RS-CLARE - Vosolub

New formulations of sunflowerbased bio-lubricants with high
oleic acid content
Dr. Amaya Igartua,
Fundación TEKNIKER, IK4-TEKNIKER,
[email protected]
1
BIOLUBRICANTS
Plant based lubricants have a number or inherent
properties that give them advantages over petroleum oils :
 reduce impact on human health and environment
 use of renewable resources
But , first of all :
 Technical performances are needed for the wide range of
applications
 COST has to be under control !
 fats and oils have to be managed,…… « differently »
2
BIOLUBRICANTS : REQUIREMENTS
One of the most important barriers to the adoption of biolubricants onto the
market is their higher price compared to mineral oil based lubricants. In order to
improve the market penetration of biolubricants, it is therefore necessary to
decrease their purchase cost.
The formulations tested in VOSOLUB project use new bases (developed in the
framework of IBIOLAB project) that are obtained from:


A new variety of oil seeds: very high oleic sunflower seeds give an oil with a very
good resistance to oxidation and good flow properties.
A new refining process: a soft refining process is used instead of complete and
classical refining (reduction of the processing costs due to the tailoring of refining
to oils and elimination of useless steps).
The new variety of oil seeds in combination with the soft refining process allow
to obtain base oils with high stability, with a reduced impact on the environment
and at a lower cost compared to polyolesters.
3
VOSOLUB PROJECT : OBJECTIVES
Creating an active European SMEs network specialized in biolubricants production
ensuring the supply of the very high oleic sunflower base oil at a competitive market
price.
Testing under real operating conditions formulations of sunflower-based biolubricants
with high oleic acid content. These formulations (including hydraulic fluids, greases, and
neat oil metal-working fluids) are being tested in three European demonstrating sites.
Evaluating and comparing the technical performance and environmental impacts of the
sun-flower-based formulations with the corresponding mineral ones.
Fostering the transfer of the VOSOLUB results at the European scale through a
dissemination plan relying on an information campaign promoting the use of biolubricants
4
VOSOLUB PROJECT: PARTNERS
VOSOLUB PROJECT: PARTNERS
Raw material production and supply
Agricultural cooperative in southern France
Sunflower seeds production and supply
Crushing and refining company, producer of vegetable oils. Vitrolles, FR
Refined very high oleic sunflower oil supplier
Biolubricant formulation and field demonstration test
Specialist Lubricants Manufacturer specialized in Rail, Oil & Gas, Steel,
Marine and Automotive lubricants. Liverpool, UK.
►Development of rail grease application
Company specialized in high performance lubricants, and industrial fluid
servicing.
►Development of cutting oil application
Chemical company with a long background in the field of research and
production of process lubricants and greases. Barcelona, Spain.
►Development of hydraulic fluids application
6
VOSOLUB PROJECT: PARTNERS
Technical support
French Research & Technical Centre for Fats & oils industries.
►Analytical assessment of based oil
Control and research laboratory working in the field of lubricants,
fuels, industrial and automotive products.
►Validation of specification for lubricant application and Eco label
Spanish technological center specialized in lubricants and tribology.
►Performance tests on biolubricants
Belgium association that promotes the use of biomass for non-food
applications.
►Dissemination of results
7
Production of the Lubricant
Harvest of seeds the 20th of September 2012
Selection of seeds with high oleic content
25 T of seeds have been sent in accordance to their
oleic acid content around 90%
For assessment of Crude and soft refined oil specification
(analytical aspects)
BFB
5 L of crude & 10L of soft refined oil
ITERG
2L of soft refined oil & 2L of food refined oil
TEKNIKER
1L of soft refined oil
For pre-test of lubricant formulation
MOTUL
100 L of soft refined oil
RS CLARE
25 L of soft refined oil
BRUGAROLAS 10 L of soft refined oil
For assesment of soft refining process
ITERG
1T of crude oil
For production of Ethyl ester
3 T (for ethyl ester production for MOTUL
ITERG
final formulation of lubricant)
For production of biolubricant for demonstration
MOTUL
2 T of soft refined oil
RS CLARE
1,5 T of soft refined oil
BRUGAROLAS 4.5 T of soft refined oil
Crushing of seeds
Soft refining of Crude oil
Sending of soft refining oil to partners
8
Production of the Bio-Lubricants
Use of soft refining process after a classical crushing step to obtain VHOSO oil
 Less energy
 Less by product
Cost of oil quite
 Positive impact on environmental aspect (ACV)
reasonable for application
forecasted
PH's refining
ITERG's identification
Crude VHOSO
E12-9526
Soft refined VHOSO Refined VHOSO
E12-9527
E12-9528
FFA %(m/m)
0,7
0,04
0,03
PV meqO2/kg
Phosphorus (mg/kg)
4,9
99,5
3,6
<3
2
<3
Rancimat (110°C, 10L/h)
Nd
25,6
28,7
Iron (mg/kg)
Cupper (mg/kg)
0,75
0,016
Nd
Nd
Nd
Nd
Tocopherols content (mg/kg)
803
691
707
% of C 18 : 1 cis
89,1
87,5
88,0
Characteristics of base oil
use in VOSOLUB
9
Specifications for Soft refined VHOSO as raw
material
•
•
•
•
•
•
•
•
Oxidation
Wear
Corrosion
Compatibility
Biodegradability
Toxicity on algae
Toxicity on daphnia
Toxcity on fishes
•
•
•
•
Performance
Properties
Physicochemical
Properties
Impact on
environment
Surface
Properties
Composition
Viscosity
Cold properties
Hot properties
• Foaming
• Air release
• Demulsibility
Evaluation and Demonstration of technical and
environmental performances (ISO 15380,…)
VHOSO Base oil characteristics
VHOSO Base oil characteristics
Soft refined VHOSO is easily
biodegradable and
non toxic on aquatic organisms
Algae growth inhibition OECD 201 – 72 hours
EC50 > 1010 mg/l (WAF)
Acute Immobilisation test on Daphnia OECD 202 – 48 hours
EC50 > 1010 mg/l (WAF)
Acute toxicity on fishes OECD 203 – 96 hours
LC50 > 1010mg/l (WAF)
Ultimate biodegradability OECD 301B – 28 days
83,7 %
Production of the Bio-Lubricants
 Application: Hydraulic Fluids
 Volume: 45000 L
 Application: Curve side-of-rail lubricant
 Volume:
 50kg Initial pilot plant batch
 1000kg batch scheduled for the trials
 Specificity: Ecologically safe, biodegradable lubricant for an application that has total loss
to the environment, while maintaining existing performance levels
 Application: Cutting oil
 Volume: 2500 L
 Specificity: Biobased products with high and long-term performances

