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Effects of Nanoclay Structure on the Mechanical Properties of EPDM - PowerPoint PPT Presentation


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PJ Yoon*, Marcus Goss Southern Clay Products Gonzales, TX Carl McAfee McAfee Consulting LLC Kennedale, TX Fall 170th Technical Meeting of the Rubber Division, American Chemical Society. Effects of Nanoclay Structure on the Mechanical Properties of EPDM . *pyoon@scprod.com.

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Presentation Transcript
slide1

PJ Yoon*, Marcus Goss

Southern Clay Products

Gonzales, TX

Carl McAfee

McAfee Consulting LLC

Kennedale, TX

Fall 170th Technical Meeting of the

Rubber Division, American Chemical Society

Effects of Nanoclay Structure on the Mechanical Properties of EPDM

*pyoon@scprod.com

slide2

Objectives and Outline

Objectives

  • Current nanoclays performance in rubber, i.e., EPDM
  • Synergetic role of nanoclays with CB or silica

Outline

  • Nanoclay structure and chemistry
  • Cure behavior of nanoclay
  • Nanoclay performance in EPDM
  • Nanoclay compatibilization in EPDM
  • Nanoclay and silica performance in EPDM
  • Summary
  • Acknowledgements
slide3

Nano Tool Benefits

  • Reinforcing filler
  • Increase modulus and tensile strength
  • Improve barrier properties
  • Increase dimensional stability
  • Widen processing window
  • Yield lower density
slide4

10 microns

Microscopy Smectite Clays

SEM Bentonite RockTEM Montmorillonite

1 micron

slide5

~100 nm

Key Properties of Montmorillonite

  • High Modulus: ~170 GPa
  • Shape: Platelet with high aspect ratio
  • Size: 1nm thick, 75-150 nm across
  • Surface Area: >750 m2/g (12g/football field)
  • Charge: unit cell 0.5-0.75 charge; 92 meq/100g clay
  • Swellability

Montmorillonite & Surface Treatment

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Exfoliation

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-OH

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Polymer Matrix Processing

slide6

Treatment Chemistries

* Variations: Quaternary Ammonium Salt, Loading

2M2HT2MBHT 2MHTL8

Investigated in this presentation

HT: Hydrogenated Tallow (~C18)

T: Tallow (partially unsaturated C18)

HTL8: - ethylhexyl

no treatment

MT2EtOH M2HT

slide7

The Processing Challenge

8µmParticle >1 Million Platelets

slide8

The Challenge & Benefit

If the aspect ratio increased from 10 to 30 at 3% volume fraction,

the permeability reduction improved from 84% to 68%.

slide10

Cure Behavior of Organoclay

Peroxide Cure

  • GEO Specialty
  • Inert to peroxide, little change in T90

Standard Package

ZnO: 5

SA: 2

ZDEC: 1.5

Sulfur Cure

  • Surface adsorption

- activator

- accelerator

  • Need to adjust curative
slide11

Compounding and Cure

Compounding (Brabender, 15 min)

EPDM (G8450, G5450) 100

EPDM-MA (Royaltuf 498) Variable

Organoclay (C15A, C20A, C10A) Variable

Antioxidant (Agerite D) 1

* Organoclay : EPDM-MA = 1 : 1

Peroxide Cure (170 C, 18 min)

Peroxide (VulCup 40KE ) 5

Coagent (SR-708) 2

Retarder (Ethanox 703) 0.3

slide12

Tensile Properties of EPDM Nanocomposites

MMT = 5.4 wt%

  • C15A > C20A > C10A in strength & elongation
  • Two long alkyl chains, higher loading favored for EPDM
  • - Maleated EPDM increased strength
slide13

Tensile Balance of EPDM Nanocomposites

With EPDM-MA

  • - Maleated EPDM increased modulus
  • Maleated EPDM made no difference in elongation
  • Homogeneous & higher aspect ratio tactoids
slide14

Tensile Balance as FMMT

* EPDM-MA included

  • - Steep increase in strength as MMT%
  • C15A max strain is higher than C20A
  • Modulus is increased linearlyand
  • identical.
  • - High loading of surfactant favored
slide15

XRD for EPDM Nanocomposites

MMT = 5.4 wt%

  • Current surfactant yieldedintercalated structure in EPDM
  • insignificant change before and after cure
  • insignificant change with maleated EPDM
slide16

TEM Dispersion Quality

* EPDM-MA included

C15A

C20A

- Overall dispersion is excellent

- No significant difference between C15A and C20A

slide17

TEM Dispersion Quality

C10A

2 platelets

5 platelets

  • For C10A, larger and thicker particle lead to fewer # of reinforcing filler
  • Final particle of 2-5 platelets with ~170 nm length leads to 10-30 aspect ratio
slide19

Model Fits

Rod-like Filler

Disk-like Filler

Guth Eq.: aspect ratio ~ 17

Halpin-Tsai Eq.: aspect ratio ~15

Chow Eq.: aspect ratio ~ 40

(Chow Eq. for nylon 6: ~ 100)

(~ 30 % reduction in Permeability)

slide20

100 nm

Pre-dispersed Organoclay

  • Maleated EPDM as host
  • 100 phr masterbatch
  • Homogeneous dispersion
  • Can utilize TSE & other
  • T process < 200 C needed
slide21

Pre-dispersed Organoclay in EPDM

5.4% MMT

  • For C15A
  • TSE low temp favored
  • but not much different

5.4% MMT

  • For C10A
  • TSE low temp favored
  • Significant improvement

*TSE: Twin Screw Extruder

INT: Internal Mixer

H: high shear config.

L: low shear config.

slide23

Compound and Cure

counted EPDM-MA as rubber phase

Silica: Hi Sil 233 (BET 150 m2/g) )

Method 1: Silica masterbatch

Method 2: Direct

Method 3: Silica masterbatch, C15A masterbatch

slide24

TEM Dispersion Quality

CSi-1 (MMT : Silica = 0: 14.3)

Strong aggregate and network

slide25

TEM Dispersion Quality

CSi-5 (MMT : Silica= 3.3 : 11.0)

slide26

Cure Behavior of C15A + Silica

- MH Gradually decrease

- T90 little change

slide27

Tensile Behavior of C15A + Silica

  • - Strength increase up to 6wt% MMT
  • - M100 little change
  • Elong. at break increase up to 4wt%
slide28

Dynamic Fatigue Behavior of C15A + Silica

De Mattia

Method 1 (silica MB)

Method 2 (direct)

  • Exponential increase to over 250 k cycles
slide29

Summary

  • For EPDM, two tail surfactant (2M2HT) was favored in dispersion of
  • organoclay, and tensile properties. High loading of 2M2HT was
  • also favored for EPDM; more organophilic nanoclay is suitable
  • to EPDM.
  • For less compatible organoclay, pre-dispersion in maleated EPDM
  • was greatly effective in enhancing tensile properties. It may be
  • related to loosen tactoid aggregates by maleated EPDM molecule.
  • For mixed C15A and silica fillers, organoclay improved tensile
  • and fatigue properties in EPDM. Apparently, it seems optimum
  • composition exists.
  • Dynamic mechanical test is in progress to understand silica
  • network as a function of MMT. Black and nanoclay also in progress.
slide30

Acknowledgements

  • Prof. Donald Paul at UT
  • Dr. Peter Dluzneski of GEO Specialty Chemicals
  • Steve Henning of Sartomer
  • Steve Chase of Excel Polymers for masterbatches
  • Lanxess, Crompton for providing the material
  • SH Bum at UA, Dr. DH Kim at UT
  • SCP