Crude Palm Oil Refining Process by Gibon 2007

Eur. J. Lipid Sci. Technol. 109 (2007) 315–335 DOI 10.1002/ejlt.
200600307 315
Véronique Gibon Palm oil refining

Wim De Greyt
Marc Kellens
Crude palm oil is rich in minor components that impart unique nutritional properties.
De Smet Technologies The most relevant are tocopherols and tocotrienols (vitamin E) and carotenoids (a- and
and Services, b-carotene). Palm oil is generally refined by the physical process, which is preferred
Zaventem, Belgium over the chemical process since high acidity (up to 5%) can lead to excessive loss of
neutral oil in the soapstock after alkali neutralization. The quality of the crude oil is to be
considered as it can greatly affect the efficiency of the refining process and the quality
of the end-products. The deterioration of bleachability index (DOBI) is a good indicator
of the capability of palm oil to be successfully refined. Beside commodities, especially
refined oils open a market for new high-quality products like golden palm oil, red palm
oil, white soaps, fractionated products (CBE), etc. Optimization of the deodorization
technology and of the process conditions for a maximal retention of natural char-
acteristics without affecting the quality of the palm oil is an important challenge.
Keywords: Chemical refining, physical refining, crude palm oil quality, DOBI, nutri-
tional quality, carotenoids, tocopherols, tocotrienols.
1 Introduction able minor constituents in the oil with the least possible
damage to the acylglycerols and minimal loss of the
The production of crude oils and fats, by normal opera- desirable constituents.
tions of rendering, crushing or solvent extraction, results
in the incorporation of variable amounts of minor com-
ponents like free fatty acids (FFA), partial acylglycerols, 2 Minor components of crude palm oil
phosphatides, sterols, tocopherols, tocotrienols, hydro-
carbons, pigments, vitamins, sterol glycosides, protein As a fruit flesh oil, palm oil is produced at the oil mill by
fragments, traces of pesticides, dioxins, heavy metals, cooking, pressing and clarification. The quality of the
etc. Not all constituents are undesirable: tocopherols and crude oil will affect the efficiency and yield of refining and
tocotrienols, for example, perform the important function the quality of the fully processed product.
of protecting oil against oxidation and possess vitamin E
activity. The sterols, on the other hand, are colorless, heat The minor components of palm oil have been reviewed by
stable and, for all practical purposes, inert; hence, they Berger [1]; beside triacylglycerols, the remaining compo-
pass unnoticed unless present in unusually large nents consist in a multitude of chemical entities, some of
amounts. Unsaturated fatty acids (mainly the poly- them having actual or potential commercial value.
unsaturated ones) are particularly sensitive to oxidation;
Review Article
this sensitivity is amplified by the presence of metal tra-
ces like iron or copper which should be removed. Phos- 2.1 FFA and partial acylglycerols
phatides in the crude oil need to be removed because
In over-ripe fruits or during harvesting, a very active
they will interfere within further processing.
lipase, most probably originating from yeast cells, will be
responsible for increased production of FFA and partial
To become acceptable for human consumption, most acylglycerols. While it is possible to obtain a crude palm
oils must be purified. Mainly, a light color, a bland taste oil with only 0.02% FFA from fresh ripe fruit, the acidity of
and a good and oxidative stability are required. To commercial crude palm oils is on average about 3.5%.
achieve this, the oils are submitted to several treatments.
The objective of the refining is to remove the objection- The monoacylglycerol (MAG) content in crude palm oil is
very low (below 0.5%). Jacobsberg and Oh [2] reported a
total diacyglycerol (DAG) concentration in crude palm oils
Correspondence: Véronique Gibon, De Smet Technologies and
ranging from 5.3 to 7.7%. They also noticed no correlation
Services, Da Vincilaan, 2 Bus G1, 1935 Zaventem, Belgium.
Phone: 132 2 716 1111, Fax: 132 2 716 1109, e-mail: giv@ between FFA, MAG and DAG contents: DAG found in
desmetgroup.com crude palm oil is probably a residual by-product of the
© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

316 V. Gibon et al. Eur. J. Lipid Sci. Technol. 109 (2007) 315–335
biosynthesis of the TAG. These observations have been oil demonstrates a low carotene content and suggests
confirmed by Goh and Timms [3] who also reported a high oxidation of the crude oil. A spectrophotometric
significant correlation (based on a statistical study) be- method is available to determine the carotene content of
tween MAG and DAG. More 1,3-DAG than 1,2-DAG iso- palm oil using n-hexane as solvent; the absorbance close
mers (in a proportion of about 2 : 1) are observed in all to 450 nm multiplied by an empirical factor 427 is fre-
crude oils. quently used to express carotene in ppm.
Carotenoids (and in particular b-carotene) are known for

2.2 Phosphatides and glycolipids their pro-vitamin A activity and are strongly associated
with the prevention of certain types of cancer [4]. Most of
According to Goh et al. [4], the main phosphatide com- the carotenoids in palm oil are destroyed during the
ponent in palm oil is phosphatidylcholine and the major refining process, giving rise to light-colored products.
glycolipid is galactosyldiacylglycerol. On the other hand, Various methods of extraction and recovery of car-
Kulkarni et al. [5] have shown that Indian crude palm oil otenoids from crude palm oil are described, including
contains (beside phosphatidycholine) phosphatidyletha- saponification, adsorption, precipitation, solvent extrac-
nolamine, phosphatidylinositol (more than 20% each) tion, molecular distillation and transesterification.
and, in lower quantities, phosphatidylglycerol. A detailed
study of phosphatides in crude palm oil showed that most
of the phosphorus determined in the oil is in fact inorganic 2.5 Sterols, methylsterols, triterpene and
phosphate rather than from phospholipids. Typically, the isoprenoid alcohols and hydrocarbons
inorganic phosphorus content is eight times that of the
phospholipid phosphorus. Detailed studies of these two The total sterol content in crude palm oil is around 500 ppm
forms of phosphorus compounds in crude palm oil indi- [7]. b-Sitosterol is the most abundant sterol (up to 60%).
cate that they are unlikely to be the direct cause of some Campesterol, stigmasterol and cholesterol are observed in
oil quality problems such as poor bleachability or lower quantities. Sterols are observed as free or esterified
increased susceptibility to oxidation. The inorganic phos- (50 : 50) [1]; free and mainly acylated sterol glucosides are
phate presumably arises from the degradation of phos- also detected (up to 300 ppm). Methylsterols and tri-
phatides by phospholipases and further chemical trans- terpene alcohols are present at a concentration of
formation [6]. 800 ppm. Isoprenoid alcohol in crude palm oil is about
80 ppm. Squalene, which is the major hydrocarbon in
crude palm oil, ranges between 200 and 500 ppm; the
2.3 Tocopherols and tocotrienols content in non-terpene hydrocarbon is about 30–50 ppm.
Crude palm oil contains also 10–80 ppm of ubiquinone-10
Characteristic of crude palm oil is its high content in and 5 ppm of ubiquinone-5, which are related to vitamin K
tocotrienols (mainly g-, a- and d-tocotrienols). g-Toco- and have antioxidant properties [1].
pherol and a-tocopherol are the main tocopherols [1], with
the total content (tocopherols and tocotrienols) ranging
from 600 to 1000 ppm [4]; the tocopherol/tocotrienol ratio 3 Crude palm oil quality
is usually around 20%. Compared to other oils, palm oil
has a high proportion of tocopherols and tocotrienols in Important aspects of the quality of the crude feedstock
relation to its unsaturation; the ratio tocopherols 1 toco- have to be considered in that they affect the refining pro-
trienols (ppm) to polyunsaturated fatty acids (PUFA) cess (effect of ripeness, storage, transportation, etc.).The
(expressed in %) is about 50 (while it is only 19 for soy- chemical and physical properties of Malaysian crude
bean and 12 for sunflower oils). Conjugated effects of palm oil have been thoroughly determined from several
high tocopherols and tocotrienols and low PUFA could surveys and the data have been incorporated in stand-
explain why palm oil would present a greater oxidative ards (Tabs. 1 and 2) [8, 9].
stability, for instance, in frying [1].
3.1 FFA content

