CHEM TECHNOLOGIES, LTD. · 1 Advancure™ Curative for Vamac® CHEM TECHNOLOGIES, LTD. Beyond the obvious from innovation to application Bonnie Stuck – Chem Technologies, Ltd

1

AdvancureAdvancure™™ Curative for VamacCurative for Vamac®®

CHEM TECHNOLOGIES, LTD.Beyond the obvious from innovation to application

Bonnie Stuck Bonnie Stuck –– Chem Technologies, Ltd.Chem Technologies, Ltd.Patricia Czomba Patricia Czomba –– Chem Technologies, Ltd.Chem Technologies, Ltd.Kim Boyd Kim Boyd –– Chem Technologies, Ltd.Chem Technologies, Ltd.Edward McBride Edward McBride –– DuPontDuPontAlice Uminska Alice Uminska –– Gold Key Processing, Ltd.Gold Key Processing, Ltd.Kevin Dominic Kevin Dominic –– Gold Key Processing, Ltd.Gold Key Processing, Ltd.

Technical Report: CTRTechnical Report: CTR--0600106001August 2006August 2006

2

BackgroundBackground

DuPont VamacDuPont Vamac®® ethylene acrylic elastomers is designed to ethylene acrylic elastomers is designed to withstand high and low temperatures and aggressive new withstand high and low temperatures and aggressive new automotive fluids in under hood automotive applications automotive fluids in under hood automotive applications such as seals, gaskets, ducts, hoses, boots and dampers. such as seals, gaskets, ducts, hoses, boots and dampers. The most often cure system used in VamacThe most often cure system used in Vamac®® compounds is a compounds is a combination of HMDC (hexamethylenediamine carbamate) combination of HMDC (hexamethylenediamine carbamate) with DOTG (diwith DOTG (di--oo--tolylguanidine) or DPG tolylguanidine) or DPG (diphenylguanidine).(diphenylguanidine).During the vulcanization process the HMDC breaks down During the vulcanization process the HMDC breaks down into HMDA (hexamethlyene diamine) which is the active into HMDA (hexamethlyene diamine) which is the active curing agent.curing agent.The HMDC curative is the second highest cost component of The HMDC curative is the second highest cost component of VamacVamac®® compounds.compounds.

3

HexamethlyenediamineHexamethlyenediamine Cure MechanismCure Mechanism

4

AdvancureAdvancure

Advancure is a 47% active liquid concentrate of Advancure is a 47% active liquid concentrate of hexamethylenediamine (HMDA) absorbed on amorphous hexamethylenediamine (HMDA) absorbed on amorphous silica in powder form. silica in powder form. Advancure is based on patented curing technology from Advancure is based on patented curing technology from DuPont and is enhanced with an innovative dispersion DuPont and is enhanced with an innovative dispersion technology from Chem Technologies. technology from Chem Technologies. Advancure is a freeAdvancure is a free--flowing, dustflowing, dust--free beaded powder that can free beaded powder that can be used to cure the majority of Vamacbe used to cure the majority of Vamac®® products at a lower products at a lower cost compared to traditional curing technologies.cost compared to traditional curing technologies.Advancure HMDA (hexamethlyene diamine) is a lower cost Advancure HMDA (hexamethlyene diamine) is a lower cost alternative to HMDC (hexamethylenediamine carbamate) alternative to HMDC (hexamethylenediamine carbamate) types. types. For the same activity level, replace 1 phr of For the same activity level, replace 1 phr of hexmethylenediamine carbamate with 1.56 phr of Advancure.hexmethylenediamine carbamate with 1.56 phr of Advancure.

5

Advancure (HMDA) Advancure (HMDA) versusversus

HMDC From Several SourcesHMDC From Several Sources

VamacVamac®® G Model CompoundG Model CompoundLaboratory StudiesLaboratory Studies

Testing done in Gold Key Processing Testing done in Gold Key Processing & Chem Technologies Laboratories& Chem Technologies Laboratories

6

Formulation Formulation

VamacVamac®® GG 100.00100.00N774 Carbon BlackN774 Carbon Black 90.0090.00Stearic AcidStearic Acid 2.002.00PolyoxyethylenePolyoxyethylene octadecyloctadecylether phosphateether phosphate 1.501.5011--ocadecanamineocadecanamine 0.500.50Di(2Di(2--ethylhexyl) ethylhexyl) sebacatesebacate 10.0010.00DOTG (diDOTG (di--oo--tolylguanidine) tolylguanidine) 4.004.00HMDC or HMDAHMDC or HMDA see next slidesee next slide

Vamac is a registered trademark of DuPont.Vamac is a registered trademark of DuPont.