and a safe HS profile
14
BRUGAROLAS
HYDRAULIC FLUID
BRUGAROLAS
OXIDATION STABILITY (DSC)
The oxidation stability of the new developed base has been measured by
means of the DSC test (Differential Scanning Calorimetry)
The Onset parameter is the temperature at the oil oxidation starts
Dynamic Method



Temperature range 50 to 500ºC at 10ºC/min rate
Crucible Al with cover of 40µl
Atmosphere 20 bar oxygen pressure
 Samples


Very High Oleic Sunflower oil refined VHOSO VOSOLUB
VOSOLUB HYDRAULIC OIL
BRUGAROLAS
OXIDATION STABILITY (DSC)
VOSOLUB DEVELOPED HYDRAULIC FLUID Vs. IBIOLAB FLUIDS
Sample name
VHOSO (Base oil)
VOSOLUB
VOSOLUB
HYDRAULIC FLUID
MINERAL OIL
Oil
VOSOLUB Base Oil
VOSOLUB developed
Hydraulic fluid
Reference mineral
hydraulic fluid
(Ibiolab)
HFBSA-1 (Brugarolas)
HFBSA-2 (Brugarolas)
HFBSA-3 (Brugarolas)
Ibiolab developed
hydraulic fluids
Dynamic method Isothermal (160ºC)
ONSET (º C)
Onset (min)
185
-
228
23
213
64
227
19
211
13
213
20
BRUGAROLAS
Ball on disc Abrasion Tests (Rotational motion)
Friction coefficient
0,16
0,14
0,12
µ
0,1
0,08
0,06
0,04
0,02
Time (s)
0
0
1000
2000
3000
4000
BESLUX HIDRO HV46
Testing Conditions





Ball: Ceramic
Disc: Steel
Time: 165 min
Speed: 3,2 m/s
Load: 30lb
InitialTemperature: 25ºC
6000
7000
8000
9000
BESLUX HIDRO-ECO 46
TEMPERATURE (ºC)
80
70
60
50
ºC

