The document describes research into developing an advanced calcium-lithium soap grease using minimal lithium hydroxide. Researchers aimed to create a grease with properties similar to lithium soap greases which have high heat resistance and shear stability. The developed grease was found to have a dropping point, mechanical stability, and wear resistance comparable to lithium soap greases. It also showed much less tendency to harden than conventional calcium greases. The grease can potentially help address the increasing demand and costs of lithium hydroxide from batteries and other uses.

1. Development of Advanced Calcium-Lithium Soap
Grease with Minimum Uses of Lithium Hydroxide
Dr. Ashok K. Goyal, N.Parameswaran, Dr. B. Ghosh & Ananda
Sengupta
Balmer Lawrie & Co Ltd
Applications Research Laboratory,
Kolkata

2. SMART WORLD

3.  Smart Phones
 Smart Watches
 Smart T.V.
 Laptops
 Tablets
 Electric Vehicles
SMART WORLD OF SMART TECHNOLOGY

4. Lithium Ion Batteries - Most Popular
 Lithium has the highest electric output per unit weight.
 Battery manufacturers across the world are moving to
lithium.
POWER SOURCE FOR SMART TECHNOLOGY

5. Ceramics and glass Industries - 35%
Rechargeable Batteries - 29%
Lubricating Greases - 8%
Air Treatment - 5%
Polymer Production - 5%
Primary Batteries - 2%
Primary Aluminum Production - 1%
Other Uses - 9%
Above data are taken from U.S. Geological Servey Minerals Yearbook, 2013
Present Uses of Lithium Hydroxide in Different Sectors

6.  Calcium Soap Greases
 Calcium Complex Greases
 Simple Lithium Soap Greases
 Lithium Complex Greases
 Aluminium Complex Greases
 Sodium Soap Greases
 Non-Soap Greases
 Polyurea Greases
 Sulphonate Complex Greases etc.
Types of Lubricating Greases

7. 76.67%
Global Grease Production Survey NLGI 2012

8. 90.88%
Grease Production Survey NLGI 2012 (India and Indian
Subcontinent)

9.  Lesser Availability of Lithium Hydroxide Because of
• Increasing Demand lithium batteries in Smart Devices
• Increasing Demand in Electric Vehicles (EV) and Hybrid
Electric Vehicles (HEV)
• Depleting Natural Sources of Lithium
 The price of Lithium Hydroxide increasing day by day
Present Scenario for Availability of Lithium Hydroxide
for Grease Manufacturing

10.  Project was taken to develop a grease without or lesser uses of
lithium hydroxide exhibiting properties near to lithium soap
greases.
 Calcium hydroxide was chosen as a main base because calcium
soap greases are the second largest produced greases.
 Calcium hydroxide (Hydrated lime) is easily available every
where at cheaper cost.
 Knowledge about the properties of conventional calcium soap
and calcium complex soap greases alongwith the lithium soap
greases is very essential to overcome the drawbacks in newly
developed grease.
Development of Advanced Calcium-Lithium Soap Grease

11.  Calcium soap greases are oldest metal soap greases
 Dropping points of calcium soap grease are in between 90-120
⁰C
 Water is very much essential to stabilize the structure of grease
 Upper temperature limit in any application is only 50-70 ⁰C
 At high temperature water evaporates leading to breaking in
grease soap structure
 Applicable only in less demanding applications
 Fair shear stablity
Calcium Soap Greases

12.  Calcium complex greases have the high dropping point
 On storage at room temperature these greases will slowly
harden when exposed to air.
 The hardening begins at the grease/air interface and slowly
extend further into the bulk of the grease with time.
 This phenomenon is well known as “Case Hardening”
 Calcium complex greases also severely harden under sustained
high temperatures.
 Because of case hardening tendency these greases can not
become popular and acceptable for uses.
 Poor Shear Stability
Calcium Complex Soap Greases

13.  High Dropping Point (High Heat Resistance)
 Excellent Shear Stability
 Smooth Texture
 No hardening Tendency
 Easily Pumpable
 Good water resistant property
 Very good anti-wear performance
 Can be used in Multipurpose applications
 Easy Manufacturing Process
Simple Lithium Soap Greases

14.  High Dropping Point (High Heat Resistance)
 Very good Shear Stability
 Smooth Texture
 No significant hardening Tendency
 Easily Pumpable
 Good water resistant property
 Very good anti-wear performance
 Easy Manufacturing Process
 Can be used in Multipurpose applications
Development of Advanced Calcium-Lithium Soap Grease