7

Curative VariablesCurative Variables

HMDC #1 HMDC #1 –– Diak 1, a trademark of DuPont.Diak 1, a trademark of DuPont.

oo at 1.50 phrat 1.50 phr

HMDC #2 HMDC #2 –– Vulcofac HDC, a trademark of Safic.Vulcofac HDC, a trademark of Safic.


HMDC #3 HMDC #3 –– Trilink 1, a trademark of LiandaTrilink 1, a trademark of Lianda


HMDC #4 HMDC #4 –– Intercure 1, a trademark of InterbusinessIntercure 1, a trademark of Interbusiness


Advancure Advancure –– HMDA from Chem TechnologiesHMDA from Chem Technologies


8

Testing ProceduresTesting Procedures

Mixing was done in a Moriyama 1.5 L lab mixer Mixing was done in a Moriyama 1.5 L lab mixer

with a dump temperature of 93with a dump temperature of 93ººC.C.

MDR Rheometer at 177MDR Rheometer at 177ººC, ASTM D 5289.C, ASTM D 5289.

Mooney at 121Mooney at 121ººC, ASTM D 1646.C, ASTM D 1646.

Physical Properties (hardness, tensile, modulus, Physical Properties (hardness, tensile, modulus,

elongation). Presselongation). Press--cured 5 minutes at 177cured 5 minutes at 177ººC, post C, post

cured 4 hours at 177cured 4 hours at 177ººC. ASTM D 412.C. ASTM D 412.

9

The Advancure compound had slightly higher torque than the The Advancure compound had slightly higher torque than the HMDC controls.HMDC controls.

MDR Rheometer at 177 CMaximum Torque

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

HMDC #1 HMDC #2 HMDC #3 HMDC #4 Advancure

Max

imum

Tor

que

(N-m

)

10

The Advancure compound had a slightly longer cure time than the The Advancure compound had a slightly longer cure time than the HMDC control compounds due its higher maximum torque value.HMDC control compounds due its higher maximum torque value.

MDR Rheometer at 177CTc90 Cure Time

0

1

2

3

4

5

6

7

8


Tc9

0 (m

inut

es)

11

The Advancure compound had a slightly longer Ts5 scorch to the The Advancure compound had a slightly longer Ts5 scorch to the HMDC controls.HMDC controls.

Mooney at 121 CTs5 Scorch Time

0

1

2

3

4

5

6

7


Ts5

(min

utes

)

12

The Advancure compound had a slightly lower viscosity level thanThe Advancure compound had a slightly lower viscosity level than the the control compounds.control compounds.

Mooney at 121 CViscosity ML 1+4

20

22

24

26

28

30

32

34

36

38

40


Visc

osity

ML

1+4

(MU

)

13

The Advancure compound had a similar durometer to HMDC #1, 2 The Advancure compound had a similar durometer to HMDC #1, 2 and 4 controls. HMDC #3 had a lower durometer.and 4 controls. HMDC #3 had a lower durometer.

Shore A Durometer

70

71

72

73

74

75

76

77

78

79

80


Dur

omet

er (p

oint

s)

14

The Advancure compound had slightly higher tensile.The Advancure compound had slightly higher tensile.

Tensile

0

2

4

6

8

10

12

14

16

18

20


Ten

sile

(MPa

)

15

The compounds had slightly lower elongation at break values.The compounds had slightly lower elongation at break values.

Elongation @ Break

0

50

100

150

200

250


Elo

ngat

ion

(%)

16

The Advancure compound had higher modulus than the The Advancure compound had higher modulus than the HMDC control compounds.HMDC control compounds.

