a and via pre

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A practical and innovative approach leading to structurally stable and tribologically effective polyurea grease via preform thickener 2020 NLGI Virtual Technical Week August 24 – 28, 2020 Presenter: Liwen Wei

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A practical and innovative approach leading to structurally stable and tribologically effective polyurea grease via pre‐form thickener

2020 NLGI Virtual Technical WeekAugust 24 – 28, 2020 

Presenter: Liwen Wei 

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Innovation in Grease : PU Pre‐form Thickener• PUG is a non‐metallic grease with soap like structures, known for its  high temperature stability, low noise characteristic, good mechanical,  oxidation and high‐shear stability, OEM and users’ first choice for premium grease ideal for sealed‐for‐life bearings, ball bearing, electric motors applications, and many more

• PU grease in‐situ manufacturing must deal with toxic  MDI/TDI and hazardous amines ‐ Hamper development & difficult for small‐medium (and new) players

• This Study provides insights into making high performance polyurea grease via pre‐form powder with ease and flexibility

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PU Grease: Opportunities & Challenges• PU grease, 6% market share globally, 29% share in Japan, is  the best option to replace Lithium (65‐75% market share)

• PU grease in‐situ manufacturing must deal with toxic  MDI/TDI and hazardous amines ‐ Hamper development &  difficult for small‐medium (and new) players

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Polyurea & Soap Thickeners are similar, made to form extensive H‐Bond Infrastructures

Lithium: Fibers(Metal base and 12‐HSA)

Polyurea: Platelets  to Fibers (Urea/  [polyurea based)

OBCSC: Spherical  (Calcite)

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Isocyanate Mono and poly amine

MDI Aliphatic & Alicyclic

MDI Aromatic

TDI Aliphatic & Alicyclic

Polyurea Thickeners have much higher H‐bond Forming Tendency with higher Melting Point than Soap Thickeners

Slide 5

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PUG = PUT Powder + Oils + Additives Specialty Additive (SA)

• A: S/P Inorganic + DMTD + FM• B: Ashless Sulfur (Inactive) + DTC• C:  B + S/P Inorganic + FM• D:  DTC + DMTD + FM

Synthetic Base Oil (SBO)• AN 23: Alkylated Naphthalene• PAG 320: Water Insoluble PAG• HSE 320: Biodegradable Complex Ester• DC 220: Di‐capped PAG 

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Stage Two Oil Back, Mill to #2 PUG

Stage One Maximize PUT Gelling

Base Oil‐1 Base Oil‐2

Stage One: Shear Thickening Process (Masterbatch Production)Stage Two: Oil back to desire grease grade (Blending Operation)

PUT to PUG Conversion

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FTIR: PUT‐made PUG versus In‐situ Commercial 

PUG

Slide 8

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FTIR: PUT‐made PUG in Various Synthetic Base 

Oils

Slide 9

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Post Process Milling is Vital to give structurally stable  PUG

5000.00

10000.00

15000.00

20000.00

0 1800 3600 5400 7200

Time (Sec)

Vis

cosi

ty (

cP)

Not milledPartially Milled Fully Milled

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Sample PUT Process SBO % 

Powder# 

Milling P0 P60 P10,000 Oil Sep (100C, 24h)

Dropping Point, C

PUG6 2‐Step AN23 10% 2 278 281 372 0.52% 248

PUG6 2‐Step AN23 10% 4 267 258 308 (P100K)

0.31% 250

PUG6 2‐Step AN23 9% 5 270 269 287 0.76% 246

PUG6 2‐Step AN23 7% 6 274 269 270 0.71% 232

PUG9 2‐Step AN23 11% 2 254 261 294 N/A 276

PUG10 2‐Step AN23 11% 2 269 303 350 N/A 283

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Grease ID Penetration P50K D1831160C/12h

Dropping  Point C

P# Delta P# Delta P#Full cup/cone Half cup/cone Half cup/cone

PUG (In Situ) 279 10 ‐2 315

PUG1 (PUT) 253 8 11 290

PUGA (In Situ) 276 23 140 252

PUGB (In Situ) 269 6 10 308

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Polyurea Grease  for Extreme Lubrication

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Steel Mill Industry Example

Challenges: Bearings experience high temperatures and loads under high speed or super low speedoperation, as well as environments contaminated with water and debris.  (Sounds familiar with Wind turbine?)

Opportunities: PU Grease or OBCSG Grease? Must be Tribologically EffectiveTesting, testing, & Verification

Slide 14

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Tribological Testing to Tackle Extreme Lubrication: Understanding StribeckCurve & Chemistry Dynamics   

• Tribological Effective Solutions • https://en.wikipedia.org/wiki/Extreme_tribology

• Beyond the original machinery design specifications.

