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Prediction of Pot life of Resin System

   Significance of the Project
 The most important application of kinetics in thermal analysis is to
 predict reaction behavior under conditions in which it is practically
 impossible to make measurements, for example for very short or very
 long reaction times.

 Pot life is an important parameter that related to the thermal stability of
 mixed resin system, which provides information for processing and
 production of materials. Kinetics prediction is an efficient method to get
 the information about stability of materials at use (ambient)
 temperature.

    Example of Application
    Reaction injection molding: large component/part
    Adhesives
Methods
 Experiment
Differential Scanning Calorimetry (DSC)


 Kinetic Analysis
   Kissinger method
Applicable to reaction that can                                  E
                                          ln    2
                                                     const. 
be described by the Arrhenius                  Tm                RTm
equation and the general rate
law..                                                  ln(1   )
                                           t 
                                                               E
Assumption: the extent of the                       A * EXP(       )
                                                               RT0
reaction at the peak exotherm
is constant and independent
of heating rate.
Isothermal Kinetic Measurements
                 5            o
                           260 C
                                                                                                                                 How about dynamic


                                                     exo
                 4                                                                                                               experiment?
                                                                                  5
-1




                                                                                               o
Heat Flow /W g




                 3                                                                        250 C




                                                                                                                exo
                                                                                  4



                                                                 -1
                 2


                                                                 Heat Flow /W g
                                                                                  3
                                                                                                                                       5
                 1
                                                                                                                                                  o
                                                                                  2                                                            240 C




                                                                                                                                                                        exo
                                                                                                                                       4
                 0




                                                                                                                      -1
                                                                                  1




                                                                                                                      Heat Flow /W g
                 -25   0    25      50    75   100         125                                                                         3
                                  Time /min                                       0
                                                                                                                                       2
                                                                                      0   10       20      30    40
                                                                                               Time /min                               1


                 The samples are not stable for isothermal                                                                             0


                 experiments.                                                                                                              0     20         40     60         80
                                                                                                                                                       Time /min


                 Maximum of heat evolution occurs at time: 0, it follows nth order kinetics.
                 The dynamic method should work.
Dynamic Kinetic Measurements
                                                o
                                           10 C/min
                                                o
                                                            Pot Life of Anonymous
                                           13 C/min
                  2                         o
                                           7 C/min
                                            o
                                           4 C/min
                                                                Resin System
-1
 Heat Flow /W g




                                                                 100
                   1




                                                              time to 5% (days)
                                                                           10
                  0


                   150   200   250   300        350   400                                                                   B
                                     o                                            1
                               Temp / C


                  DSC curves for sample B at                                                                                A
                  different heating rate.                                             0   10    20     30         40   50
                                                                                                            o
                                                                                               Temperature ( C)


                                                            Samples B is more thermally
                                                            stable.
                                                            Sample A has lower stability.
Summary

Kinetic analysis can be applied in kinetics prediction.
We can use the values A and E to easily obtain time to
any conversion at any temperature of interest.

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Kinetics Prediction of Pot Life

  • 1. Prediction of Pot life of Resin System Significance of the Project The most important application of kinetics in thermal analysis is to predict reaction behavior under conditions in which it is practically impossible to make measurements, for example for very short or very long reaction times. Pot life is an important parameter that related to the thermal stability of mixed resin system, which provides information for processing and production of materials. Kinetics prediction is an efficient method to get the information about stability of materials at use (ambient) temperature. Example of Application Reaction injection molding: large component/part Adhesives
  • 2. Methods Experiment Differential Scanning Calorimetry (DSC) Kinetic Analysis Kissinger method Applicable to reaction that can  E ln 2  const.  be described by the Arrhenius Tm RTm equation and the general rate law..  ln(1   ) t  E Assumption: the extent of the A * EXP( ) RT0 reaction at the peak exotherm is constant and independent of heating rate.
  • 3. Isothermal Kinetic Measurements 5 o 260 C How about dynamic exo 4 experiment? 5 -1 o Heat Flow /W g 3 250 C exo 4 -1 2 Heat Flow /W g 3 5 1 o 2 240 C exo 4 0 -1 1 Heat Flow /W g -25 0 25 50 75 100 125 3 Time /min 0 2 0 10 20 30 40 Time /min 1 The samples are not stable for isothermal 0 experiments. 0 20 40 60 80 Time /min Maximum of heat evolution occurs at time: 0, it follows nth order kinetics. The dynamic method should work.
  • 4. Dynamic Kinetic Measurements o 10 C/min o Pot Life of Anonymous 13 C/min 2 o 7 C/min o 4 C/min Resin System -1 Heat Flow /W g 100 1 time to 5% (days) 10 0 150 200 250 300 350 400 B o 1 Temp / C DSC curves for sample B at A different heating rate. 0 10 20 30 40 50 o Temperature ( C) Samples B is more thermally stable. Sample A has lower stability.
  • 5. Summary Kinetic analysis can be applied in kinetics prediction. We can use the values A and E to easily obtain time to any conversion at any temperature of interest.