15. Manufacturing Process
Similar to the process of simple lithium soap greases or lithium
complex greases
 Fatty Acid / Fat Melting
 Saponification
 Complexation / Chelation
 Cooling
 Additive Mixing
 Homogenization after cooling
Developed grease offers substantial savings in terms of reduced
power and fuel consumption due to lesser processing temperature
required for manufacturing
Development of Advanced Calcium-Lithium Soap Grease

16.  Dropping point of the developed grease
was checked as per ASTM D 566 test
method
 Results were compared with Calcium
Soap, Calcium complex and lithium soap
greases
 Dropping Point of developed grease was
found near to the lithium soap greases
Dropping Point
Development of Advanced Calcium-Lithium Soap Grease

17. S. No. Type of Grease
Dropping
Point, ⁰C
1. Calcium soap grease (Hydration method) 86
2. Calcium soap grease (Anhydrous method) 123
3.
Calcium complex Grease (Conventional
Method)
266
4. Advanced calcium-lithium soap grease 195
5. Simple lithium soap grease 199
Dropping Point Test Data of Different Greases with Developed
Grease
Dropping Point

18. Evaluation of the grease soap structure
stability was carried out by Two Methods
 100,000 Up & Down Strokes (Vertical
Shearing) ASTM D 217
 Rolling Stability Test at Room Temp.
(Rotational Shearing under load)
ASTM D 1831
Stability Against Mechanical Shearing

19. S.
No.
Type of Grease
Penetration
after 60 strokes
@ 25 ⁰C
Penetration after
100000 strokes @
25 ⁰C
Penetration
change after roll
stability test @
rt, 16 hrs.
1.
Calcium soap grease
(Hydration method)
287 353 (+70) +63 Units
2.
Calcium soap grease
(Anhydrous method)
292 366 (+74) +66 Units
3.
Calcium complex Grease
(Conventional Method)
285 376 (+91) +87 Units
4.
Advanced calcium-
lithium soap grease
283 316 (+33) +36 Units
5.
Simple lithium soap
grease
288 315 (+27) +32 Units
Test Data of Mechanical Shearing Stability of Developed Grease and Other
Greases
Stability Against Mechanical Shearing

20. Case hardening tendency of the developed grease has been
checked by
 At Room Temperature in Open Air
 Wheel Bearing Leakage Test at 105
⁰C for 6 hours (ASTM D 1263)
 Roll Stability Test at 82 ⁰C for 96 hours
(modified ASTM D 1831)
Hardening Tendency

21. S. No. Type of Grease
Unworked
Penetration @
25 ⁰C
Penetration @
25 ⁰C after 60
days storage at
rt
Penetration
@ 25 ⁰C after
90 days
storage at rt
1. Calcium complex Grease 274 187 (-87) 171
2.
Advanced calcium-lithium
soap grease
276 273 (-3) 272
3. Simple lithium soap grease 279 277 (-2) 277
Tendency of Case Hardening in Different Greases on Storage at
Ambient Temperature
Hardening Tendency

22. S. No. Test Performed
Test Results
Advanced Ca-Li
soap Grease
Simple lithium
soap grease
1.
Change in penetration after roll stability
at 82 ⁰C for 96 hrs.
+43 units +54 units
2. Wheel bearing Leakage Test
i Oil leakage in grams 0.73 0.88
ii
Change in penetration of grease applied
in bearing hub of the instrument
-9 units -8 units
iii Condition of the grease Smooth Smooth
Tendency of Case Hardening in Different Greases on Storage at
Elevated Temperature
Hardening Tendency

23. Anti-wear properties of the grease was testes by
 Four Ball Wear Scar Diameter Measurement (ASTM D 2266)
RPM - 1200
Time - 3600 Sec.
Temp. - 75 ⁰C
Load - 40 kg.
 Coefficient of Friction by SRV Instrument (ASTM D 5707)
Temp. - 50 ⁰C
Time - 7200 Sec.
Amplitude/stroke - 1
Frequency - 50 Hz.
Anti-wear Characteristics

24. Calcium Soap grease
Advanced Ca-Li Soap Grease
Simple Lithium Soap Grease
Simple Lithium Soap Grease
Advanced Ca-Li Soap Grease
Lithium soap grease with AW/EP additive
Advanced Ca-Li grease with AW/EP Additive
Frictional Torque
with Time During
Four Ball Anti-Wear
Test with and
without Anti-Wear
Additive in different
greases
Anti-wear Characteristics

25. S. No. Type of Grease
Four Ball Wear
Scar Dia, mm
Coefficient of
Friction by SRV
1. Calcium soap grease 0.71 0.119
2.
Advanced calcium-lithium soap
grease
0.57 0.113
3.
Advanced calcium-lithium soap
grease with EP/AW additives
0.46 0.106
4. Simple lithium soap grease 0.55 0.111
5.
Simple lithium soap grease with
EP/AW additives
0.45 0.104
Anti-Wear Characteristics Data of the Greases Received from Four
Ball and SRV Test Methods
Anti-wear Characteristics