2.4 Carotenoids
A powerful hydrolytic enzyme is present on the exterior of
As its deep red color testifies, crude palm oil is a rich the palm fruits, and if it is not deactivated promptly after
source of carotenoid components (500–2000 ppm). a- harvesting, any oil escaping from damaged fruits or dur-
Carotene and mainly b-carotene are the main constitu- ing processing splits rapidly into FFA and partial
ents (about 90% of the total) [7]. Light-colored crude palm acylglycerols.

Eur. J. Lipid Sci. Technol. 109 (2007) 315–335 Palm oil refining 317
Tab. 1. Quality requirements for crude palm oil (source: 3.3 Oxidation products and metal traces
MS 814/1994) [8].
Values as low as a peroxide value (PV) of 4 meq O2/kg, an
Characteristics Special Standard Standard anisidine value (AnV) of 4, iron of 3 ppm and copper of
quality quality quality 0.1 ppm are desirable in the crude oil. Whereas in 1970
(SQ) grade I II
crude palm oil at a maximum content of 10 ppm iron and
FFA (as palmitic) [% max] 2.5 3.5 5.0 0.2 ppm copper was commonly offered, good crude palm
Moisture and impurities 0.25 0.25 0.25 oil at a maximum of 3 ppm iron and 0.02 ppm copper is
[% max] available today. Copper is particularly unwanted as
Peroxide value [meq O2/kg max] 2.0 – – quantities below 0.02 ppm are capable of encouraging
Anisidine value (max) 4.0 – – oxidative attack [13]: copper is considered as ten times
DOBI [min] 2.8 2.5 2.2 more active as pro-oxidant than is iron. Contamination
with trace metals mainly arises because of mechanical
wear and corrosion at the oil mill or during storage and
transportation; use of stainless steel can greatly reduce
Tab. 2. Specifications for crude palm oil [9]. this level. Also, oil recovered from effluent treatment is
particularly rich in iron [9].
Special Lotox Standard Contractual
grade As specified before, crude palm oils of several grades are
FFA (as palmitic) [% max] 2.5 2.5 3.5 5.0 commercially available, with the FFA content varying be-
Moisture [% max] 0.2 0.2 0.2 Basis pure tween 2.8 and 5%. High FFA levels generally result in high
Impurities [% max] 0.02 0.02 0.02 Basis pure iron and copper levels, picked up during transportation
Peroxide value 3 3 5 – and storage, resulting in an acceleration of oxidation and
[meq O2/kg max] an increase in Totox (two times PV 1 AnV) which cannot
Anisidine value (max) 4 3.5 – – be sufficiently reduced during refining.
Carotene [ppm max] – 600–700 – –
Fe [ppm max] 4 4 5 – Refiners using good-quality palm oil can easily fulfill the
Cu [ppm max] 0.02 0.2 0.2 – requirements of a good-quality refined oil based on FFA,
iron, copper and color. But the Totox value seems to be
critical: because transport conditions are governed more
by commercial requirements than by quality require-
Freshly expelled crude palm oil, promptly dried and ments, this value can increase greatly during transporta-
cooled, will show low hydrolysis and oxidation. Crude tion, obliging the European refiners to re-treat the already
palm oil can be produced at less than 2.5% FFA and processed oil.
0.15% H20; at this moisture level, both hydrolysis and
oxidation are slowed [10, 11]. An FFA content below
3% gives some guarantee that fresh and unbruised 3.4 Oxidized carotenoids
fruits were used and that the crude oil was stored and
transported under good conditions. Too high levels Good-quality crude palm oils of different origins show
(together with high iron and copper picked up during absorption peaks in the region of 458 nm (UV spectros-
storage and transportation) will lead to too high oxida- copy) due to carotenoids. Modest deviations from a pre-
tion [12]. cise absorption pattern are explicable by some variation
in the carotenoids present in different species. If the crude
oil has suffered from damage, the height of the absorption
peak is diminished and a displacement towards 450 nm is
3.2 Phosphatide content observed [13]. Low-grade crude palm oils may suffer
autoxidation of the carotenoids, giving rise to off-flavors.
The phosphorus content of crude palm oil is quite vari- It is also shown that carotene has a pro-oxidant behavior
able, both in amount and in quality. Normally in the range that can overcome the positive effect of up to 0.1% of
of 10–20 ppm, values less than 5 ppm have been reported tocopherols and tocotrienols as scavengers of oxygen-
as well as values exceeding 30 ppm. As already men- free radicals [14].
tioned, only 10–30% of this phosphorus occurs as phos-
phatides; the major content being described as inorganic. Nitrogen blanketing of storage tanks during transporta-
The exact nature of this phosphorus component is still tion retards oxidation. Antioxidants can be added to the
unknown [4, 6]. crude oil (combination of TBHQ and citric acid), assuring