100% Modulus

0

1

2

3

4

5

6

7

8

9

10


100%

Mod

ulus

(MPa

)

17

Advancure (HMDA) Versus HMDC Advancure (HMDA) Versus HMDC in Various Vamacin Various Vamac®® Formulations Formulations

Formula #1: Standard Vamac compound with 10 phr plasticizerFormula #1: Standard Vamac compound with 10 phr plasticizerFormula #2: Standard Vamac compound with no plasticizerFormula #2: Standard Vamac compound with no plasticizerFormula #3: Vamac compound with no plasticizer and with Formula #3: Vamac compound with no plasticizer and with

““flexflex”” curecure

DuPont LaboratoriesDuPont Laboratories

18

FormulationsFormulations

IngredientIngredient Formula #1Formula #1 Formula #2Formula #2 Formula #3Formula #3Vamac Vamac ®® GG 100.00100.00 100.00100.00 100.00100.00N550 Carbon BlackN550 Carbon Black 60.0060.00 50.0050.00 50.0050.00Ether/Ester PlasticizerEther/Ester Plasticizer 10.0010.00 0.000.00 0.000.00Stearic AcidStearic Acid 1.501.50 1.501.50 1.501.50PolyoxyethylenePolyoxyethylene 1.001.00 1.001.00 1.001.00octadecyloctadecyl ether phosphateether phosphate11--ocadecanamineocadecanamine 0.500.50 0.500.50 0.500.504,4' 4,4' Di(a,aDi(a,a--dimethylbenzyldimethylbenzyl) ) 2.002.00 2.002.00 2.002.00diphenylaminediphenylamineDPG DPG 0.000.00 0.000.00 2.002.00(N,N'(N,N'--diphenylguanidine)diphenylguanidine)DOTGDOTG 4.004.00 4.004.00 2.002.00(di(di--oo--tolylguanidine)tolylguanidine)HMDC (Diak 1)HMDC (Diak 1) 1.501.50 1.501.50 1.201.20oror

AdvancureAdvancure 2.342.34 2.342.34 1.871.87

Formula #1: Standard Vamac compound with 10 phr plasticizerFormula #1: Standard Vamac compound with 10 phr plasticizerFormula #2: Standard Vamac compound with no plasticizerFormula #2: Standard Vamac compound with no plasticizerFormula #3: Vamac compound with no plasticizer and with Formula #3: Vamac compound with no plasticizer and with ““flexflex”” curecure

Diak 1 and Vamac are trademarks of DuPont.Diak 1 and Vamac are trademarks of DuPont.

19

Cure DataCure Data

MDR Rheometer, ASTM D5289MDR Rheometer, ASTM D5289Mooney, ASTM D1646Mooney, ASTM D1646

20

The Advancure compounds had similar torque values to the HMDC The Advancure compounds had similar torque values to the HMDC control compounds.control compounds.

MDR Rheometer at 177 CMaximum Torque

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

HMDCControl

Advancure

Max

.Tor

que

(lb-in

)

Formula #1 Formula #2 Formula #3

21

The Advancure compounds had similar cure times to the HMDC The Advancure compounds had similar cure times to the HMDC control compounds.control compounds.

MDR Rheometer at 177 CTc90 Cure Time

0

2

4

6

8

10

12

HMDCControl

Advancure

Tc9

0 (m

inut

es)


22

The Advancure compounds had similar scorch times to the HMDC The Advancure compounds had similar scorch times to the HMDC control compounds.control compounds.

Mooney Scorch at 121 CT10 Scorch

0

2

4

6

8

10

12

14

16

HMDCControl

Advancure

T18

(min

utes

)


23

The Advancure compounds had similar viscosity to the HMDC The Advancure compounds had similar viscosity to the HMDC control compounds.control compounds.