5000
40
30
20
10
Time (s)
0
0
2000
4000
BESLUX HIDRO HV-46
6000
8000
BESLUX HIDRO-ECO 46
10000
BRUGAROLAS
ball on disc Abrasion Tests (Rotational motion)
ECO 46
BALL WEAR
DISC WEAR
REFERENCE (HV-46 )
It can be concluded that under the selected testing conditions the new developed
hydraulic fluid BESLUX HIDRO-ECO-46 has better behavior than the reference mineral
based hydraulic fluid BESLUX HIDRO-HV-46, in all the measured parameters (Friction
coefficient, Increase of temperature and wear)
BRUGAROLAS
FZG Scuffing test - DIN ISO 14635-1 (test method A/8,3/90)
Evaluation of the load capacity of oils:
Special gear wheels are run in the lubricant under test,
at a constant speed for a fixed time, in a dip lubrication
system. Loading of the gear teeth is raised in stages.
After load stage 4 the pinion gear teeth flanks are
inspected for damage and any changes in tooth
appearance are noted
Results and concusions:
•
•
•
Failure load stage: >12
Pinion torque at failure load stage: >534,5 N/m
BELSUX HIDRO-ECO 46 oil has reached the
maximum load stage defined in DIN ISO 14635-1
without scuffing failure appearance.
RS-CLARE
Vosolub Lubricant manufactured as an NLGI number 1 grease
Specially designed for Curved Rail
Sheffield Supertram
Vosolub Trial set up September 2013
21
RS-CLARE
Light Rail/Tram system
Lubricator
LB Foster PW37
RS-CLARE
Vosolub Curve Rail Grease
Two MC3 GDU’s with grease pumping out
Close up of GDU
(grease distribution unit)
RS-CLARE
GREASE
RS-CLARE
Wheel/Rail simulation tests (“twin-disc” configuration)
Twin Disc Tribometer
Speed
Slip rate
Máx. Par
Normal Load 50 – 5000 N
Disc dimension
Engine Powder
100 – 4000 rpm
0 – 100%
0 Nm
10 – 50 mm
1 kW y 0.5 kW
Testing Conditions
Testing conditions
Test 1
Test 2
Load
1000N
2000N
Pressure
1.3GPa
1.8 GPa
Rail speed
950 rpm
Wheel speed:
1000 rpm
Sliding %
Wheel
5,1%
Time
8 hours
Number of cycles
480000
Contact
3 mm
RS-CLARE
Wheel/Rail simulation tests (“twin-disc” configuration)
Rail Wear Reference XP788
Rail Wear VOSOLUB
RS-CLARE
Wheel/Rail simulation tests (“twin-disc” configuration)
Conclusions
•
•
•
•
The friction coefficient of the new developed VOSOLUB grease is much lower than
the friction coefficient obtained with the reference grease. Not great differences
have been observed in the friction coefficient in the different testing conditions.
During the first test the wheel and the rail suffer an initial wear mechanism of
surface polishing. But when increasing the load, a fatigue phenomena appears,
which translates into the pitting and micro-pitting suffered by the samples
Concerning the wear, the mineral based XP788 grease suffers higher wear than
the new developed grease in terms of mass loss, and also suffer much more
pitting and micropitting.
It can be concluded that under the selected testing conditions new developed
VOSOLUB grease has better behavior than the reference mineral XP788 grease.
Neat metal working fluids
MOTUL
MOTUL
Cutting fluids-Neat Oils
OBJECTIVE: formulating an high performance neat cutting oil
based on sustainable feedstock comparable with the best
available mineral oil based technology
Test Performance for validation of the developed cutting fluid
 Simulation test performed with the Tapping Torque Machine (ASTM
5619 standard)
 Turning tests on a real lathe CNC machine
MOTUL
TAPPING TORQUE TESTS
Tapping Cutting Tests-Based on ASTM D5619 Standard Test Method
Ref. Fluid Torque (Nm)
X 100 =
Test Fluid Torque (Nm)
Test conditions
Steel
Titanium
Tapping speed
M10X1,5mm
HSS
242 rpm
Ti6Al4V (grade 5),
(Ø9,75mm)
M10X1,5mm
HSS
250 rpm
Temperature
Room temperature
Room temperature
Specimen nut
Specimen tap
F1508-51 (Ø8,53 mm)
Efficiency
MOTUL
TAPPING TORQUE TESTS
Relative Efficiency of the neat oils when testing with Steel
Torque (Nm)
1
2
3
4
5
Mean
value
Efficiency
(%)
Mineral (REF)
4,04
4,37
4,15
4,2
4,4
4,234±0,15
100
VOSOLUB
4,29
4,73
4,21
4,43
4,5
4,426±0,20
97
Mineral (REF)
4,42
4,18
4,35
4,41
4,5
4,376±0,13
100
Lubricant
Tapping Cutting (Steel)
% Relative efficiency
120
100
100
97
Mineral (REF)
VOSOLUB
80
60
40
20
0
MOTUL
TAPPING TORQUE TESTS
Relative Efficiency of the neat oils when testing with Titanium
Torque (Nm)
Lubricant
1
2
3
Mean value
Efficiency (%)
23,8
21,06
20,71
21,85±1,69
100
VOSOLUB
20,21
23,46
29,09
24,25±4,49
98
Mineral (REF)
24,32
23,98
28,43
25,57±2,48
100
Mineral (REF)
Tapping Cutting (Titanium)
% Relative efficiency
120
100
100
98
Mineral (REF)
VOSOLUB
80
60
40
20
0
TAPPING TORQUE TESTS
MOTUL
CONCLUSIONS OF TAPPING TORQUE TESTS