a better color of the oil after refining and allowing the the use of chemicals (like phosphoric acid, sulfuric acid
reduction of bleaching earth consumption because the and caustic soda), reduction of water and effluent, and
amount of oxidized crude oil has been substantially hence considerable reduction of the environmental
reduced [11]. impact [17, 18]. Unfortunately, bleaching earth consump-
tion will be higher.
3.5 Deterioration of bleachability index The final choice between chemical and physical refining
will depend on a number of factors: the quality and the
The deterioration of bleachability index (DOBI) is a good acidity of the crude oil, the ability to get rid of the soap-
test to assess the quality of a crude palm oil [15]. The stock, and local environment legislation. Although physi-
DOBI is basically the ratio between the content of car- cal refining can be applied to almost any quality of crude
otenes (measured at 446 nm) and secondary oxidation oil, the process more depends on the crude oil quality
products (measured at 269 nm). Practically, the crude oil than chemical refining. This can be explained by the fact
is dissolved in iso-octane or n-hexane and the absorb- that a wide range of undesirable products is much more
ance at 269 nm and 446 nm is measured. It must be said easily removed by alkali neutralization than by degum-
that the DOBI is now recognized as an ISO method [ISO ming.
7932:2005].
For crude palm oil with low phosphatides, high initial FFA
Absorbance at 446 nm
DOBI ¼ (up to 5%) and high carotene content, physical refining is
Absorbance at 269 nm
preferred in terms of operating costs and refining losses;
An arbitrary scale has been suggested [13]:
deodorization at reduced temperature and improved
DOBI 3.25 (very satisfactory quality); DOBI =62.75 vacuum are an alternative when retention of minor com-
(average quality); DOBI ,2.0 (very poor oil). ponents like tocopherols and tocotrienols is important.
However, other sources [16] propose less severe classifi- Chemical refining is still used at a limited capacity [neu-
cations: tralized, bleached and deodorized (NBD) palm oil]. Crude
palm oil is mixed with citric or phosphoric acid for easy
DOBI .2.3 (more easily refined); DOBI = 2.0–2.3 (unpre- removal of gums prior to neutralization of the FFA. Neu-
dictable); DOBI ,2.0 (difficult to refine). tralized oil is separated from the soapstock by cen-
trifugation; the neutralized oil is then washed with warm
water to reduce the residual soaps and dried under
4 Refining practices for crude palm oil vacuum, before proceeding to bleaching and deodoriza-
tion.
Crude oils are refined to remove all impurities such as
undesirable odor, flavor and color, but at the same time
retaining the beneficial components such as vitamins,
5 Physical refining practices
pro-vitamins and antioxidants. Refining can be operated
according to two main routes: chemical refining or physi- 5.1 Degumming
cal refining. The principal difference between the two
routes is how the FFA are removed. In a physical opera- Water degumming is the simplest method for phospha-
tion, most FFA are removed in the deodorizing unit; oper- tide reduction. However, mainly the hydratable phospha-
ating conditions (temperature, vacuum and steam) are tides [phosphatidyl choline (PC) and phosphatidyl inositol
carefully selected in order to allow removal of the acids; a (PI)] can be removed by mixing the oil just with water.
well-designed deodorizer operating at an acceptable
Oils with a low content in phosphatides can be degum-
efficiency will reduce the costs of the process. As distilla-
med straight according to a wet acid degumming tech-
tion requires a high-temperature treatment, the oil must
nique. The hot crude oil (80–90 7C) is thoroughly mixed
be carefully degummed and bleached before entering the
with phosphoric or citric acid, followed by a retention time
deodorizing unit. At the opposite, if the chemical refining
of approximately 5–20 min; then 2–5% water is mixed
option is chosen, the oil is cleared from gums and FFA
with the oil before going to a centrifugal separation. In
during the alkali neutralization step and soapstocks are
fact, one common property of phospholipids is that they
produced. More than 95% of crude palm oil in Malaysia is
form hydrates in contact with water, and these hydrates
refined through the physical route [refined, bleached and
are insoluble in oil. The rate of hydration of phospholipids
deodorized (RBD) palm oil].
varies substantially at 80 7C. PC and PI hydrate very fast
The physical refining process can offer important advan- while phosphatidic acid (PA) and phosphatidyl ethanola-
tages to the refiner, such as higher oil yield, reduction of mine (PE) (mainly present as calcium and/or magnesium

salts) react considerably more slowly with water. The PC ate is added to neutralize any remaining phosphoric acid
hydrate is not only rapidly formed but it can also encap- before filtering, but this is not good since non-hydratable
sulate PA 1 PE 1 PI at about 80% of its own weight [19]. calcium phosphatides are formed, leading to less satis-
This means that when the phospholipids in the crude oil factory phosphorus removal [22]; when strong phosphor-
contain about 55% PC, they all can be removed by fast ic acid is used (85%), iron removal seems to be more dif-
hydration at elevated temperature. If the phospholipids ficult [23]. These problems can be avoided by using citric
contain only about 30–35% PC, fast hydration will give acid (0.05 wt-% dose of citric acid as a 30 or 50% solu-
only partial removal of the slowly hydrating phospholip- tion in water), a mixture of phosphoric and citric acids
ids. An acceleration of the rates of hydration of the cal- (2 : 1), or a diluted phosphoric acid solution (.50%).
cium and magnesium salts of PA and PE can be obtained
Adsorptive cleansing should reduce the phosphorus level
by addition of a strong acid prior to hydration. This
to an acceptable limit (below 2 ppm), lower the trace
explains the varied performance of wet acid degumming
metal content (Fe ,0.1 ppm) and minimize oxidation
according to the composition of the gums. Wet acid
products. The color of palm oil after earth bleaching alone
degumming is mainly used for crude palm oils with high
seems to be not important as carotenoids are known to
phosphatide and iron contents.
be efficiently thermally bleached under the conditions of
Soft degumming [20] is another option to remove phos- deodorization. After 20 min at 180 7C, half the carotene
phatides from crude palm oil with high phosphatide and has disappeared, at 200 7C about 70%, and at 240 7C
iron contents. In this case, the oil is heated (75–85 7C) and more than 98% [24, 25].
mixed with a water solution (2%) containing a complexing
At a certain moment, the question was raised as to
molecule [ethylene diamine tetracetic acid (EDTA)] and,
whether the thermal bleaching and deodorization of palm
eventually, a wetting compound [sodium dodecyl sulfate
oil at temperatures around 270 7C for a few minutes or at
(SDS)]. EDTA is able to form strong chelates with magne-
220–240 7C for longer times give rise to polycyclic aro-
sium, calcium and iron. As a consequence, non hydrat-
matic hydrocarbons from the carotenoid pigments; it is
able phospholipids will be more easily removed. After
now clear that this effect should be negligible [4, 26].
20 min of retention time followed by centrifugation, less
than 1 ppm of phosphorus can be achieved. Iron is
reduced to below 0.1 ppm as it forms an oil-insoluble 5.2 Bleaching
complex with EDTA.
Adsorptive bleaching is an integral part of the process of
For palm oil, dry degumming is the most common way.
refining edible oils and can only exceptionally be omitted
Classically, crude palm oil is first mixed with about 0.05–
if the oil to be refined is very low in components requiring
0.1% concentrated phosphoric acid; after a short reten-
removal.
tion time, about 1 or 2% acid-activated bleaching earth is
added under vacuum at a temperature of 80–120 7C. After
a suitable contact time, the spent earth is removed by fil- 5.2.1 Principle
tration. The phosphoric acid disrupts non-hydratable
phosphatides by decomposing magnesium and calcium The removal of minor components through adsorptive
complexes; it coagulates the phosphatides, sequestrates bleaching is based on several adsorption mechanisms.
iron and copper, before being removed by adsorption on Part of the coloring pigments (carotenoids in the case of
bleaching earth. Sometimes citric acid is also used, but palm oil) are physically adsorbed on the bleaching clays,
due to economical reasons, phosphoric acid is mainly involving “Van der Waals” surface attraction forces. Other
used by Malaysian refiners. The amount of acid intro- components are chemically bound to the bleaching clay
duced into the oil is quite critical: under- or over-dosage surface via covalent or ionic bonds. Part of the impurities
may lead to darkening of the oil during deodorization. is removed through molecular entrapment in the porous
Phosphatides (due to low acid dosage) break down at the structure of the clays. During bleaching, some minor
deodorization temperature, leading to darkening and off- components are chemically altered due to the catalytic
flavor problems [13]. An excess of phosphoric acid (over- activity of the clays: a typical example is the decomposi-
dosage) also promotes darkening of the RBD palm oil tion of the hydroperoxides into unsaturated conjugated
[21]. products.
When using concentrated phosphoric acid with 85% The most important factors affecting absorptive bleach-
strength (commonly 0.05–0.1%), there is a danger to ing are temperature and humidity, but the structure (par-
promote phosphorylation of some triacylglycerols (lipo- ticle size distribution) and the type of bleaching earth
philic phosphorus) [13, 16]. Sometimes, calcium carbon- [heat- (neutral) or acid-activated] also play a crucial role.