Mooney Viscosity at 121 CML 1+4

0

5

10

15

20

25

30

35

40

45

50

HMDCControl

Advancure

Visc

osity

(MU

)


24

Physical Properties Physical Properties -- Unaged Unaged

Press Cure: 5 min. at 175Press Cure: 5 min. at 175ººCCPost Cure: 4 hours at 175Post Cure: 4 hours at 175ººCC

Shore A Durometer, ASTM D2240Shore A Durometer, ASTM D2240Stress Strain, ASTM D412Stress Strain, ASTM D412Die C Tear, ASTM D624Die C Tear, ASTM D624Compression Set, ASTM D395Compression Set, ASTM D395

25

The Advancure compounds had slightly higher durometer values to The Advancure compounds had slightly higher durometer values to the HMDC control compounds.the HMDC control compounds.

Shore A DuromterUnaged

60

62

64

66

68

70

72

74

76

HMDCControl

Advancure

Dur

omet

er (p

oint

s)


26

The Advancure compounds had similar 50% modulus values to the The Advancure compounds had similar 50% modulus values to the HMDC control compounds.HMDC control compounds.

50% ModulusUnaged

0

0.5

1

1.5

2

2.5

HMDCControl

Advancure

50%

Mod

ulus

(Mpa

)


27

The Advancure compounds had similar tensile values to the HMDC The Advancure compounds had similar tensile values to the HMDC control compounds.control compounds.

TensileUnaged

0

2

4

6

8

10

12

14

16

18

20

HMDCControl

Advancure

Ten

sile

(MPa

)


28

The Advancure compounds had slightly lower elongation values to The Advancure compounds had slightly lower elongation values to the HMDC control compounds.the HMDC control compounds.

ElongationUnaged

0

50

100

150

200

250

300

350

400

450

500

HMDCControl

Advancure

Elo

ngat

ion

(%)


29

The Advancure compounds had slightly lower Die C tear to the The Advancure compounds had slightly lower Die C tear to the HMDC control compounds.HMDC control compounds.

Die C TearUnaged

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

HMDCControl

Advancure

Tea

r (M

Pa)


30

The Advancure compounds had similar compression set to the The Advancure compounds had similar compression set to the HMDC control compounds.HMDC control compounds.

Compression Set - UnagedAfter 1 Week at 150 C

0

5

10

15

20

25

30

HMDCControl

Advancure

Com

pres

sion

Set (

%)


31

Aged Physical PropertiesAged Physical Properties

Aged 1 week at 150CAged 1 week at 150Cin IRM903 Oil, ASTM D471in IRM903 Oil, ASTM D471

32

The Advancure compounds had similar change in durometer to the The Advancure compounds had similar change in durometer to the HMDC control compounds.HMDC control compounds.

Shore A Duromter Change1 week in IRM903 at 150C

-21.4 -21.6

-19.3-20.4

-23.7 -23.6-25

-20

-15

-10

-5

0

HMDCControl

Advancure

Dur

omet

er C

hang

e (p

oint

s)


33

The Advancure compounds had less change in 50% modulus than the The Advancure compounds had less change in 50% modulus than the HMDC control compounds.HMDC control compounds.

50% Modulus Change1 week in IRM903 at 150C

-24%

-17%

-30%

-18%

-32%

-23%

-35%

-30%

-25%

-20%

-15%

-10%

-5%

0%

HMDCControl

Advancure

50%

Mod

ulus

Cha

nge

(%)


34

The Advancure compounds had similar change in tensile to the The Advancure compounds had similar change in tensile to the HMDC control compounds.HMDC control compounds.

Tensile Change1 week in IRM903 at 150C

-28% -27%

-39%

-35%-32%

-29%

-45%

-40%

-35%

-30%

-25%

-20%

-15%

-10%

-5%

0%

HMDCControl

Advancure

Ten

sile

Cha

nge

(%)


35

The Advancure compounds had similar to less elongation change thThe Advancure compounds had similar to less elongation change than an the HMDC control compounds.the HMDC control compounds.

Elongation Change1 week in IRM903 at 150C

-35% -36%

-40%

-36%

-40%

-36%

-45%

-40%

-35%

-30%

-25%

-20%

-15%

-10%

-5%

0%

HMDCControl

Advancure

Elo

ngat

ion

Cha

nge

(%)


36

Aged Physical PropertiesAged Physical Properties

Aged 1 week at 175Aged 1 week at 175ººC in Air, C in Air, ASTM D572ASTM D572

37

The Advancure compounds had similar retained durometer to the The Advancure compounds had similar retained durometer to the HMDC control compounds.HMDC control compounds.

Shore A Duromter Change1 week heat aging in Air at 175C

9.510.1

3.9 4.13.9

5

0

2

4

6

8

10

12

HMDCControl

Advancure

Dur

omet

er C

hang

e (%

)


38

The Advancure compounds had similar change in 50% modulus to The Advancure compounds had similar change in 50% modulus to the HMDC control compounds.the HMDC control compounds.

50% Modulus Change1 week heat aging in Air at 175C

81% 83%

19%22%25% 25%

0%

10%

20%

30%

40%

50%

60%

70%

80%

90%

HMDCControl

Advancure

50%

Mod

ulus

Cha

nge

(%)


39

The Advancure compounds had similar to higher change in tensile The Advancure compounds had similar to higher change in tensile compared to the HMDC control compounds.compared to the HMDC control compounds.

Tensile Change1 week heat aging in Air at 175C

6% 6%

1%

12%

-8%-10%

-15%

-10%

-5%

0%

5%

10%

15%

HMDCControl

Advancure

Ten

sile

Cha

nge

(%)


40

The Advancure compounds had higher elongation to the HMDC The Advancure compounds had higher elongation to the HMDC control compounds.control compounds.

Elongation Change1 week heat aging in Air at 175C

-25%

-20%

-15%

-10%

-5%

0%

5%

10%

HMDCControl

Advancure

Elo

ngat

ion

Cha

nge

(%)


41

Factory Mixing TrialsFactory Mixing Trials

Gold Key ProcessingGold Key ProcessingKrupp Intermesh 45 LKrupp Intermesh 45 L

Testing Testing –– Gold Key Processing and Gold Key Processing and Chem Technologies LaboratoriesChem Technologies Laboratories

42

Formulation Formulation

VamacVamac®® GG 100.00100.00N774 Carbon BlackN774 Carbon Black 90.0090.00StearicStearic AcidAcid 2.002.00PolyoxyethylenePolyoxyethylene octadecyloctadecylether phosphateether phosphate 1.501.5011--ocadecanamineocadecanamine 0.500.50Di(2Di(2--ethylhexyl) ethylhexyl) sebacatesebacate 10.0010.00DOTG (diDOTG (di--oo--tolylguanidine) tolylguanidine) 4.004.00HMDC (Diak 1)HMDC (Diak 1) 1.501.50OrOrAdvancureAdvancure 2.302.30

Diak 1 and Vamac are trademarks of DuPont.Diak 1 and Vamac are trademarks of DuPont.

43

Testing ProceduresTesting Procedures

Mixing was done in a Krupp 45L intermesh mixer Mixing was done in a Krupp 45L intermesh mixer with a dump temperature of 93with a dump temperature of 93ººC.C.

MDR Rheometer at 177MDR Rheometer at 177ººC, ASTM D 5289.C, ASTM D 5289.

Mooney at 121Mooney at 121ººC, ASTM D 1646.C, ASTM D 1646.

Physical Properties (hardness, tensile, modulus, Physical Properties (hardness, tensile, modulus, elongation). Presselongation). Press--cured 5 minutes at 177cured 5 minutes at 177ººC, post C, post cured 4 hours at 177cured 4 hours at 177ººC. ASTM D 412.C. ASTM D 412.

44

The Advancure compound had slightly higher maximum torque The Advancure compound had slightly higher maximum torque values than the HMDC control compound.values than the HMDC control compound.

MDR Rheometer - Maximum Torque

1.331.401.42

1.49

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

Diak 1 Advancure

Max

imum

Tor

que

(N-m

)

177 C 190 C

45

The Advancure compound had a similar Tc90 cure times to the The Advancure compound had a similar Tc90 cure times to the HMDC control compound.HMDC control compound.

MDR Rheometer - Tc90 Cure Time

3.834.10

2.61 2.65

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

Diak 1 Advancure

Tc9

0 (m

inut

es)

177 C 190 C

46

The Advancure compound has a rheometer curve similar to the The Advancure compound has a rheometer curve similar to the HMDC control but with a higher state of cure.HMDC control but with a higher state of cure.

MDR Rheometer at 177 C

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

0 1 2 3 4 5 6Time (minutes)

Tor

que

(N-m

)

HMDC ControlAdvancure

47

The Advancure compound has a rheometer curve similar to the The Advancure compound has a rheometer curve similar to the HMDC control but with a higher state of cure.HMDC control but with a higher state of cure.

MDR Rheometer at 190C

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

0 1 2 3 4 5 6

Time (minutes)

Tor

que

(N-m

)

HMDC ControlAdvancure

48

The Advancure compound had a similar scorch time to the HMDC The Advancure compound had a similar scorch time to the HMDC control.control.

Mooney Scorch at 121C

5.966.20

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

Diak 1 Advancure

Ts5

(min

utes

)

49

The Advancure compound had a similar Mooney viscosity to the The Advancure compound had a similar Mooney viscosity to the HMDC control compound.HMDC control compound.

Mooney Viscosity at 121C

29.5830.43

20.00

22.00

24.00

26.00

28.00

30.00

32.00

34.00

36.00

Diak 1 Advancure

Ts5

(min

utes

)

50

The The AdvancureAdvancure compound had a similar Shore A compound had a similar Shore A durometerdurometer values to values to the the DiakDiak 1 compound.1 compound.

Shore A Durometer

77.2

78.4

70.0

71.0

72.0

73.0

74.0

75.0

76.0

77.0

78.0

79.0

80.0

Diak 1 Advancure

Dur

omet

er (p

oint

s)

51

The The AdvancureAdvancure compound had a slightly higher tensile than the compound had a slightly higher tensile than the DiakDiak1 compound.1 compound.

Tensile

13.4414.28

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

Diak 1 Advancure

Ten

sile

(MPa

)

52

The The AdvancureAdvancure compound had slightly lower elongation than the compound had slightly lower elongation than the DiakDiak 1 compound.1 compound.

Elongation

220202

0

50

100

150

200

250

Diak 1 Advancure

Elo

ngat

ion

(%)

53

The The AdvancureAdvancure compound had slightly higher 100% modulus than compound had slightly higher 100% modulus than the the DiakDiak 1 compound.1 compound.

100% Modulus

8.13

7.24

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

Diak 1 Advancure

100%

Mod

ulus

(MPa

)

54

Costing & ConclusionsCosting & Conclusions

55

The Advancure curative offers a significant cost savings versus The Advancure curative offers a significant cost savings versus HMDC products.HMDC products.

Cost Index

100

70

80

70

45

0

20

40

60

80

100

120

HMDCSource A

HMDC Source B

HMDCSource C

HMDCSource D

Advancure

Cos

t Ind

ex (r

elat

ive

to H

MD

C S

ourc

e A

)

56

ConclusionsConclusions

The Advancure curative was tested in four different The Advancure curative was tested in four different VamacVamac®® G compounds in two different laboratory G compounds in two different laboratory studies and also in factory trials. Advancure had studies and also in factory trials. Advancure had equal cure and physical properties to the HMDC equal cure and physical properties to the HMDC controls.controls.Advancure can offer significant cost savings Advancure can offer significant cost savings compared HMDC sources currently on the market.compared HMDC sources currently on the market.In a typical VamacIn a typical Vamac®® formulation this cost savings formulation this cost savings could result in a $0.15 to $0.20 a pound compound could result in a $0.15 to $0.20 a pound compound savings.savings.

57

Confidentiality & DisclaimerConfidentiality & Disclaimer

The confidential information, data and The confidential information, data and formulations contained in this document are the formulations contained in this document are the property of Chem Technologies, Ltd and property of Chem Technologies, Ltd and DuPont. No guarantee as to the suitability or DuPont. No guarantee as to the suitability or performance of the data contained in this performance of the data contained in this presentation is made beyond the information presentation is made beyond the information contained herein. contained herein.

Documents

CHEM TECHNOLOGIES, LTD. · 1 Advancure™ Curative for Vamac® CHEM TECHNOLOGIES, LTD. Beyond the obvious from innovation to application Bonnie Stuck – Chem Technologies, Ltd