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Technical Information

Epoxy Curing with INVISTA Diamines


NH 2

H2N NH 2
NH 2
DYTEK® A amine
2-Methylpentamethylenediamine
DYTEK® DCH-99 amine
1,2-Diaminocyclohexane

H2N NH 2

DYTEK® EP diamine
1,3-Pentanediamine

Epoxy resins cured with DYTEK® amines have Table 1 summarizes the process properties,
excellent properties for use in coating, civil mechanical properties, and chemical resistance
engineering, adhesive, and composite of Epon® 828 resin cured with DYTEK® A amines
applications. These properties include greater and DYTEK® EP diamines, and with DYTEK®
flexibility for DYTEK® A amine, better chemical DCH-99 amine and IPDA.
resistance and extremely low odor and low color Table 2 summarizes the properties of an Epon®
for DYTEK® EP diamine, best chemical 828 and Grilonit® RV 1812 (hexanediol
resistance and higher glass transition diglycidylether) resin blend cured with the same
®
temperature for DYTEK DCH-99 amine, and a diamines.
lower adduct viscosity for DYTEK® A amine, Table 3 summarizes the properties of the same
DYTEK® EP diamine, and DYTEK® DCH-99 resin blend cured with four amine adducts.
amine versus competitive amines. These adducts were prepared by reacting each
Three series of tests, summarized in Tables 1–3, diamine with Epon® 828 resin in benzyl alcohol
were done for each of the amines to measure using a 5:1 molar ratio of diamine to resin.
their performance with a standard epoxy resin These amine adducts have low viscosities.
and with two basic epoxy formulations. Higher levels of adduction, 4:1 molar ratio of
Isophoronediamine (IPDA) was included in the diamine to resin, are recommended to optimize
test series for comparative purposes. surface properties.
Stoichiometric amounts of each amine were The DIN test methods used are listed at the
used to cure the resin in all three series. A 24-hr bottom of page 5 along with reference to similar
cure at 23°C followed by a 16-hr post-cure at ASTM methods.
70°C was used for all formulations. The
stoichiometry and cure schedule used may not
be optimal in each case. For example, the
DYTEK® EP diamine, DYTEK® DCH-99 amine,
and IPDA formulations reported in Tables 1 and
2 were not completely cured using the test cure
schedule.

14 March 2012
Table 1
Properties of a Standard Epoxy Resin Cured with Amines
Test Method DYTEK® A DYTEK® EP DYTEK® DCH-99 IPDA
amine diamine amine

Resin
®
Epon 828 (EEW = 188), wt% 100 100 100 100
®
Grilonit RV 1812 (EEW = 142), wt% 0 0 0 0
Resin EEW 188 188 188 188
Amine
Class Aliphatic Aliphatic Cycloaliphatic Cycloaliphatic
HEW 29.0 25.5 28.5 43
Curative Formulation
Amine, wt% 100 100 100 100
Concentration, phr 15.4 13.6 15.2 22.9
Process Properties
Viscositya, cP ISO 2431 900 600 1400 1900
Gel Timeb, tgel, min ASTM D2471 55 73 145 145
Potlifec, t40°C, min ZTV-SIB-TP-OS 37 41 65 73
Maximum Temperature
Tmax., °C 252 230 230 210
Time to Exotherm, tTmax., min ZTV-SIB-TP-OS 50 55 88 100
Cure Conditions
Cure, 24 hr, °C 23 23 23 23
Post-Cure, 16 hr, °C 70 70 70 70
Mechanical Properties
Tg, (DSC), 2nd run, °C ASTM E1356 115 133 176 158
Tg, (DSC), 1st run, °C ASTM E1356 97 99 100 107
HDT, °C DIN 53461 84 92 94 97
Shore D Hardness DIN 53505 78 82 86 86
Izod Impact Strength,
Unnotched, ft-lbf/in2 ISO 180-82 8.8 6.2 6.0 7.1
Charpy Impact Strength,
ft-lbf/in2 5.9 4.3 4.8 6.9
Flexural Strength, psi X 103 DIN 53452 14.8 16.7 12.8 12.1
Elasticity Modulus, psi X 103 DIN 53452 370 415 439 377
Tensile Strength, psi X 103 DIN 53455 10.0 10.9 4.4 6.4
Elongation at Break, % DIN 53455 6.6 5.3 2.4 2.1
Coefficient of Thermal Expansion DIN 53752
αT X 106, m/m°C
Temperature Range, °C:
–20 to 20 58.7 55.2 54.4 53.0
23 to 40 65.4 64.1 61.4 58.8
–20 to 40 60.6 57.7 56.4 54.6
Chemical Resistance ISO 175 % weight gain after 4 weeks immersion at 23°C
Demineralized Water –0.17 –0.22 –0.15 –0.01
10% Sodium Hydroxide 0.66 0.88 0.75 0.80
10% Hydrochloric Acid 1.56 1.26 0.59 1.63
10% Acetic Acid 7.44 0.59 2.01 4.09
Gasoline (DIN 51600d) 0.20 –0.05 0.66 0.41
Xylene 0.22 –0.23 0.12 0.47

aViscosity was measured immediately after mixing the resin and amine.
bGel time: Time for a 120 mL sample at 23°C to reach the gel point.
cPotlife: Time for a 100 mL sample at 23°C to reach 40°C.
dGerman specification for premium (high octane) leaded gasoline.
Table 2
Properties of an Epoxy Resin Blend Cured with Amines