Neutral bleaching clays are aluminum silicates which 5.2.3 Single-step bleaching
contain relatively high amounts of calcium, magnesium or
iron. These clays are normally activated through heat The oldest method of bleaching, which is still followed in
treatment; the high metal content limits the adsorptive various bleaching plants, is the batch bleaching where all
activity of these clays. The metals can be removed from operations are executed in the same vessel (except for
the reactive spots by means of an acid treatment, result- the filtration).
ing in acid-activated clays with a much higher adsorptive
capacity. It is generally assumed that the spent filter cake Continuous vacuum bleaching protects the oil from oxi-
contains about 20–30 wt-% oil, but is has been proved dation since deaeration is more efficient. The total holding
[27] that the amount of neutral oil losses when disposing time of the oil is much shorter, which minimizes the risk of
of the cakes is considerably higher than generally recog- unwanted side reactions such as conversion of soaps into
nized (above 45%). FFA in the case of acid bleaching earth. Another benefit of
continuous bleaching is the energy savings that can be
obtained by heat recovery. In the case of dry degumming
5.2.2 Bleaching process of crude palm oil, there is no separate degumming step;
the acid-activated phosphatides are adsorbed on the
The bleaching process is by far the most expensive pro- bleaching clay and as such removed from the oil (Fig. 1).
cess in refining when considering the utility costs. The
relatively high cost of the bleaching clays as well as the
oil-in-earth losses and bleaching adsorbent disposal
5.2.4 Multi-step bleaching
costs largely affect the operating cost of a bleaching
plant. In order to reduce bleaching earth consumption, alter-
native multi-step bleaching processes have been devel-
The strong environmental regulations are also forcing all
oped.
refiners to reduce as much as possible the solid waste
streams as they are difficult to treat. Several bleaching
The most known are the two-stage co-current and coun-
processes have been developed over the years to reduce
ter-current bleaching processes.
the bleaching earth consumption.
Bleaching is performed in several stages: The co-current process is the least complicated and less
performing two-stage process: bleaching earth is added
Prior to bleaching, the oil is properly deaerated and dried in two consecutive stages to the oil, with a filtration after
under reduced pressure (,100 mbar) to a moisture con- every stage. The counter-current bleaching process is the
tent of 0.1%. Deaerated bleaching earth is added to the most efficient (Fig. 2). In this process, the spent bleached
oil under controlled conditions of temperature, acidity and earth from the second bleaching stage is re-used in the
humidity for a specific residence time (20–30 min). The first stage. The efficiency of the counter-current process
bleaching clay is dosed directly to the oil or in a slurry is largely affected by the way the filtration with spent
form (pre-mix of oil with bleaching earth). It is of great bleaching clay is performed. The easiest way is to use a
importance that both oil and bleaching earth are free from third filter operating in counter-current at the inlet of the
oxygen before mixing, to avoid oxidation and hence bleacher. The pre-filtration of the oil through the spent
deterioration of the oil. The oil is further heated under bleaching clay cakes in the filter, built up during the sec-
reduced pressure and intensively mixed, sometimes by ond bleaching stage, already results in a saving of 10–
injection of steam to ensure intimate contact between the 15% bleaching earth as compared to conventional single-
bleaching earth and the oil. Finally, the mixture is trans- stage bleaching. The main function of pre-filtration is to
ferred to a filter, usually a hermetic leaf filter (horizontal or remove all solid impurities as well as to absorb most of
vertical) with stainless-steel mesh elements, followed by the phosphatides and soaps. This allows a more efficient
polishing filtration. The first oil that passes through the bleaching in the second stage. Even more efficient than
leaf filter is normally recycled back to the bleacher vessel the counter-current pre-filtration process is the Oehmi
as it may still contain too much bleaching earth. The process [28] which guarantees savings up to 40%. This
bleached oil is afterwards diverted to the bleached oil process features two bleachers and two sets of filters
storage tanks and kept under nitrogen. Bleaching filtra- (Fig. 3). The spent bleaching clay of the second filtration is
tion is sometimes improved with a pre-coat of diatomac- mixed back into the degummed oil in a specific manner
eous earth. The spent bleaching earth cake is blown by and subsequently filtered. It is interesting to note that over
steam or nitrogen to recover as much as possible the 60% of the undesirable substances are removed in the
entrained oil from the cake. first process stage.

Fig. 1. Classical single-stage bleaching (continuous vacuum bleaching with acid pre-treatment) [17].
Fig. 2. Two-stage counter-current bleaching with pre-filtration.
For palm oil, bleaching earth consumption has been Recently, a multi-stage modular bleaching system
quantified with conventional single-stage and counter- (Combiclean) has been developed [29]. Basically, it
current processes [17]. A bleaching earth consumption of combines silica pre-treatment, pre-filtration with spent
1% can be reduced to 0.8% with a conventional pre-fil- bleaching clays, bleaching, and eventually activated-car-
tration, and up to 0.6% with the full counter-current sys- bon post-treatment (Fig. 4). Savings of up to 30% are
tem. reported. Pre-treatment with silica is particularly interest-

ing earth and potentially toxic spent activated carbon.

