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Lipid Structural Properties Symposium
Unilever R&D Colworth, UK
16-17th October 02
LATEST TRENDS IN DRY
FRACTIONATION OF FATS
Dr. Véronique GIBON
Fractionnement TIRTIAUX SA
Fleurus - Belgium
RECENT TRENDS IN DRY FRACTIONATION




FRACTIONATION
DRY FRACTIONATION
EQUIPMENTS
WHY FRACTIONATE ?
–
–
–
–
–
–
–
Hydrogenated Soybean Oil
Crude Fish Oil (High w - 3)
Cottonseed Oil
Extra virgin olive Oil
Anhydrous Milkfat
Beef Tallow
Palm Oil
– Palm Kernel Oil

CONCLUSIONS
FRACTIONATION
Fractional distillation
Super-critic extraction
Liquid-liquid extraction
Adsorption
Solvent fractionation
Detergent fractionation
DRY FRACTIONATION
Volatility
Solubility
Solubility
Solubility
Crystallisation
Crystallisation
Crystallisation
KEY OF SUCCESS = SELECTIVITY
• THE SIMPLEST AND CHEAPEST FRACTIONAL CRYSTALLISATION PROCESS.
• “GREEN” TECHNOLOGY.
• SELECTIVITY IMPROVED BY :
•THE MASTERY OF POLYPHASIC AND THERMAL PROPERTIES OF
TRIGLYCERIDES : POLYMORPHISM, INTERSOLUBILITY, SEEDING IN
SUPERCOOLING CONDITIONS.
•DEVELOPMENT OF MEMBRANE FILTER-PRESSES
DRY FRACTIONATION
STEARIN :
Solid fraction
1) CRYSTALLISATION :
CONTROLLED
CRYSTALLISATION OF THE
MELTED OIL,
CONDUCTED ACCORDING
TO A SPECIFIC COOLING
PROGRAM.
OLEIN :
Liquid fraction
2) SEPARATION OF THE CRYSTALLISED OIL :
Vacuum belt
(or drum) filter :
Soft stearin.
Membrane filter
press :
Hard stearin.
Higher yield in olein.
Nozzle centrifuge :
Soft stearin.
Closed and small
space.
EQUIPMENT : CRYSTALLYSERS
Type 1 :
Crystallizing oil
Agitator
Exchange plates
Type 2 :
EQUIPMENT : SEPARATION
Florentine filter :
Scraping of the
stearin cake
EQUIPMENT : SEPARATION
Hermetic membrane filter press :
Discharge of the stearin cakes
EQUIPMENT : SEPARATION
Nozzle Centrifuge :
Patented by GEA - Westfalia
WHY FRACTIONATE ?
Improvement of the oxidative stability.
 Improvement of the cold stability.

• PARTIAL HYDROGENATION + FRACTIONATION (Winterization) :
Oils containing poly-unsaturated fatty acids of polyenic
type : Hydro Soybean, Hydro Fish Oil, Hydro Rapeseed, …
• FRACTIONATION (Winterization) :
Fish oil (High w -3), Cottonseed Oil, Olive oil ...
Human imagination to tailor new products.
 Oriented economical policy.

• SINGLE OR MULTI-STEP FRACTIONATION :
Solid or semi-solid fats :
- Anhydrous Milkfat
- Beef Tallow
- Palm Oil
- Palm Kernel Oil ...
