1. Oil Extraction from non-food Oilseeds for Renewable Aviation Fuel Production
PI: Lin Wei
Co-PIs: K. Muthukumarappan, James Julson, Jimmy Gu
Department of Agricultural & Biosystems Engineering
South Dakota State University
March 2015

2. Background
Funded by DOT and SD Oilseeds Council through NC Sun Grant Initiative in Aug
The goal is to economically produce military specific aviation fuels from non-food oil seeds using proven processes.
Non-food oilseed crops including brown mustard, carinata, sunflower, rape, cranbe, camalina, field pennycress, and flax seeds.
Evaluate the best oilseed species and cost-effective oil extraction technologies.

3. Objectives
Investigate solvent extraction , cold press, and novel continuous extraction to develop cost effective technologies for oil extraction from non-food oilseeds
Examine the effects of oilseed crops growth and oil extraction processes on fat acid profile (FAP) of the oils produced
Upgrade the vegetable oils into aviation fuels

4. Methods Solvent (Hexane) extraction Cold press
determine the upper limit of available oil from the oilseeds
screen the best oilseed species
Cold press
To determine optimal conditions for oil extraction
Evaluate economic feasibility of cold press
Novel continuous extrusion extraction
combine high shear extrusion and high efficient solvents
Evaluate economic feasibility of extrusion method

5. Accelerated Solvent Extraction (ASE) Separates Oil and solvent mixture
Run with 10 g of sample
About 15 min oil extraction time
16 ml. solvent consumption
Oil+Hexane
mixture
Hexane
recovered
Oil
ASE System
For oil extraction
RotoVap System
Separates Oil and solvent mixture

6. Carinata oil yield rates by hexane extraction
Treat.
Cond.
Time
(min)
Temp
(°C)
Oil yield rate
(%) 1 40 80
31.50±0.04 2
100
31.67±0.13 3
120
33.10±0.14 4 65
32.70±0.01 5
33.02±0.17 6
33.29±0.13 7 90
32.82±0.31 8
34.40±0.32 9
33.89±0.13

7. Characterization of carinata oils
Time
(min)
Temp
(°C)
Heating value (MJ/kg)
Density (kg/m3)
Viscosity
(cp)
Acid value 40 80
40.01±0.21
923.57±2.12
61.27±1.61
5.58±0.21
100
40.15±0.03
924.73±1.41
65.51±1.12
4.54±0.08
120
40.04±0.20
913.24±1.54
58.45±0.71
5.01±0.38 65
40.29±0.02
930.43±1.36
71.50±0.71
5.04±0.07
40.20±0.41
928.27±1.83
72.75±0.35
4.65±0.17
40.21±0.05
926.58±1.95
66.85±1.98
4.50±0.08 90
40.37±0.13
924.21±1.41
64.15±1.41
4.47±0.04
40.49±0.14
924.51±1.95
72.50±0.71
4.67±0.11
40.42±0.36
922.12±1.41
67.15±1.83
4.49±0.03

8. Cold press for oil extraction
Sunflower
Safflower
Mustard
Flax
Canola
Feeding cone
Motor
Extraction meal
Oil press
Oil
VFD

9. Brassica carinata oil and meal yield
Nozzle dia.
(inch)
Speed (Hz)
Seed quantity (kg)
Meal (kg)
Oil (kg)
Oil yield rate, %
0.2 15 2
1.3
0.7 34 20 35 25
0.3
1.4 33
0.6 32
0.5 27 28

10. Brassica carinata oil characterization Calorific value (MJ kg-1)
Nozzle
(in)
Speed (Hz)
Calorific value (MJ kg-1)
Density
(kg m-3)
Viscosity
20°C
Acid
value
Oil water content (%)
0.22 15
40.40 ± 0.2
872.7 ±8.5
70.0 ± 0.8
1.76 ± 0.2
0.06 20
40.32 ± 0.2
870.7 ±2.8
70.4 ± 1.2
1.78 ± 0.1
0.05 25
40.57 ±0.3
874.6 ±10.4
70.5 ± 1.3
1.73 ± 0.1
0.25
40.19 ± 0.7
878.3 ±6.2
70.3 ± 0.8
1.74 ± 0.1
40.51 ±0.1
874.7 ± 4.9
71.5 ± 1.1
1.80 ± 0.2
0.07
40.47 ±0.1
871.4 ±10.5
71.4 ± 0.9
1.73 ± 0.2
0.28
40.44 ±0.1
875.1 ± 6.3
69.9 ± 0.9
40.36 ±0.3
876.9 ± 11.2
70.5 ± 1.1
40.48 ±0.1
879.5 ± 2.6
69.5 ± 0.7
1.77 ± 0.1