Such separation may be important for further utilization or
disposal. On top of that, active-carbon consumption is
reduced by 50%.
5.2.5 Packed (fixed)-bed bleaching
Packed- (or fixed-) bed bleaching is used in some re-

fineries; it refers to pre-loading all or some of the bleach-
ing earth on a filter and pressing the oil through the
packed-bed instead of continuously mixing all the earth
with oil [13]. This ensures the optimum use of the bleach-
ing earth by pre-coating it onto a filter in the form of a
short, wide chromatography column [27]. Silica adsor-
bents are mainly used in combination with bleaching
earth to prevent blocking of the oil flow due to soaps and
Fig. 3. Two-stage counter-current bleaching according to phosphatides; in this case, the filter cake consists of two
the Oehmi principle. (1) Bleacher 1 (pre-bleaching), layers: a first layer with silica and a second layer with
(2) pump, (3) pump, (4) bleacher 2 (final bleaching), bleaching earths. Residual bleaching capacity is con-
(5) mixer, (6) bleaching earth doser, and (7) filter [32]. tinuously monitored by on-line measurement of a specific
component; when this capacity has been reached, the
filter is cleaned in the normal way and re-coated.
ing to selectively remove phosphatides and soaps if cer-
tain unwanted minor components have to be considered.
In some cases, active carbon is applied to take out non- 5.2.6 Wet and dry bleaching
volatile contaminants such as high-molecular-weight
polycyclic aromatic hydrocarbons or dioxins. Active car- Continuous bleaching units are often operating by means
bon is added together with bleaching earths or mixed with of the wet bleaching concept. With wet bleaching, the
the bleached oil after bleaching. Full separation of removal is more effective and the consumption of
bleaching clays and active carbon is preferred as it results bleaching earths can be reduced. It is known that during
in two separated waste streams: non-toxic spent bleach- bleaching, soaps are converted into FFA due to the acidic
Fig. 4. Multi-stage modular bleaching (Combiclean) [29].

properties of the bleaching earth. Another side reaction Tab. 3. Influence of temperature and acid (concentration
that can occur during bleaching, in case the oils are not and type) on residual phosphorus content (ppm) of
sufficiently dried or the earths are still too wet, is the bleached palm oil$ [32].
hydrolysis of TAG that will increase the DAG and FFA
Temperature 0.15% Phosphoric 0.15% Phosphoric 1.5% Citric
contents [30]. The second side reaction can be avoided
[7C] acid (85% acid (10% acid (10%
by simply drying the oil before bleaching and assuring solution) solution) solution)
that the bleaching earths are not too wet. Nevertheless, it
can be desirable that the oil contains sufficient amount of 90 9.8 3.3 1.7
water when bleaching earth is added. During the so- 120 21.1 3.6 1.3
called wet bleaching [31], non-hydratable phosphatides 150 38.8 3.7 3.4
are hydrated in the presence of chelating acids and water;
$
the presence of water will increase the cation exchange Crude palm oil: P: 9.9 ppm; FFA: 5.6% (as palmitic).
capacity of the bleaching earth. The best performance is Bleaching earth: 1.5% Tonsil Supreme FF.
Calcium carbonate used after phosphoric acid treatment.
observed for an amount of water of about 50–100% of the
amount of bleaching earth, which is not always econom-
ically acceptable. In wet bleaching, the materials are
allowed to come into contact with each other under at- Tab. 4. Influence of added water and temperature on
mospheric pressure for 20 min at about 70–90 7C. This is residual phosphorus content (ppm) of bleached palm oil$
[32].
followed by the usual bleaching process under vacuum
for 15–30 min. During this step, the excess water evapo- Temperature 0% 0.5% 1.0% 1.5%
rates so that the bleaching earth can be filtered without [7C] Water Water Water Water
problems.
120 8.5 5.3 3.2 2.7
Certain silica gels with a water content of 60–70% can 135 6.8 4.5 3.0 2.9
also be used instead of wet bleaching to remove phos- 150 6.6 4.0 2.5 3.2
phatides. Compared to the normal bleaching earths,
$
these materials have a much higher adsorption capacity Crude palm oil: P: 17.1 ppm.
for phosphatides, soaps and metal traces and can par- Bleaching earth: Tonsil Supreme FF.
tially replace the bleaching earths. However, pigments
(chlorophyll, carotenoids) are weakly adsorbed by these
silical gels [32].
5.2.8 Adsorption of pigments
In the physical refining of crude palm oil, full reduction of

5.2.7 Residual phosphorus content after carotene by bleaching is not necessary as carotenoids
bleaching are mainly decomposed by heat during deacidification
(heat bleaching; see Section 5.1).
After bleaching, the oil should be almost free from phos-
phorus, iron and copper.
When palm oil is to be used for biodiesel production, the
According to Zschau [32], the efficiency of phosphorus color is of minor importance; removal of phosphatides is
removal in dry degumming of palm oil depends on the then the most critical aspect of the pre-treatment; in this
conditions chosen; temperatures below 120 7C and acti- case, the addition of bleaching earth might not be neces-
vation of phosphatides with diluted phosphoric acid or sary and simple acid washing or soft degumming is a
with citric acid are preferred (Tab. 3). If instead of phos- suitable alternative option (Tab. 6) [33].
phoric or citric acid, pure water (up to 1.5%) is added at
the same time as the clays at atmospheric pressure (wet Rossi et al. [34] have studied the effect of bleaching on the
bleaching), phosphorus removal is very efficient; the data color of degummed palm oil. Five concentrations of one
correlate with the quantity of water (Tab. 4) [32]. Indeed, neutral and two acid-activated bleaching clays mixed
the clays have also acidic properties and ion exchange with a fixed amount of synthetic silica were used for
capacity and could take the role of phosphoric and citric bleaching (110 7C, 20 min under vacuum) after acid
acids. When quite concentrated phosphoric acid is used degumming. Neutral bleaching clays seem to be less
(.75%), there is a critical relationship between the acid efficient than acid-activated clays to remove carotenoids
and bleaching earth dosages and the residual phos- (Tab. 7). For the activated clays, pigment removal clearly
phorus content (Tab. 5) [33]. increases with the amount.

