James Coulton

2363011
Dr. Suong Hoa

MECH 425 Manufacturing of Composites

Lab 1: Gel Time and Peak Exothermic Temperature of Thermosetting Resins

Lab performed: September 16, 2014

Lab due: September 30, 2014

OBJECTIVE
The objective of this experiment is to familiarize ourselves with the manipulation, curing time
and cleaning/disposal of vinyl ester resins. Measurement of vinyl ester gel time and peak
exothermal temperature is also done two different standards.
INTRODUCTION
In the manufacturing of resins for composites, gel time and peak exothermal temperature are the
two most important properties for a thermosetting material. Gel time is the time available to
manipulate and spread the resin before it solidifies into a gel. The change in viscosity from a
liquid to a gel is due to the cross-linking reaction taking place inside the resin after the
introduction of the catalyst. In our case, the catalyst is methyl ethyl ketone peroxide (MEKP). It
initiates the cross linking inside the vinyl ester resin (VER) resin. To speed up the reaction, a
promoter/accelerator is used: cobalt naphthenate (CoNaph). Once the proper proportions of each
constituent is placed in a mixture, the American Society for Testing and Materials proposes two
standards for characterizing thermosetting resins.
The first is the ASTM D2471 which is based on probing the surface of a beaker containing
reactants until the surface reaches a gel-like state and noting the time. Simultaneously a
thermocouple is placed in the geometric center of the beaker to record the temperature of the
core over time.
The second standard is the ASTM D3056 which utilizes a gel time apparatus that uses a torsion
wire that detects when the viscosity becomes too high. It is called a Gel Time Meter.

PROCEDURE
1.
2.
3.
4.
5.
6.

Set up the Get Time Meter and computer for the temperature recording
Weigh 80 g of resin to the nearest 0.01 g
Calculate the corresponding mass of the promoter (CoNaph) and catalyst (MEKP)
Add the promoter into and mixture and stir for 2 mins
Add the catalyst into the and stir for 1 min, then start the stop watch
Fill up the test tube at the indicated level and place it into the Gel Time Meter

7. Turn on that apparatus and simultaneously place a thermocouple in the center of the
remaining resin contained in the beaker
8. Every 15 seconds, probe the beaker with an applicator stick to the surface
9. Keep probing until the resin surface is hard enough to not adhere to the stick and record this
gel time
10. Once the Gel Time Meter reaches a high viscosity. It will make contact, buzz and the timer
will stop. Record this time and compare with probing time
11. Save thermocouple data from computer
RESULTS & DISCUSSION
Group 1:
Fig #
7

This group should have a mixture with the bulk of its weight to be occupied by 80 g of
vinyl ester resin (VER). The cobalt naphthenate (CoNaph) promoter should have a weight of
0.15% that of the resin. The methyl ethyl ketone peroxide (MEKP) catalyst should have a weight
of 10 times the promoter. The following Table shows the desired and actual weights of each
ingredient.

Resin (VER)
Promoter (CoNaph)
Catalyst (MEKP)

Desired Weight [g]

80.000
0.120
1.200

Measured Weight [g]

79.978
0.131
1.200

Using both standards for measuring gel time are displayed in the following Table. Note that
D3056 refers to the torsion wire test while D2471 refers to the hand-probing and thermocouple
test.
Gel Time [Min]

D3056
D2471
17.7
16.0

Only the D2471 standard measures peak exothermic temperature and time. The results are shown
below.

Temperature of bulk center Vs Time

200
150
Temperarure [C]

100
50
0
28:48.0

43:12.0

57:36.0

12:00.0

Time [Min:Sec:Millisec]

Peak Exothermic Temp [C]

Peak Exothermic Time [Min]

170
24

Group 2:
Fig #
7

This group will do repeat the tests but with a slightly different mixture percentage. The
mixture should have the bulk of its weight to be occupied by 80 g of vinyl ester resin (VER). The
cobalt naphthenate (CoNaph) promoter should have a weight thats 0.125% that of the resin. The
methyl ethyl ketone peroxide (MEKP) catalyst should have a weight thats 10 times that of the
promoter. The following Table shows the desired and actual weights of each ingredient.

Resin (VER)
Promoter (CoNaph)
Catalyst (MEKP)

Desired Weight [g]

80.000
0.100
1.000

Measured Weight [g]

80.060
0.129
1.300

Using both standards for measuring gel time are displayed in the following Table. Note that
D3056 refers to the torsion wire test while D2471 refers to the hand-probing and thermocouple
test.
Gel Time [Min]

D3056
D2471
17.7
15.0

Only the D2471 standard measures peak exothermic temperature and time. The results are shown
below.

Temperature of bulk center Vs Time

200
150

Temperarure [C]

100
50
0
57:36.0 12:00.0 26:24.0 40:48.0

Time [Min:Sec:Millisec]

Peak Exothermic Temp [C]

Peak Exothermic Time [Min]

168
22

Although Group 2 was supposed to transfer different percentages of the ingredients into the
mixture, it proved to be difficult and we both ended up with relatively the same mixture.
CONCLUSION:
The heat generated by the matrix appears to pick up slowly but then increases exponentially. This
is because the reaction of the cross-linking of the ingredients generates heat. The very same
reaction also increases in speed with a temperature increase. If a slower reaction rate and lower
peak exothermal temperature are desired then the heat of the reaction must be dissipated to the
environment quicker. This is why we placed the thermocouple to measure temperature in the
center of the beaker. It is at the point that is hardest to dissipate heat so it should be the peak
temperature. Other ingredients such as retardants may be added to slow down the reaction.
Another interesting conclusion is that the peak exothermal temperature happens in a point into
after the gel time. The reactants continue to react until the resin mixture becomes a complete
solid.