11. Continuous Extrusion-Solvent Extraction
Combine high shear extrusion and high efficient solvents to efficiently extracting oils from different oilseeds for further conversion into aviation fuels.
Using a single screw extruder to determine the upper limit of available oil from the oilseeds
Combine with solvent extraction
Quality analysis of the extracted oils
Equipment: Single-screw extruder (Brabender, Plasti-Corder (PL 2000)

12. Extrusion conditions
Evaluating of the effect of extrusion temperature and rotating speed on oil extraction yield & quality
SAE extracted Canola oils and meals
T (˚C)
SS (rpm) 40 80
120

13. Characterization of canola oil and meal
Parameter
Viscosity
(mPa.s)
Density
(g/cm3)
Water content (%)
Heating value
(MJ/kg)
Oil content of meal
(%)
Temperature
 (°C) 60
0.070 a
0.908 a
0.07 a
39.21 b
10.6 a
(0.00)
(0.01)
(0.20)
(0.54) 80
0.071 a
0.904 a
39.56ab
8.8 b
(0.33)
(1.34)
100
0.901 a
39.64 a
8.6 b
(0.02)
(0.55)
(1.07)
Screw-Speed
(RPM) 40
0.912 a
39.74 a
10.3 a
(0.57)
(0.67)
0.900 a
39.37 ab
8.9 b
(0.14)
(1.42)
120
0.902 a
0.068 a
39.31 b
8.74 b
(0.32)
(1.45)

14. Catalytic cracking of vegetable oils for hydrocarbons
Reaction conditions
Preheat at 450°C
Catalytic cracking at 500°C
~ 1.5 bar (23 psi)
Vegetable oil
Pump
Furnace 1
Preheat
Furnace 2
Catalytic upgrading
Hydrocarbon fuels
Non-condensable gases
Fixed-bed Tubular Reactor
Catalysts used
No catalyst
ZSM-5
ZSM-5-Zn-10
ZSM-5-Zn-20
ZSM-5-Zn-30

15. Converting Camelina oils into hydrocarbon fuels
upgraded oil
Hydrocarbon fuel

16. Product yield rates of oil cracking
The product yields of camelina oil cracking at different conditions

17. Characterization of upgraded oils
Catalyst
Viscosity
(cP)
Moisture
(%)
Density
(g/mL)
HHV (MJ/Kg)
No catalyst
9.50±0.53
0.73±0.04
0.85±0
40.9±0.17
ZSM-5
1.88±0.04
0.16±0.01
0.88±0
41.9±0.08
ZSM-5-Zn-10
1.73±0.01
0.13±0.01
0.86±0.01
42.2±0
ZSM-5-Zn-20
6.14±0.21
0.60±0.08
0.85±0.01
42.7±0.07
ZSM-5-Zn-30
4.20±0.16
0.39±0
0.84±0
43.0±0.12
Zn loading levels affected biofuel properties. The viscosity, moisture content and density decreased but higher heating value increased.

18. GC-MS analysis of oils and biofuels
Fatty Acids of Camelina oil were broken into hydrocarbons
b) upgraded oil
a) Camelina oil
Fatty acids (camelina)
Palmitic acid
Linoleic acid
Linolenic acid
Oleic acid
Stearic acid
Relative contents (Area %) of various compounds in upgraded oil
Compounds
No catalyst
ZSM-5
ZSM-5-Zn-10
ZSM-5-Zn-20
ZSM-5-Zn-30
Fatty acids
36.73
3.44
21.31
22.53
51.53
Hydrocarbons
29.02
40.09
64.15
77.48
45.19
Ketones
- -
1.34

19. Analysis of non-condensable gases
The relative content of non-condensable gases produced from camelina oil cracking over different catalysts

20. Summary
Completed oil extractions from Carinata seeds using cold press and solvent extraction methods.
Characterization of the oils produced.
Upgraded Camelina oil to hydrocarbon fuels that can be used for aviation fuel production
Developed Zn/ZSM-5 catalysts for Camelina oil upgrading.

21. Future plans…
We will use the single screw extruder and green solvents (Terpenes) simultaneously to extract the oils from more oilseeds.
Oil qualities of extracted oil will also be evaluated.
Optimize catalytic cracking for vegetable oil upgrading into hydrocarbon fuels

22. Funding supported by DOT:
Acknowledgements
Team members:
Bishnu Karki (postdoc)
Xianhui Zhao (PhD student)
Umesh Lohani (PhD student)
Sample analyses helped by:
Dr. Douglas Raynie Ms. Changling Qiu and Ms. Shanmugapriya Dharmarajan in the Chemistry Dept. at SDSU
Funding supported by DOT: