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A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis,...

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A Statistical Compatibility A Compatibility A Devulcanized Polypro P. Mutyala, Department of Che University of Water IPR -201 Study Of The And Curing Of And Curing Of d Rubber And opylene C. Tzoganakis emical Engineering, rloo, Ontario, Canada 1 1, UW, ON 1 IPR 2011
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Page 1: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

A Statistical Compatibility ACompatibility A

DevulcanizedPolypro

P. Mutyala, Department of Che

University of Water

IPR -201

Study Of The And Curing OfAnd Curing Of

d Rubber And opylene

C. Tzoganakisemical Engineering,

rloo, Ontario, Canada

11, UW, ON1

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Page 2: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

DEVULCANIZATION

* C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13, (2007)2

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Page 3: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

OutOut

• IntroductionObj ti• Objectives

• ExperimentalExperimental• Results• Conclusions

lineline

3

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Page 4: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

IntrodIntrodi f• Review of work on blen

rubber and plastics

• Role of compatibilizersp

• Cure compatibilization• Cure compatibilization

• Mixture designs

uctionuctioni inding devulcanized

s

nn

4

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Page 5: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

ObjecObjec

To statistically evaluate:

1. The compatibility brubber and Polyprorubber and Polypro

2. Compatibilizing effi

ctivesctives

etween devulcanized opylene (PP)opylene (PP)

iciency of sulphur curing

5

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Page 6: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

ExperimA. Materials:

31 01 (• PP - PP31KK01 (MFI=5America , TS 24 MPa and ED l i d R bb T• Devulcanized Rubber- TreaEB of 388%

• Sulphur (S) and zinc oxid• Sulphur (S) and zinc oxidSigma Aldrich and Fischer

• Stearic acid (St A) andStearic acid (St. A) andWestern Reverse Chemical

• Dicumyl Peroxide (DCP)-99y ( )

mental

)5), Lyondell Basell, NorthEB of 7%

d b d TS 9 MP dad based, TS= 9 MPa and

de (ZnO) are supplied byde (ZnO) are supplied byScientific respectively.

d TBBS are supplied byd TBBS are supplied byCo.

9% was by Sigma Aldrich.y g

6

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Page 7: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

ExperimExperimB. Procedure:

Mixing: Rheomix 3000 tt h d t H k Rh d 90

Mol40 0attached to Haake Rheocord 90

, 180°C, 80 rpmDR, PP, ZnO, St. A, Curing package

40,0

mentalmental

lded - 180 °C, 000 i

Instron 000 psi tensiometer

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Page 8: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Experi

C Experimental design -CoC. Experimental design -Co• Variables and constraint

20% 60% S: 0 5% 4% T20%- 60%, S: 0.5%-4%, T• ZnO and St. A were assum

i hi h hranges in which the experhence were kept constant

• Another set: 3% DCPblends DR: PP 60:40, 70:3

mental

onstrained Mixture Designonstrained Mixture Designs – DR: 40% - 80%, PP:TBBS: 0 5% 4%TBBS: 0.5%- 4%.med to be sufficient for thei i d driment was carried out and

and 2% S added to the30 and 80:20.

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Page 9: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

ExperimExperimData points

Experiment No. 1 2 3 4 (

Components

DR % 75.50 40.00 40.00 57

PP % 20.00 52.00 59.00 37

Sulphur % 0.50 4.00 0.50 2.2Sulphur % 0.50 4.00 0.50 2.2

TBBS % 4.00 4.00 0.50 2.2

ZnO % 1.72 1.72 1.72 1.

St. A % 1.15 1.15 1.15 1.

mentalmental

(3) 5 6 7 8 9

.75 40.00 79.00 72.00 40.00 75.50

.75 55.50 20.00 20.00 55.50 20.00

25 4.00 0.50 4.00 0.50 4.0025 4.00 0.50 4.00 0.50 4.00

25 0.50 0.50 4.00 4.00 0.50

72 1.72 1.72 1.72 1.72 1.72

15 1.15 1.15 1.15 1.15 1.15

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Page 10: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults andd Discussiond Discussion

Tensile Strength

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Page 11: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults andd Discussiond Discussion

Elongation at break

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Page 12: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults andIf x = DR content %, y = PP c, y

• TS: Dosages of DR, PP, sbetween ‘DR + PP’ and ‘DRTS = + 3.0*x + 11.9*y + 4614 79*( 012)*x 148 06*( 0114.79 (-.012) x - 148.06 (-.01

• EB: Dosages of DR, PP anEB: Dosages of DR, PP anPP’, and ‘DR+ S’ seem signifEB = + 35.6*x + 7.7*y - 102 4*( 01)* 1 *( 012)*27.4*(-.01)*x + 15.7*(-.012)*z

d Discussiond Discussioncontent %, z = S content %), )

sulphur (S) and interactions+ S’ seem significant.

6.9*z - 9.89*x*y - 36.50*x*z +12)*z 0 112) z - 0.1

nd interactions between ‘DR+nd interactions between DR+ficant.0.0*z - 42.49*x*y-16.42*x*z +

0 0z - 0.012

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Page 13: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults and• The significant negativeThe significant negative

and EB - a statistic‘incompatibility’ betweeincompatibility betwee

Th i i fl• The negative influence oEB - Sulphur cure sy

ibilicompatibilizer.

d Discussiond Discussioninfluence of DR+PP on TSinfluence of DR+PP on TS

cal representation of theen DR and PP phasesen DR and PP phases.

f ‘DR S’ b h TS dof ‘DR + S’ on both TS andystem is not an effective

13

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Page 14: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults andd Discussiond Discussion

Tensile Strength

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Page 15: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results andResults andd Discussiond Discussion

Elongation at breakg

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Page 16: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

Results and525

500

600

400

500

oper

ty

199

300

nge

in a

pro

199

100

200

rcen

t ch

an

0

100

60 7

Per

-44-100

60 7

DR% (rema

d Discussion‘Sulphur cure’ versus p‘peroxide/sulphur cure’(3% DCP and 2% S )

T.SE B179

67

E.B

3067

70 8070 80

aining being PP%) 16

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Page 17: A Statistical Study Of The Compatibility ACompatibility ......DEVULCANIZATION * C. Tzoganakis, “Method of Modifying Crosslinked Rubber”, Patent Number US 7189762 B2, March 13,

ConcluConclu• A mixture design approa

the compatibility bthermoplastic elastomer

• DR and PP matrix haveto be mutually incompaty phas been shown to bcompatibilizer.

• Peroxide/ sulphur cupromising properties anpromising properties ancompatibilizer.

usionsusionsach can be used to analyzeetween phases in a.

e been proven statisticallytible. Sulphur cure systemp y

be ineffective as a cure

ure system has shownd a better option as a cured a better option as a cure

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