Tab. 5. Influence of acid dosage on dry degumming effi- Tab. 7. Influence of degumming and bleaching earth
ciency of crude palm oil [33]. quality and quantity on carotenoid retention (ppm) in palm
oil (bleaching conditions: 110 7C, 50 mbar, 20 min;
0.07% Phosphoric acid (75%); 1% Tyco Classic bleaching earth 0.125% synthetic silica added to the bleaching clays)
[34].
Crude palm oil Degummed palm oil
FFA (as palmitic) [%] 5.68 – Treatment Carotenoids
P [ppm] 17.5 4.6 [ppm]
Fe [ppm] 7.5 0.1
Crude palm oil 455.8
Ca [ppm] 18.2 0.2
Acid-degummed palm oil 415.0
Mg [ppm] 4.9 0.1
Bleached with acid-activated clay 1:
0.055% Phosphoric acid (75%); 1% Tyco Classic bleaching earth 0.5% bleaching clay 1 297.0
Crude palm oil Degummed palm oil 0.75% bleaching clay 1 245.8
1.0% bleaching clay 1 223.4
FFA (as palmitic) [%] 3.94 –
P [ppm] 13.6 1.7 Bleached with acid-activated clay 2:
Fe [ppm] 3.2 0.04 0.5% bleaching clay 2 327.9
Ca [ppm] 12.7 0.2 0.75% bleaching clay 2 313.9
Mg [ppm] 3.7 0.02 1.0% bleaching clay 2 258.6
0.045% Phosphoric acid (75%); 1% Tyco Classic bleaching earth Bleached with neutral clay:
0.5% neutral clay 324.4
Crude palm oil Degummed palm oil 0.75% neutral clay 329.9
FFA (as palmitic) [%] 5.04 – 1.0% neutral clay 304.0
P [ppm] 16.0 1.4
Fe [ppm] 5.3 0.2
Ca [ppm] 19.2 0.3 oxides; while PV decrease rapidly during bleaching, AnV
Mg [ppm] 3.6 0.05 only decline. This leads to the reasonable deduction that
0.03% Phosphoric acid (75%); 1% Tyco Classic bleaching earth the catalytic decomposition of peroxides is preferred over
the adsorption of aldehydes and ketones on the active
Crude palm oil Degummed palm oil
site of the clays [13]. It is described that oils refined using
FFA (as palmitic) [%] 4.38 – acid-activated earth during bleaching have a better final
P [ppm] 17.1 not detected acidity and oxidative stability than oils refined using non-
Fe [ppm] 6.2 0.1 acid-activated earth [35]. It has also been reported that
Ca [ppm] 14.0 0.2 refined oil bleached with low-quality clay exhibits less
Mg [ppm] 4.5 0.1
stability in color, FFA and peroxides [30].
Tab. 6. Influence of several pre-treatments on residual Conjugated dienes and trienes are formed during bleach-
phosphorus content of crude palm oil [33]. ing of palm oil as a result of the decomposition of hydro-
peroxides [36]. For a given oil, the amount of conjugated
Pre-treatment Residual P Residual Fe dienes, measurable at 233 nm, is related to the bleaching
Water washing$ 13 10 earth dosage; bleaching earth below 1% seems to allow
Acid water washing$ 6 4 less formation of conjugated dienes. An increase of con-
Soft degumming§ 2.5 0.5 jugated trienes during bleaching depends on the crude
Acid conditioning followed by 7.5 1 palm oil quality, independently of the bleaching earth
partial caustic treatment and used. Some of these conjugated trienes can be removed
water washing$ later during deodorization. Low conjugated dienes and
$
trienes in the refined oil are an indicator of mild refining
Crude palm oil: FFA: 4.8%; P: 16.0 ppm; Fe: 13.0 ppm.
§ conditions and good-quality crude oil.
Crude palm oil: FFA: 4.8%; P: 13.7 ppm; Fe: 3.8 ppm.
5.2.9 Catalytic properties of bleaching earths 5.2.10 Irradiation bleaching
Some reactions observed during bleaching can be clearly Recently, irradiation bleaching has been described [37]
attributed to the catalytic properties of the clays. The on red palm oil, palm olein and palm stearin. The bleach-
most important one is the decomposition of hydroper ing level achieved by irradiation is comparable to the

bleaching achieved by heating. The general quality of the When the initial FFA content is low, as in the case of a
resulting oils is better if they are bleached with irradiation, classical deodorization, (Va – V0) becomes so small that
as the amount of the polar fraction resulting from irradia- Eq. (1) can be simplified to:
tion is minimal relative to that found in heat-treated oil.
The conclusion is that infrared bleaching is economically S Pt Va
¼ : ln (2)
more viable than solar irradiation techniques and heat O E:P0i V0
bleaching, as it can be performed easily with no oil losses
In the case of physical refining, the partial pressure of the
and less energy consumption.
fatty acids cannot be neglected, and omitting the term
(Va – V0) would lead to a considerable underestimation of
the stripping medium requirements.
5.3 Deodorization
This simplified Eq. (2) is also known as the “Bailey Equa-
tion”. It states that the amount of steam required for deo-
5.3.1 Process parameters and conditions
dorization or physical deacidification is directly propor-
Deodorization is basically a vacuum steam stripping at tional to the amount of oil and the absolute pressure in the
elevated temperature, during which FFA and volatile odi- deodorizer and inversely proportional to the vapor pres-
ferous components are removed to obtain a bland and sure of the pure volatile component at the process tem-
odorless oil. Although the process is commonly named perature and the overall vaporization efficiency E.
‘deodorization’, it is actually a combination of three dif- The last factor in Eq. (2) (ln Va/V0) indicates that it is
ferent operations: (a) distillation, i.e. stripping of volatile impossible to eliminate all volatile components from the
components (FFA, tocopherols, tocotrienols, sterols and oil, since this would require an infinite amount of stripping
contaminants like pesticides or light polycyclic aromatic medium.
hydrocarbons, etc.); (b) actual deodorization, i.e. removal
of odoriferous components; and (c) heating effect, i.e.
thermal destruction of pigments (carotenoids) while 5.3.3 Deodorizer systems
maintaining low side reactions such as “cis-trans” iso-
merization, polymerization, etc. Deodorization can be conducted in different ways (batch,
semi-continuous and continuous) [38]. The selection of
Optimal deodorizing parameters (temperature, operating the most appropriate deodorizer technology depends on
pressure and amount of stripping gas) are determined by many factors, such as the oil quality requirements, the
the type of oil and the selected refining process (chemical number of feedstock changes, heat recovery, investment
or physical refining), but also by the deodorizer design. and operating costs.
Physical refining requires more severe conditions than Batch deodorization is especially suitable for small ca-
chemical refining. This is mainly because of the distillative pacities, irregular production, or in processing small
removal of the FFA, which is more critical in physical batches of different oils. Semi-continuous deodorizers
refining as the initial FFA levels are considerably higher. are basically batch operating systems designed for larger
capacities. In most designs, a batch of oil is transferred
into the system and then sent by gravity in a time
5.3.2 Theory sequence through a number of vertically stacked com-
partments or trays.
The stripping medium requirements are described by the
following mathematical equation derived from “Dalton’s” Continuous deodorizers are most preferred by high-ca-
and “Raoult’s” laws. pacity plants with few stock changes. The main advan-
tages are the moderate investment costs, the possible
! high heat recovery and the easy maintenance. Vertical
S Pt Va Pt
¼ :ln þ 1 :ðV a V o Þ (1) tray-type deodorizers are probably the most used type of
O E:P0i V0 E:P0i
continuous deodorizers (Fig. 5). Their design is based on
a series of trays or compartments stacked vertically in a
whereby S = total moles of steam; O = total moles of oil; Pt
cylindrical shell, with each tray designed for a specific
= total pressure; Pio = vapor pressure of a given fatty
task.
acid i; E = vaporization efficiency; Va = initial molar con-
centration of the volatile component in the oil; and V0 = All operations, heating, deodorization and heat recovery,
final molar concentration of the volatile component in the are combined in a single vessel. All different deodorizer
oil. designs attempt to provide the best contact between the

