EFFECT OF DIFFERENT DEGUMMING PROCESSES ON
MINOR COMPOUNDS IN CANOLA CRUDE OIL
Campos, L. A; Chiu, M. C; Basso, R. C; Viotto, L. A; Grimaldi, R; Gonçalves, L. A. G.
Luciene Ara Campos
UNICAMP – Fats and Oils Laboratory
Sydney, 2009
Canola Crude oilCanola Crude oil
Remove
� Phospholipids
�Water
� Colored compounds
� Chlorophyll
� FFA
� Odoriferous compounds
Preserve
� Tocopherol
� Sterols
Deodorized
RefiningIntroduction
ConventionalConventional DegummingDegummingRemovalRemoval ofof phospholipidsphospholipids
Crude oil
Mixing Tank,80°C
Centrifuge
Degummed oil
Citric acid orPhosphoric acid
Phospholipids
Water
Introduction
PhospholipidsPhospholipids
Phosholipids at
presence of non
polar solventes such
as hexane forms
inverse micelle of
20000 Da
Water is added to crude
oil and the polar lipids
start to swell and form
aggregates of high
molecular weight
becomming insoluble
on oil
Introduction
UltrafiltrationUltrafiltration
Polymeric
membrane
Permeate
Degummed oil
crude oil,
miscella or
pre-treated
oil
Retentate
Cross Flow
Introduction
Concetration factor = mass of feed / mass of retentate
TheThe objectiveobjective ofof thethe workwork
� Conventional process
� Ultrafiltration of canola crude oil
� Ultrafiltration of miscella (crude oil+hexane)
�Microfiltration of pre-treated oil
To compare the behaviour of
minor compounds under different
degumming processes such as:
MethodologyMethodology
� Conventional degumming
�Addition of 0.2% (w/w) citric acid solution, 1.8% (w/w) water;
80°C, 30 min in to a mixer, centrifuge.
�Ultrafiltration of crude oil
�Polyvinylidene fluoride (PVDF 30 kDa) membrane, crude oil as
feed, 40°C, cross flow pilot unit ~ 20L, 2.8 bar, tangential velocity
of 6.25 m s-1 and concentration factor of 1.02.
Photomicrography of PVDF
30 kDa membrane amplified
1000 times
MethodologyMethodology
� Ultrafiltration of miscella
� Polyvinylidene fluoride (PVDF 30 kDa) membrane, miscella
30% (oil + hexane, w/w), 40°C, cross flow pilot unit ~ 20L, 1.6
bar, tangential velocity of 3.24 m s-1.
At concentration factor of 1.34 a permeate
flux of 162 L m-2 h-1 was achieved.
Pilot Unit
MethodologyMethodology
�Microfiltration of pre-treated oil
� Pre-treatement: addition 0.3 % (w/w) of phosphoric acid (85%)
and solution of NaOH (20%, w/v) to promote the neutralization of
FFA.
� Polyvinylidene fluoride (PVDF 0.45) µm membrane, 25°C,
“dead end” stirred cell, 2.0 bar, 600rpm and concentration factor
of 1.34.
� Form bigger clusters, can be separated by
microfiltration and this process promote
a degumming and neutralization as a single
Step.
Based on: Hafidi et al, Innovative Food Science and Emerging
Technologies, v. 6; p. 203-212 , 2005.“dead end” stirred cell
MethodologyMethodology
� Analytical determinations based on
American Oil Chemists' Society (AOCS) Methods
� Crude oil characteristics:
• Moisture: 0,24 %
• Phospholipids: 405 (mg kg-1) of phosphorus
• Color Lovibond (Yelow / Red): 70 / 3,8
• Chlorophyll: 12,7 (mg kg-1)
• Tocopherol: 755 (mg kg-1)
ResultsResults –– PhospholipidsPhospholipids
59,0
17,3
96,8 99,0
0
10
20
30
40
50
60
70
80
90
100
Conventional
Degumming
Ultrafiltration
crude oil
Ultrafiltration
miscella
Microfiltration
pre-treated oil
Percent reduction of phospholipids
(%)
ResultsResults –– MoistureMoisture
54,258,3
95,8
75,0
0
10
20
30
40
50
60
70
80
90
100
Conventional
Degumming
Ultrafiltration
crude oil
Ultrafiltration
miscella
Microfiltration
pre-treated oil
Percent reduction of moisture
(%)
ResultsResults –– RedRed ColorColor ((carotenscarotens))
31,6
13,2
39,5
34,2
0
5
10
15
20
25
30
35
40
Conventional
Degumming
Ultrafiltration
crude oil
Ultrafiltration
miscella
Microfiltration
pre-treated oil
Percent reduction of red color (carotens)
(%)
18,9
23,6
31,5
36,2
0
5
10
15
20
25
30
35
40
Conventional
Degumming
Ultrafiltration
crude oil
Ultrafiltration
miscella
Microfiltration
pre-treated oil
Percent reduction of Chlorophyll
Results Results –– ChlorophyllChlorophyll
(%)
ResultsResults –– TocopherolTocopherol
729
786
776
723
755
690
700
710
720
730
740
750
760
770
780
790
Conventional
Degumming
Ultrafiltration
crude oil
Ultrafiltration
miscella
Microfiltration
pre-treated oil
Canola crude
oil
Total tocopherol content (mg kg-1)
ConclusionsConclusions
• The use of membrane process results in better
retention of phospholipids, moisture, red color
(carotens) and chlorophyll when comparared to
conventional degumming process
• The ultrafiltration either with crude oil or miscella
used as feed showed total preservation of tocopherol
• The process which uses processing aids (NaOH or
phosphoric acid) such as conventional degumming
and microfiltration of pre-treated oil showed lost of
tocopherol
ACKNOWLEDGMENTS
Work Team
THANK YOU!
(OBRIGADO!)
Photo: John Woudstra