• Beyond the original machinery ambient parameters & application in challenging environmental conditions

• Beyond the original lubricant design specification.

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Grease SBO  (ISO)

Total Dosage

Add. Package

S/P Booster

Sulfur EP

DTC/  DMTD FM

PUG9   AN23 7% A x x xLi G AN23 5% B x xPUG9   AN23 5% B x xPUG9  AN23 7% C x x x xPUG9   AN23 7% D x x

Tribological Testing Summary

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Grease SBO  (ISO)

Total Dosage

Add. Package

S/P Booster

Sulfur EP

DTC/  DMTD FM 4‐Ball 

WeldFalex Weld

Ball on Disc Wear

Pin on Disc Wear

4‐Ball AW

PUG9   AN23 7% A x x x 800+ 1750+ Nil Best 0.65LiG AN23 5% B x x 625+ 4500+

PUG9   AN23 5% B x x 315+ 1750+ High   Worst 0.56PUG9  AN23 7% C x x x x 800+ 4500+ High   Better 0.55PUG9   AN23 7% D x x 800+ 4500+ 0.60

Tribological Testing* Summary

Slide 17

*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233

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Grease SBO  (ISO)

Total Dosage

Add. Package

S/P Booster

Sulfur EP

DTC/  DMTD FM 4‐Ball 

WeldFalex P&V

Ball on Disc Wear

Pin on Disc Wear

4‐Ball AW

PUG9  AN23 7% A x x x 800+ 1750+ Nil Best 0.65Li G AN23 5% B x x 625+ 4500+PUG9  AN23 5% B x x 315+ 1750+ High   Worst 0.56PUG9  AN23 7% C x x x x 800+ 4500+ High   Better 0.55PUG9  AN23 7% D x x 800+ 4500+ 0.60

Maximum EP Performance with Mitigating AW/FM Performance : A, C, &D

Slide 18

*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233

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0

500

1000

1500

2000

2500

3000

3500

4000

4500

PUG 9‐AN23 PUG 9‐E320 PUG 9‐G320 PUG 9‐DC220 CommercialPUG‐5%B

PUG 9‐5%B CommercialPUG‐5% S/P

PUG 9‐5%A PUG 9‐5%C

+ 5% B+ 5% B

+ 5% C+ 5% A

+ 5% S/P

+ E320+AN23 + G‐320 +DC‐220

Falex P&V is highly repeatable(Line Contact, Variable Load Stages)

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Grease SBO  (ISO)

Total Dosage

Add. Package

S/P Booster

Sulfur EP

DTC/  DMTD FM 4‐Ball 

WeldFalex P&V

Ball on Disc Wear

Pin on Disc Wear

4‐Ball AW

PUG9  AN23 7% A x x x 800+ 1750+ Nil Best 0.65Li G AN23 5% B x x 625+ 4500+PUG9  AN23 5% B x x 315+ 1750+ High   Worst 0.56PUG9  AN23 7% C x x x x 800+ 4500+ High   Better 0.55PUG9  AN23 7% D x x 800+ 4500+ 0.60

4-Ball AW is not effective(Point contact, fixed Load/Speed)

*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233

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Ball‐on‐Disc: Wear/COF/Wear Tracks

Ball on Disc (Point Contact/Rotating)

Rotary Speed: 16 stages/30s to 4,000RPMForce: 100N Constant

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Ball‐on‐Disc Wear Scars  

Effectively Ranks Base 

Oils and Additives

Additive A: EP with AW/FM Additive B: S‐EP Additive C: S‐EP with S/P Booster

Base Oil 1 ‐ Polyalkylene Glycol Base Oil 2 – Alkylated Naphthalene Base Oil 3 ‐ High Stability Ester

Slide 22

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Pin on Disc Picks the Winner A

• Pin On Disc • (Area Contact/Rotating)• Step One: 100N @50RPM• Step Two: 250N @500RPM

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Conclusion (I):

PUG made via Pre‐Form 

Thickener is a Premium High Temperature 

Grease

• Organic Thickener: Inherently Structurally Stable and Environmentally Friendly 

• Dropping Points: 2600C‐300+0C 

• Outstanding High Temperature Mechanical Stability (160C@D1831)

Slide 24

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Conclusion (II):

PUG is Tribologically Effective with 

EP/Load Carrying& Mitigating AW/FM 

Performance

• Explore use of Special Additives and Synthetic Base Oils

• Achieved 800+Kg 4‐ball Weld & 4500#+ Falex P&V load 

• Ball on Disc and Pin on Disc offer Clear ranking of formulated Polyurea grease

Slide 25

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Thank you & NLGI

Acknowledgement• John Blalock• Steven Mayorga• Jamie Blalock• Argentina Martinez