the gel time. For the group 3 is the shorter gel time, 7 minute
when 1.5g of methyl ethyl ketone peroxide was put. Compare to group 1 and the 2 the
longer gel time which showed 10.03 and 7.35 minutes to become gel. The group 1 of
methyl ethyl ketone peroxide is very less, there does not have effect at all, not net force to
each other. So, the gel time become the longer compare to the group 2, 3 and group 4.
Besides that, the colour of resin of group 1 remain the same. From the experiment, it can
shown that the bubble inside become less when stir it slower. And the heat will release
when reach the gel time.
In the casting process, a liquid material is poured into a mold and allowed to solidify
by physical (cooling) or chemical ( polymerization) means resulting in a rigid object that
generally reproduces the mold cavity detail with great fidelity. Fillers can be added to
resin to produce a desired consistency such as talk adds bulk and weight and reduces
material costs. It increases viscosity and reduces cracking in castings by lowering
exothermal value. It also reduces shrinkage in polyester.

Polymerization is the method of creating a synthetic polymer by combining many

small monomer molecules into chain held together by covalent bonds. There are two
major forms of polymerization, step growth polymerization and chain growth
polymerization. The main difference between the two types of polymerization is that in
chain growth polymerization, monomer molecules are added to the chain one at a time. In
the case of step growth polymerization, monomer molecules can bond directly with one
another. It goes without saying that the process of polymerization is full of complexity
and unique terminology. Both of which we will not go into in-depth in this particular
article. If one were to look at a polymer chain close up, they would see that the visual
structure and physical properties of the molecule chain would mimic the actual physical
properties of the polymer. For example, if the polymer chain is comprised of tightly
twisted bonds between monomers and are difficult to break. Chances are this polymer
will strong and tough. In otherwise, if a polymer chain on a molecular level exhibits
stretchy characteristics, chances are this polymer will have flexible properties as well [4].
Most polymers, commonly referred to as plastics or thermoplastics, are not cross
linked polymers. Meaning, the bonds between molecules and polymer chains can be
broken and re-attached. If you think about most common plastics, they can be bent into
shapes with heat. They can also be recycled. Plastic soda bottles are melted down and can
be reused to make everything from carpet to fleece jackets, or made into new water
bottles. This is all done simply with the addition of heat. When polymer chains are linked
together by cross-links, they lose some of their ability to move as individual polymer
chains. For example, a liquid polymer (where the chains are freely flowing) can be turned
into a "solid" or "gel" by cross-linking the chains together.
In polymer chemistry, when a synthetic polymer is said to be "cross-linked", it
usually means that the entire bulk of the polymer has been exposed to the cross-linking
method. The resulting modification of mechanical properties depends strongly on the
cross-link density. Low cross-link densities decrease the viscosities of polymer melts.
Intermediate cross-link densities transform gummy polymers into materials that have
elastomeric properties and potentially high strengths. Very high cross-link densities can
cause materials to become very rigid or glassy, such as phenol-formaldehyde materials.

Cross linked polymers on the other hand cannot re-bond after the cross linked bond
between molecules is broken. Cross linked polymers often exhibit desired properties such
as higher strength, rigidity, thermal properties and hardness. In FRP (Fiber Reinforced
Polymer) composite products, cross linked polymers are most commonly used, and they
are referred to as resin, or thermoset resin. The most common polymers used in
composites are polyester, vinyl ester, and epoxy. However, perhaps the greatest negative
attribute to thermoset resins is the inability of the polymer to be reformed, reshaped, or
recycled [5].
Gel time is one of the most important parameters in any molding process. The gel
time reflects the activity of system according to temperature. Measurements are
performed in constant temperature. Gel time increases with the decreasing curing agent
content at the same temperature; gel time shortens with the rising of constant temperature
at the same phr of curing agent. When increase the temperature. the gel time also
increase. This is because thermoset formed without adding the heat. It will release heat
when we formed the thermoset.
As the theoretical, the group 2 is most suitable and have shorten time in gel time. The
result in experiment shown different is because of some errors occurred during
experiment. This error is believed due to the human error during the experiment.
Different people will feel when the plastic is hot in different time, some of it may stop the
timing watch when a bit heat and some of them stop it when really feel it. Besides that,
the surroundings of experiment carried out also affect the result obtained. The air
conditioned or humidity surrounding may affect the gel time.

6. CONCLUSION
As a conclusion, we chosen the group 2. The group represent 2% of methyl ethyl
ketone peroxide. The group 2 is more suitable and have shorter time in the gel time. Too
much or too little hardener will produce inferior results. Besides that, gel time also

depends on the resin, the volume, and the temperature. Higher volumes and higher
temperatures accelerate the cure, shorten your working time.

7. REFERENCES
1. Steven D. Gordin, Akbar M. Eslami, Howard L. Price.(2004).Gel Time and
Temperature for Two Thermosetting Resins. American Society for
Engineering
Education 1186 session 1793.
2. Dispenza, C.; Carter, J.; McGrail, P.; Spadaro, G. Cure behaviour of epoxy resin
matrices for carbon fibre composites. Polym. Int. 1999, 48, 1229
1236.
3. A. Heierle, "Statische Mischer-Wrmetauscher", Chemie-Anlagen + verfahren,
1994.
4. Sydansk, R.D. 1988. New Conformance-Improvement-Treatment Chromium(III)
Gel Technology. Presented at the SPE Enhanced Oil Recovery
Symposium, Tulsa, Oklahoma, 1621 April.
5. J. K. Stille.(n.d).Step-Growth Polymerization.Colorado State University. Fort
Collins, CO 80523