Epoxy Lab

Objective:
 To learn about synthesis of epoxy resin.

 To learn about polycondensation process.
 To know about different type of epoxy resin
Introduction:
Epoxy resins are a large family of materials that are defined as low molecular weight pre-
polymer thermosets with more than one epoxide ring. Epoxy resins are commonly employed in
structural applications as composite materials because they provide a unique mix of qualities that
no other thermoset resin offers. Prileschajew developed epoxy resins in 1909, whereas the first
synthesis of epoxy resin was performed in the United States in the late 1930s by the reaction of
Bisphenol-A with epichlorohydrin.
The outstanding capacity of the epoxy ring in the basic structure of these thermosets to react with
a wide range of chemical compounds and functional groups makes them a versatile class of
thermosets. Treatment of epoxy resins with additional chemical compounds is often referred to
as curing, which results in the formation of insoluble and recalcitrant thermoset polymers. As a
thermoset material, epoxy is highly resistant to chemical and corrosive environments; it has
outstanding mechanical and thermal characteristics; it has little shrinkage after curing; and it is
straightforward to manufacture. A range of epoxy resin and curing agent combinations may be
used to manufacture materials of choice for usage in various structural applications, in order to
suit market needs [1].
According to the range of starting materials employed in the synthesis of epoxy resins, a number
of epoxy resins have been discovered so far. These epoxy resins were manufactured utilizing
diverse synthetic processes and ambient temperature and solvent conditions. Bisphenol-A epoxy
resins, bisphenol-F epoxy resins, cycloaliphatic epoxy resins, trifunctional epoxy resins, tetra-
functional epoxy resins, novolac epoxy resins, bio-based epoxy resins, fluorine containing epoxy
resins, phosphorus containing epoxy resins, and silicon containing epoxy resins are the most
frequent categories of epoxy resins explored and synthesized lately. Depending on the initial
ingredients utilized in their synthesis, the physical state of these epoxy resins ranges from liquid
to semi-solid and even solid [2].
In this experiment, bisphenol-A epoxy resin was synthesized. The method includes dissolving
bisphenol A and epichlorohydrin, and then adding a cocatalyst and NaOH solution to perform
etherification for 1-3 hours at 45-800C and absolute pressures of 15-25 kPa, adding the NaOH
solution dropwise; after the reaction is finished, removing water and excess epichlorohydrin to
obtain coarse epoxy resin; and using an organic solvent to dissolve the coarse epoxy resin,
adding NaOH solution to react for 1-4h at 60-100 0C, removing salt and waste polymer by
washing, and removing the solvent to achieve the high-purity, low-organochlorine, and low-
viscosity liquid epoxy resin.
Fig.1: Synthesis of Epoxy resin

Experimental Procedure:
1. A 3-neck round flask was charged with 15gm of bisphenol A and 5ml of 10%
aqueous NaOH.
2. Then the flask was equipped with condenser, dropping funnel and thermometer.
3. The flask was placed with its content on a silicon oil bath.
4. The compounds in the flask were warmed to 45 0 C and allowed to mix for 10-15
minutes.
5. After that 10 mL of epichlorohydrin was added in the mixture.
6. The mixture was now heated to 850 C and allowed the polycondensation to go about 2
hours.
7. After polycondensation process, the mixture was separated in two phases.
Epoxy product is an emulsion of the resin and sodium salt.
1st Phase:
 The epoxy product was dissolved in a solvent (acetone) to separate the resin from
sodium salt.
 The resin was dissolved in the solvent whereas the salt didn’t.
 Then the salt was filtered out by the filter paper and the solvent is removed by
fraction distillation (2nd phase)
Fractional Distillation:
Fractional distillation is a basic technique in which an unnamed liquid is gently heated to a boil
in a "pot." The component with the lowest boiling point will boil first, forcing the vapor to move
up the fractioning column via the three-way adapter (head) containing the thermometer. The
thermometer measures the temperature of the vapor as it flows through the head and into the
west condenser, where it cools and liquefies before being collected in a test tube (5mL at a time).
Because the second tube includes a combination of the two chemicals, only the first and third
tubes are utilized and examined. This is due to an impure combination of residual unknown A
and unknown B that has started to boil in tube 2. The boiling points of each unknown are
represented by the average head temperatures for tubes 1 and 3, which are then compared to the
boiling points of known compounds to identify the identities.
Conclusion:
This experiment was carried out in three stages. First, a polycondensation procedure was
performed in which a combination of bisphenol A and epichlorohydrin was heated to 80 0 C for 2
hours. The combination was then dissolved in a solvent, and the salt was filtered off. Finally, a
viscous liquid epoxy resin was created by the fractional distillation procedure. Due to the
limitations of our laboratory facilities, we were unable to complete the final procedure.
References:
[1] L.C. Over, E. Grau, S. Grelier, M.A.R. Meier, H. Cramail, Synthesis and Characterization
of Epoxy Thermosetting Polymers from Glycidylated Organosolv Lignin and Bisphenol A,
Macromol. Chem. Phys. 218 (2017) 1600411.
[2] S. Gul, A. Kausar, M. Mehmood, B. Muhammad, S. Jabeen, Progress on Epoxy/Polyamide
and Inorganic Nanofiller-Based Hybrids: Introduction, Application, and Future Potential,
Polymer-Plastics Technology and Engineering. 55 (2016) 1842–1862.

Epoxy Lab

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Epoxy Lab

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Objective:

 To learn about synthesis of epoxy resin.

Fig.1: Synthesis of Epoxy resin

Epoxy product is an emulsion of the resin and sodium salt.

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