Fig. 5. Continuous vertical deodorizer (De Smet) [38].
gas phase and the oil phase by creating large contact Packed columns (Fig. 6) are more and more used in edible
surfaces and/or thin oil films together with an optimal oil deodorization. A packed column is basically a single-
sparge steam distribution (for an optimum level of vapor- shell vertical vessel in which a structured packing is
ization efficiency). The sparge steam is introduced into installed. In fact, in the past, a structured packing was
the oil through special distributors, which can be sparge often installed to increase the capacity of existing deo-
coils with very fine holes (between 0.5 and 2.5 mm) (shal- dorizers. Its main function was to reduce the sparge
low-bed deodorizer) or even sintered metal pipes (deep- steam consumption of the deodorizing unit by pre-strip-
bed deodorizers). Steam lift pumps have been introduced ping the main part of the volatile material. The deacidified
in order to improve agitation and overall deodorization oil is then sent to the deodorizer for the final deodoriza-
efficiency by continuously refreshing the oil in the top tion. In palm oil deodorization, for example, the FFA level
layer [38]. The vapors from the different compartments is first reduced from 3–5% to below 0.5% in a structured
are collected in a central chimney and sent to a separate packing before the oil enters the deodorizer. In this way,
vapor scrubber with a sprayer system. In some cases, an the capacity of a deodorizing plant can be significantly
extra structured packing is installed in the scrubber to increased. The main advantages of the structured packed
improve condensation and to reduce fatty matter carry- column are the higher efficiency to remove FFA and the
over to the barometric water condenser system. short residence time (only a few minutes).
Due to the new market demands for minimizing “trans” Recently, a fully modular single-vessel (continuous)
fatty acid and tocopherol and tocotrienol retention, a stand-alone deodorizer was designed (Qualistock) (Fig. 7)
dual-temperature concept has been recently developed. which requires no building and minimal piping. In this way,
In the first tray, the incoming oil is heated to moderate the erection costs can be significantly reduced. This con-
temperature, after which it passes through the first deo- cept allows the integration of different processing options
dorization trays. In these trays, deacidification and deo- with specific functions to improve the overall quality of the
dorization take place under mild conditions (moderate deodorized oil: dual-temperature treatment, deep- or
temperature/moderate stripping). After the first trays, the shallow-bed deodorization, packed column pre-strip-
oil passes a second heating tray in which the oil is heated ping, dual condensation, etc.
to a final and higher temperature. In the last tray, final
stripping and heat bleaching occur. The process param-
eters can be adjusted to arrive at the desired tocopherol 5.3.4 Dry (or ice) condensing systems
and tocotrienol level in the refined oil. In general, the dual-
temperature deodorizer shows a number of benefits that Normal deodorizers operate at 3–4 mbar. Today, special
are important for oil refiners. The benefits include low vacuum production units have been developed to reach
“trans” fatty acid formation because the time at high lower pressures (,2 mbar) and better operating costs
temperature is restricted, maximum heat bleaching and, at the same time, to reduce emissions and effluents
effect, and adjustable tocopherol and tocotrienol by a more efficient condensation of the volatiles. The dry
removal, mainly by steam injection at high temperature. condensing system [38] is becoming more and more the

Fig. 6. Packed column stripper (Alfa-

Laval) [38].
Fig. 7. Modular single-vessel stand-alone deodorizer (Qualistock-De Smet) [38].
standard in new refining plants. In this system, the vapor condensing system significantly reduces the motive
is condensed on surface condensers working alternately steam consumption, but requires extra electrical energy.
at very low temperature (around –30 7C). The remaining
non-condensables are removed either by mechanical The commercially available dry condensing systems
pumps or roots blowers in series with a liquid ring pump consist of two or more condensers, with either horizon-
or by a vacuum steam ejector system (booster). The dry tally or vertically orientated straight tubes, a refrigeration

plant for the generation of cold refrigerant (usually NH3) Removing FFA and partial acylglycerols (mainly MAG) will
which is evaporated in the tubes, and a vessel with rela- also change the physical properties of palm oil; mainly the
tively warm water for defrosting and cleaning of the tubes solid fat content at low temperature will be affected
after a certain period of freezing. A new dry condensing (increased in the refined palm oil).
system has recently been developed [38]; the most
essential feature of this system (Sublimax) (Fig. 8) is the
vertical orientation of the freeze condensers, combined
6 Chemical refining practices
with individual refrigerant injection in the tubes and
sparge steam inlet at the top. In the case of chemical refining, the non-hydratable
phosphatides which remain in the oil after acid treatment
are further removed during the neutralization stage. It is
5.3.5 Side effects of deodorization assumed that caustic soda converts the non-hydratable
phosphatides into sodium salts, which are more easily
Possible changes that may occur on the chemical and removed as they are less oil soluble. On the other side,
physical properties of palm oil and palm fractions under both calcium hydroxide and magnesium hydroxide are
different refining conditions have been described. In the strong bases and therefore do not replace easily the
case of palm olein and palm mid fraction, “trans” fatty equally strong base sodium hydroxide. In this context, it is
acids are mainly formed at 280 7C after a residence time known [39] that the pH must be very high for the residual
of 4 h (2.1 and 1.5%, respectively) [36]. In commercial phosphorus to be ,5 ppm.
refined palm oil products, not more than 0.6% of total
“trans” fatty acids are reported for processing conditions The high soap content in combination with intense water
of 260–275 7C and a residence time of 45–90 min. washing improves the removal of the phosphatides. The
only drawback is the soapstock which needs to be treat-
Intra-molecular rearrangements of fatty acids can be ed accordingly.
observed in oils subjected to drastic refining conditions
(above 270 7C for long residence times); intra-esterifica- The long mix technique (American route) was developed
tion may occur during deodorization of palm oil, resulting based on a long time/low temperature sequence. Histori-
in an increase in saturated fatty acids at the 2-position of cally, it has been especially designed to treat fresh North
the TAG. This intra-esterification has a detrimental effect American soybean oil. On the other hand, the short mix
on the efficiency of dry fractionation of palm oil and on the technique (European route) consists in a short contact
quality of the final fractions. time at higher temperature.
Fig. 8. Schematic diagram of the improved Sublimax Dry Condensing system [38].