FRACTIONATION (Winterization) : Hydrogenated Soybean OIl
Single fractionation
Multi-step fractionation
Hydrogenated soybean oil
IV : 77
DP : 35°C
Hydrogenated soybean oil
IV : 105
DP : 18°C
Stearin
IV : 91
DP : 32.2°C
Margarines,
shortenings
Olein
IV : 108.3
CT : 7 hours
at 0°C
Salad oil
Hydrogenated soybean oil
IV : 84
DP : 25.8°C
Stearin
IV : 61
DP : 45.1°C
Margarines,
shortenings
Olein
Semi-liquid
IV : 81
shortening
DP : 31.2°C for frying
Second Stearin
IV : 73
DP : 35,0°C
Olein
IV : 88
DP : 18,2°C
CBR
Frying oil
100
SFC = f (T)
Stearin
DP : 34.6°C
Margarines,
shortenings
80
60
Olein
DP : 16.3°C
Frying oil
40
20
0
10
15
20
25
30
35
FRACTIONATION (Winterization) : Fish oil (High w -3)
• Crude Fish Oil A :
IV = 172 - EPA+DHA = 25,26% ; EPA < DHA
Olein :
FFA (C18:1) = 2,05 %
D EPA+DHA > 9 % ; Cold test at least 6 hrs at 0°C
Color - Gardner - = 12
Crystal type A
Stearin :
Temperature
5°C
10°C
15°C
20°C
25°C
35
SFC
32
25
15
11
6
F is h O il A
30
S te a rin A
25
20
15
10
5
0
5
10
15
20
25
30
35
40
• Crude Fish Oil B :
IV = 163 - EPA+DHA = 22,62% ; EPA > DHA
Olein :
FFA (C18:1) = 1,34 %
D EPA+DHA > 12 % ; Cold test at least 4 hrs at 0°C
Color - Gardner - = 10,75
45
Crystal type B
Stearin :
Temperature
5°C
10°C
15°C
20°C
25°C
SFC
40
35
27
21
9
40
Fish Oil B
35
S tearin B
30
25
20
15
10
5
0
5
10
15
20
25
30
35
40
FRACTIONATION (Winterization) : Cottonseed Oil
Neutralized and bleached Cottonseed Oil :
•Winterization at 4°C
•Filtration on Membrane Filter Press
or with Centrifuge
Very Small Crystals
Cottonseed Oil
IV : 109,1
Stearin : S
Filter Press - IV : 92,0 - SFC 15°C : 17°C
Centrifuge - IV : 100,0 - SFC 7°C : 6°C
Temperature
5°C
10°C
15°C
20°C
25°C
SFC (MFP)
30,0
25,5
17,0
1,0
0
Olein : O
Filter Press - IV : 114,8 - CP : - 8,5°C
Centrifuge - IV 116,3 - CP : - 7,5°C
SFC (Cent.)
21,0
14,5
6,5
1,0
0
Cold test at 0°C > 6 hours
FRACTIONATION (Winterization) : Olive Oil
Extra Virgin Olive Oil :
•Filtration on Membrane Filter Press
Second Stearin : S
IV : 63,4
DP : 25°C
First Stearin :
IV : 74,7
DP : 16,4 °C
Second Olein : O
IV : 78,5
First Olein : O
IV : 80,5
SFC (%)
Olive Oil
IV : 79,6
40
35
30
25
20
15
10
5
0
First Stearin
Second Olein
Second Stearin
5
10
15
20
25
30
35
Temperature (°C)
MULTISTEP DRY FRACTIONATION OF
ANHYDROUS MILK FAT (AMF)
AMF : DROPPING POINTS BETWEEN 45°C and 6°C ...
Triple fractionation : the best solution for all qualities of AMF
Hard
Stearin : S
DP : 45°C
AMF
DP : 34°C
Olein : O
DP : 21°C
Third
Stearin : OSS
DP : 32°C
Second (Soft)
Stearin : OS
DP : 26°C
Olein : OSO
DP : 24°C
Recycling
Stearin : OOS
DP : 21°C
Super Olein : OO
DP : 13°C
Top Olein : OOO
DP : 6°C
AMF FRACTIONS : Spreadable or soft butter
SFC (%)
70
60
AMF
50
40
Soft Butter
30
Spreadable butter
20
10
0
5
10
15
Very soft or cooking butter
20
25
30
T e m p e r a t u r e ( °C )
35
MULTISTEP DRY FRACTIONATION OF BEEF TALLOW
Super Hard Stearin : SS
DP : 54°C
Stearin : S
DP : 49°C
Olein : SO
DP : 45°C
Recycling
Beef Tallow
DP : 43.2°C ; IV : 44.2
Second
Stearin : OS
DP : 26.7°C
Olein : O
DP : 18.9°C
Recycling
Super
Olein : OO
DP : 14°C
SFC (%)
Third
Stearin : OOS
DP : 18.1°C
Top
Olein : OOO
CP Mettler : -3°C
100
90
SS
80
S
70
SO
60
B e e f T a llo w
OS
50
OOS
40
O
30
OO
OOO
20
10
°C
0
5
10
15
20
25
30
35
40
Hard fractions ;
Shortenings ;
Margarine ;
Semi-liquid
frying
shortenings;
Salad oils ...
MULTISTEP DRY FRACTIONATION OF PALM OIL
= FRYING OIL ;
COOKING OIL ;
SHORTENINGS ;
MARGARINES ;
SALAD OIL ...
= SALAD
OIL
PALM OIL
IV: 51-53
OLEIN
IV : 57-59
SUPER
OLEIN
IV: 64-66
SOFT
PMF
IV :42-48
= SHORTENINGS ;
MARGARINES ;
COATING ...
= SALAD
OIL
TOP
OLEIN
IV: 70-72
HARD STEARIN
IV : 32-36
Recycling
SUPER
STEARIN
IV: 17-21
= BACKERY
SHORTENINGS ;
MARGARINES ;
VANASPATI ;
MANTECA
SOFT
STEARIN
IV : 40-42
= SUBSTITUTE
OF HYDROGENATED
PRODUCTS
= SHORTENINSG
100
“OLEINS”
HARD
PMF
IV : 32-36
80
60
40
SFC = f (T)
20
= CBE
0
10
15
20
25
30
35
RED PALM LIQUID FRACTIONS, RICH IN CAROTENE
PALM OIL
IV: 51-53
RED COLOUR
OF CRUDE PALM OIL :
b- CAROTENE
OLEIN
IV : 57-59
= SALAD
OIL
DEODORISING AT LOW TEMPERATURE :
REFINED PALM OIL WITH HIGH LEVELS
IN b- CAROTENE : “ RED PALM OIL ”
MULTISTEP FRACTIONATION :
“ RED PRODUCTS ” WITH HIGH OXYDATIVE AND
COLD STABILITIES AND NUTRITIONAL LABEL
SUPER
OLEIN
IV: 64-66
TOP
OLEIN
IV: 70-72
• NB PALM OIL
• RED OLEIN
• RED
SUPEROLEIN
• RED
TOPOLEIN
IV
CP
AOCS
(°C)
CAROTENE
(PPM)
51.9
56.7
21.6
8.1
382
409
63.2
3.3
670
71.3
-2.4
854
RED PALM FRACTIONS : WHICH MARKET ?
PALM OIL
b-Carotene : 382 PPM
OLEIN
409 PPM
STEARIN
280 PPM
NUTRITIONAL LABEL :
- BENEFICIAL EFFECT ON
CELLULAR AGEING.
-PROTECTION AGAINST
CANCER.
• OLEIN , SUPEROLEIN , TOPOLEIN :
SUPER
OLEIN
670 PPM
SOFT PMF
235 PPM
TOP
OLEIN
854 PPM
HARD
PMF
80 PPM
HIGH VITAMINIC SALAD OIL WITH HIGH
COLD AND OXIDATIVE STABILITY.
FRYING OIL (“LOW” TEMPERATURE).
• STEARIN AND PALM MID FRACTIONS :
RICH IN VITAMINS PRODUCTS FOR
DIETETIC USE : MARGARINE,
SHORTENINGS ; CBE.
FRACTIONATION OF PALM KERNEL OIL : CBS
C6-C10
C12
C14
C16
C18
C18:1
C18:2
SFC (%)
PKO
IV 18
PKS
IV 9
PKS
IV 7
Hydrogenated PKS
IV 7 to 0,4 = CBS
7%
48%
16%
9%
2%
15%
2%
6%
53%
21%
9%
2%
8%
1%
4%
55%
22%
9%
2%
7%
1%
4%
55%
22%
9%
9%
0,5%
0%
C12;C14
C18:1
100
90
CBS
80
70
IV 7
60
IV 7 to 0,4
50
IV 9
40
30
IV18
20
10
°C
0
20
25
30
35
40
CONCLUSIONS
It can be difficult to imagine that the mastery and the automatic control of
DRY FRACTIONATION is born only 50 years ago.
In 1959 in BELGIUM a 8T/day dry fractionation unit is installed for the production
of Beef Tallow Olein for frying, still now commercialised as “Blanc de Boeuf”.
In the 60ies and the beginning of 70ies, such types of unit are installed in
MALAYSIA, INDONESIA, AUSTRALIA, LATIN AMERICA and CENTRAL AFRICA
for the fractionation of animal fats, palm oil, AMF and partially hydrogenated
soybean and fish oils.
The fractionation process has been consequently developed,
with a range of different companies entering the market of construction
of dry fractionation equipment.
Lipid Structural Properties Symposium
Unilever R&D Colworth, UK
16-17th October 02
THANKS FOR YOUR
ATTENTION
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http://www.tirtiaux.com