Due to the difficulties of machining Titanium it has been necessary to test
specimens with higher diameter (9,75mm instead of the 8,53 mm of the
standard steel specimens)

The torque values obtained with Titanium specimen are much higher
than those obtained with Steel (around five times higher).

Under the selected testing conditions (Steel and Titanium) it can be
concluded that no significant differences between the tested fluids
can be observed.
TURNING TESTS
TURNING TESTS ON A REAL CNC MACHINE

Machine tool: CNC CMZ lathe TL 15 M 8 (5000
rpm, 14 Kw)

Machining process: external turning of bars with
2 different cutting oils

Machining material: Alloy steel 1.6580
(30CrNiMo8) (quenching and tempering to
31HRc) bars of diameter 110mm and length 260
mm
Cutting Conditions
Values
Cutting speed (Vc)
100-300 m/min
Feed rate (F)
0.1-0.4 mm/rev
Depth of cut (Ap)
0.3- 0.4 mm
MOTUL
TURNING TESTS
MOTUL
TURNING TESTS ON A REAL CNC MACHINE
Cutting Tool

CNMG 120408 inserts from
Mitsubishi with a CVD coated
Grade for steel
Monitoring variables:

Tool flank wear (VB) obtained by contact microscope Keyence VH-5901

Work piece surface quality (Ra) obtained by portable perfilometer Mitutoyo
SJ-201P
Tool life criterion:

ISO 3685:1993 standard with a flank wear (VB)
limit of 0.3 mm or

Machining time of 20 min when the previous
threshold is not reached.
MOTUL
TURNING TESTS
TOOL FLANK WEAR (Depth of cut 0,3mm)
Real values
Mean values
MOTUL
TURNING TESTS
Workpiece Roughness (Depth of cut 0,3mm)
Real values
Mean values
MOTUL
TURNING TESTS
TOOL FLANK WEAR (Depth of cut 0,5mm)
Real values
Mean values
MOTUL
TURNING TESTS
Workpiece Roughness (Depth of cut 0,5mm)
Real values
Mean values
TURNING TESTS
MOTUL
Flank wear (Depth 0.3mm)
VOSOLUB
MINERAL
t=0
t=6,15
t=12,02
t=20,30
TURNING TESTS
MOTUL
Flank wear (Depth 0.5mm)
VOSOLUB
MINERAL
t=0
t=6,28
t=12,35
t=14,33
TURNING TESTS
MOTUL
CONCLUSIONS OF TURNING TESTS

Turning tests under 2 different cutting conditions with the two studied cutting
oils have offered similar results concerning tool wear, which is the main
aspect to take into account regarding the general machining performance.

Turning tests under 2 different cutting conditions with the two studied cutting
oils have offered similar results regarding workpiece roughness in the
case of Doc:0.3mm and some small variations in the case of Doc:0.5mm
where the piece is supporting more aggressive cutting conditions but this
difference could be assumed within the scatter range generally
associated with this kind of machining tests.

Therefore the objective of formulating an high performance neat cutting oil based
on sustainable feedstock comparable with the best available mineral oil based
technology has been achieved
General conclusions
In the frame of VOSOLUB Project, it has been realised a
soft refining process for the high oleic sunflower oil able
to reduce the processing cost without loosing
performance.
3 Applications are being developed based on this oil :
hydraulic oils, greases and cutting fluids, showing up to
the moment some promising results.
43
With support of
45

Download Report