26.  Application temperature limit of metallic soap greases are
decided by their dropping/melting points.
 Maximum application temperature of greases are generally 70-
100 ⁰C lesser than their dropping points
 Maximum temperature limit for simple lithium greases is kept
around 100-120 ⁰C
 Similarly Maximum temperature limit for Advanced Calcium -
Lithium soap grease should be around 100-120 ⁰C
 Anti-wear test at SRV instrument has been performed with
ramping of temperature
Heat /Thermal Stability of the Grease Thickener

27. Frequency - 50 Htz
Amplitude/stroke - 1.0 mm
Temperature - Time
50 ⁰C - 30 minutes
80 ⁰C 30 minutes
100 ⁰C - 30 minutes
120 ⁰C - 30 minutes
150 ⁰C - 30 minutes
180 ⁰C - 30 minutes
Heat /Thermal Stability of the Grease Thickener
Temperature Ramping Anti-wear test at SRV

28. Temperature Ramping Anti-wear test at SRV
Anti-wear performance of
developed calcium-lithium soap
grease is very good up to 100 ⁰C
and shows similar behavior as
shown by simple lithium soap
grease.
Heat /Thermal Stability of the Grease Thickener
Calcum Complex Grease
Advanced Calcum –
Lithium Soap Grease
Lithium Soap Grease

29.  Advanced calcium-lithium soap grease is substantially non-
corrosive (with additive) under prolonged wet conditions
 The grease also retains its chemical composition for extended
periods of time under operating conditions.
 Advanced calcium –lithium soap grease does not suffer from loss
of lubricating power due to case hardening
 No significant hardening is associated with an improvement in
the pumpability of the developed grease
Miscellaneous Characteristics

30. S.
No.
Characteristics
Advanced Ca-Li
Non EP Grease
Advanced Ca-Li
EP Grease
Simple Li Soap
Grease
Simple Li Soap
EP Grease
Test Method
1. Appearance
Smooth &
Homogenous
Smooth &
Homogenous
Smooth &
Homogenous
Smooth &
Homogenous
Visual
2.
Worked Penetration, after 60 strokes
(W60)
283 285 288 289 ASTM D 217
3.
Worked Penetration after 100000
strokes (change in Units)
316 (+33) 319 (+34) 315 (+27) 318 (+29) ASTM D 217
4. Dropping Point, °C 195 213 199 198 ASTM D 566
5. Wear Scar Dia, mm 0.57 0.46 0.55 0.45 ASTM D 2266
6. Four Ball Weld Load, Kgs. 160 250 160 250 IP 239
7.
Roll Stability test 16 Hrs @ room
temp., Change in Penetration
+36 Unit +38 Units +35 Units +37 Units
ASTM D 1831
(Modified)
8.
Roll Stability test 96 Hrs @ 82 ⁰C,
Change in Penetration
+43 Units +47 Units +54 Units +57 Units
ASTM D 1831
(Modified)
9.
Wheal Bearing Leakage Test
ASTM D 1263
(i) Oil Leakage in gms, 0.73 0.86 0.88 0.97
(ii) Evidence of abnormal change in
consistency for structure of the
material
No abnormal
change
No abnormal
change
No abnormal
change
No abnormal
change
10.
Hardening on Storage after 3 months,
change in penetration
No significant
hardening
No significant
hardening
No significant
hardening
No significant
hardening
ASTM D 1403
Comparison of the Properties of Advanced Calcium-Lithium Soap Greases with Lithium Soap Greases

31.  Advanced calcium-lithium soap grease has been developed by
using easily available calcium hydroxide as a main alkaline
material with minimal use of lesser abundant lithium hydroxide.
 Excellent tribological properties and suitable for use in industrial
applications.
 Very good mechanical shear stability in both vertical and
rotational motion
 Very good dropping point results which are comparable with the
dropping point of simple lithium soap grease.
 Wear characteristics of the developed grease are closer to the
simple lithium soap greases.
Conclusions

32.  The case hardening tendency has been overcome in the
developed grease
 No significant hardening was also observed at elevated
temperatures
 Equal flexibility to the grease formulators to develop high
performance products by using additives as used in lithium soap
greases.
 Substantial savings in terms of reduced power and fuel
consumption due to lesser processing temperature required for
manufacturing
 Developed grease may be very useful for the grease Industry to
reduce the uses of lithium hydroxide in grease making
Conclusions

33. Acknowledgments
The Authors are sincerely grateful to the Management
of M/s. Balmer Lawrie & Co. Ltd. for giving an
opportunity to present the paper at 18th NLGI-IC
Conference

34. T
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