Test Method DYTEK® A DYTEK® EP DYTEK® DCH-99 IPDA


amine diamine amine

Resin
®
Epon 828 (EEW = 188), wt% 80 80 80 80
®
Grilonit RV 1812 (EEW = 142), wt% 20 20 20 20
Resin EEW 179 179 179 179
Amine
Class Aliphatic Aliphatic Cycloaliphatic Cycloaliphatic
HEW 29.0 25.5 28.5 43
Curative Formulation
Amine, wt% 100 100 100 100
Concentration, phr 16.2 14.3 16.0 24.0
Process Properties
Viscositya, cP DIN 53211 160 160 290 280
Gel Timeb, tgel, min ASTM D2471 45 60 135 115
Potlifec, t40°C, min ZTV-SIB-TP-OS 20 24 52 66
Maximum Temperature
Tmax., °C 255 222 223 203
Time to Exotherm, tTmax.,min ZTV-SIB-TP-OS 40 40 77 95
Cure Conditions
Cure, 24 hr, °C 23 23 23 23
Post-Cure, 16 hr, °C 70°C 70°C 70°C 70°C
Mechanical Properties
Tg, (DSC), 2nd run, °C ASTM E1356 83 96 130 120
Tg, (DSC), 1st run, °C ASTM E1356 81 87 100 104
HDT, °C DIN 53461 60 78 94 91
Shore D Hardness DIN 53505 78 84 84 85
Chemical Resistance ISO 175 % weight gain after 4 weeks immersion at 23°C
Demineralized Water 0.29 0.00 0.10 0.14
10% Sodium Hydroxide 0.87 0.82 0.94 0.94
10% Hydrochloric Acid 4.41 3.42 1.62 3.17
10% Acetic Acid 12.52 3.71 7.09 6.75
Gasoline (DIN 51600d) 0.20 0.34 0.45 0.44
Xylene 0.25 0.25 0.45 0.45
a
Viscosity was measured immediately after mixing the resin and amine.
b
Gel time: Time for a 120 mL sample at 23°C to reach the gel point.
c
Potlife: Time for a 100 mL sample at 23°C to reach 40°C.
d
German specification for premium (high octane) leaded gasoline.
Table 3
Properties of an Epoxy Resin Blend Cured with Amine Adducts

Test Method DYTEK® A DYTEK® EP DYTEK® DCH-99 IPDA


amine diamine amine
Resin
Epon® 828 (EEW = 188), wt% 80 80 80 80
Grilonit® RV 1812 (EEW = 142), wt% 20 20 20 20
Resin EEW 179 179 179 179
Amine
Class Aliphatic Aliphatic Cycloaliphatic Cycloaliphatic
HEW 29.0 25.5 28.5 43
Curative Formulation
Amine, wt% 38.8 35.8 38.8 48.2
Epon® 828 (EEW = 188), wt% 25.1 26.3 25.1 21.3
Benzyl Alcohol, wt% 36.1 37.9 36.1 30.6
Molar Ratio (diamine:resin) 5:1 5:1 5:1 5:1
Adduct Viscosity, 21.5°C, cP 7.5 6.5 17.5 86.5
Adduct HEW 83 79 82 98
Concentration, phr 46.5 44 46 55
Process Properties
Viscositya, cP DIN 53211 730 680 700 1330
Gel Timeb, tgel, min ASTM D2471 20 40 80 60
Potlifec, t40°C, min ZTV-SIB-TP-OS 7 20 20 27
Maximum Temperature
Tmax., °C 207 181 170 176
Time to Exotherm, tTmax., ZTV-SIB-TP-OS 17 35 40 54
min.
Dry Time, Dust-free, hr DIN 53150 3.5 7 7 4
Cure Conditions
Cure, 24 hr, °C 23°C 23°C 23°C 23°C
Post-Cure, 16 hr, °C 70°C 70°C 70°C 70°C
Mechanical Properties
Tg, (DSC), 2nd run, °C ASTM E1356 43 52 83 74
Tg, (DSC), 1st run, °C ASTM E1356 38 43 70 41
HDT, °C DIN 53461 35 40 52 50
Shore D Hardness DIN 53505 78 81 80 83
Chemical Resistance ISO 175 % weight gain after 4 weeks immersion at 20°C
Demineralized Water 1.11 1.18 0.63 0.72
10% Sodium Hydroxide 1.54 1.60 1.35 1.42
10% Hydrochloric Acid 5.63 3.76 1.85 2.83
10% Acetic Acid 30.9 7.31 6.54 4.80
Gasoline (DIN 51600d) 0.70 0.63 0.60 0.64
Xylene –0.54 0.52 0.54 0.56
a
Viscosity was measured immediately after mixing the resin and amine.
b
Gel time: Time for a 120 mL sample at 23°C to reach the gel point.
c
Potlife: Time for a 100 mL sample at 23°C to reach 40°C.
d
German specification for premium (high octane) leaded gasoline.
Test Method Equivalents

DIN ASTM Test


53150 D1640 Drying Time

53461 D648 Heat Deformation Temperature

53505 D2240 Shore D Hardness


53452 D790 Flex Properties
53455 D638 Tensile Properties
53752 D3386 Thermal Expansion

For Samples and Information:


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