6.1 Typical process conditions Tab. 8. Quality and oxidative parameters of palm acid oil
(mean of 27 samples) [40].
The non-hydratable phosphatides are removed by add-
ing 0.03–0.1 wt-% of concentrated phosphoric acid to Parameter Mean Standard
the crude palm oil. The quantity of caustic solution is value deviation
calculated based on the FFA content of the oil; in a Moisture content [%] 0.98 0.53
short mix process, 20–227 Bé caustic soda (10–30% Free fatty acids [%] 62.6 11.5
excess) is generally used and mixed to the oil at 90– Peroxide value [meq O2/kg] 4.1 3.8
95 7C in order to avoid emulsion formation. The contact Iodine value 50.2 5.3
time is generally 30 s to prevent high saponification Saponification value 186 5.6
losses. The soapstock/oil mixture is delivered to Unsaponifiable matter [%] 0.53 0.42
separators. The outgoing light phase is the neutralized
oil containing traces of soaps, free caustic, phospha-
tides and other soluble impurities. The neutral oil losses value, saponification value and unsaponifiable matter
should be usually between 20 and 30%. Soft water at have been quantified. A few samples showed the pres-
about 90 7C is added to the oil for washing and sepa- ence of aldehydes, ketones, furans and volatile acids.
rated in a second centrifuge into water-washed oil as
light phase and soapy water as heavy phase. The range
of the FFA content in neutralized oil is usually between 7 Deodorizer distillate
0.08 and 0.25%, and the soap content is below
50 ppm. After drying, the neutralized oil is sent for 7.1 Composition of deodorizer distillate
bleaching and deodorization (220–240 7C) to remove The composition of the deodorizer distillate is not only oil
mainly odoriferous components and to bring the final dependent, but it is also determined by the refining tech-
acidity into the range of 0.02–0.08%. nique applied (physical or chemical) and the operating
conditions during deodorization [17, 18] (Tab. 9). In the
case of physical refining of palm oil, the distillate mainly
6.2 Soapstock splitting consist of FFA (83–88%) with only small amounts of unsa-
ponifiable components (2–4%) and neutral oil (8–13%).
Soapstock splitting is closely connected with caustic Deodorizer distillate is generally sold as a source of indus-
refining and is completely omitted in physical refining trial fatty acids or eventually for soap production in some
plant facilities. Soapstock from alkali refining is pumped cases after deodorizing to reduce the color. It can also be
to the splitting plant for acid oil production. The total considered as a feedstock for biodiesel production.
fatty matter of diluted soapstock is usually around 10–
15%. Sulfuric acid is mixed and the reaction takes place
in a decantation tank, to break down the emulsion Tab. 9. Typical composition (%) of a deodorizer distillate
from a chemical and a physical refining plant [18].
formed due to the presence of phosphatides, proteins
and other mucilaginous substances. Acid water is Composition Chemical Physical
removed, leaving acid oil to pass through a separator, refining refining
allowing the removal of last traces of water and mucila-
ginous material. Extra washing is performed to assure Neutral oil 25–33 5–10
that no sulfuric acid is left in the acid oil. Soap splitting is Fatty acids 33–50 80–85
Unsaponifiable matter (including 25–33 5–10
generally done at pH ,3. The FFA content of the acid oil
tocopherols and sterols)
produced is usually between 40 and 70%, depending on
the quality of the soapstock used and more especially
the amount of neutral oil in the soapstock. The main
components of palm acid oil are FFA, neutral oil and 7.2 Neutral oil losses during deodorization
moisture. It is mainly used for making laundry soaps and
for producing calcium soaps for animal feed formula- Neutral oil losses during deodorization generally depend
tions. on the oil composition and deodorizing conditions [38]. In
the case of chemical refining, improvement of the deo-
Properties (quality and oxidative parameters) of palm dorizer design has significantly reduced entrainment los-
oil acid oil have been carefully analyzed in order to ses to 0.1–0.2%. For physical refining of palm oil, addi-
build up specifications and a clear definition of palm tional loss directly proportional to the FFA content and
fatty acids (Tab. 8) [40]; moisture, FFA, PV, iodine mainly due to mechanical carryover has to be taken into

account. Higher MAG contents of high acidity oils also Tab. 11. Characteristics of golden palm oil produced by
contribute to losses. In practice, there is also limited physical refining at pilot scale [43].
hydrolysis during deodorization; under normally applied
deodorizing conditions, hydrolysis results in the produc- Crude Degummed RBD
palm bleached golden
tion of 0.015–0.020% additional FFA [41].
oil palm oil palm oil§
FFA (as palmitic) [%] 3.8 0.08

7.3 Dual condensing system or washing section Phosphorus [ppm] 19 ,2
Iron [ppm] 2.1 0.1
The FFA content of palm deodorizer distillate is usually Lovibond 5”1/4 (R/Y) – 50/20 18/20
around 85–90%. With the introduction of a dual Carotenes [ppm] 520 380 105
condensing system [33], in some designs also called Tocopherols/ 856 790 760
washing section [42], the content of acylglycerols (MAG, tocotrienols [ppm]
DAG and TAG), tocopherols, sterols, squalene, etc., in the
§
condensed fatty acids can be reduced. The composition 0.5 mbar, 180 7C, 3% steam, 180 min.
of palm oil distillate without and with this system is pre-
sented in Tab. 10; the total amount of FFA is increased to refined palm oil with improved quality parameters: more
98% min. natural color and higher tocopherol tocotrienol contents:
dual temperature at 200–220 7C combined with low pres-
Tab. 10. Composition (%) of palm fatty acid distillate sure, 1 mbar (Tab. 12), seems to be the best option for a
including or not a washing section [42]. maximal retention of carotenoids, tocopherols and toco-
trienols, for a good oxidative stability and efficient
Components Without washing With washing removal of the FFA.
section section
FFA 87.4 98.1

MAG 2.0 0.7 8.2 Red palm oil with high vitamin content
DAG 0.7 0.05
TAG 8.0 0.1 With the removal of FFA also comes in a considerable
Tocopherols, sterols, 1.9 1.0 extent of removal of impurities. It has been shown that an
squalene efficient alkali refining plant is able to purify crude palm oil
so effectively that it can be deodorized directly (without
bleaching) or in the worst case with very small amounts of
non-activated bleaching earths or silica [13]. Such a pro-
8 Special products cess will require very-good-quality crude palm oil (low
FFA and high DOBI), with the cleansing action of neu-
8.1 Golden palm oil tralization being mainly limited to phosphorus removal
while keeping the carotenoids unaffected.
A golden palm oil rich in carotene, tocopherols and toco-
trienols can be obtained by physical refining. In some applications, the thermal bleaching would only
operate during deodorization conducted around 240 7C
The characteristics of a high-vitaminic physically refined and with a very short residence time, resulting in reduced
palm oil (produced under pilot conditions) have been losses in tocopherols and tocotrienols and very good
described [43]. It has been claimed that this golden oil oxidative stability for the final product (Tab. 13).
should retain 20% of the initial carotene and 89% of the
tocopherol and tocotrienol content (Tab. 11), which looks Thermal bleaching conducted at lower temperature
to be very high compared to physically refined palm oil would result in limited destruction of carotenoids, to-
produced in Malaysia. Long retention time at relatively gether with keeping high amounts of tocopherols and
low temperature combined with high steam consumption tocotrienols in the oil.
are the necessary conditions to decrease the acidity to
sufficiently low levels while preserving carotenoids, toco- Dedicated products issued from special refining proce-
pherols and tocotrienols. dures and labeled as “Red Cooking Oils” are available on
the Asian market: “Carotino Cooking Oil” and “Nutrolein
More recently, it has been proved [33] that dual tempera- Golden Palm Oil” are the main representative products.
ture and low pressure (using an ice condensing vacuum Nutrolein for example (which is produced by Unitata Ber-
system) can be used to produce an industrially physically had in Malaysia) is a superolein issued from dry-fractio-

Tab. 12. Relationship between process conditions (physical refining) and oil characteristics for
golden palm oil production [33].
Reference§ A B C D E
FFA (as palmitic) [%] 0.07 0.20 0.08 0.04 0.07 0.07
Lovibond 5”1/4 (R/Y) 2.5/25 11.6/70 4.8/50 2.9/29 6.2/50 4.1/42
Tocopherols/tocotrienols [ppm] 544 709 629 431 671 699
OSI at 97.8 7C [h] 70.5 61.5 50.6 36.7 63.0 53.4
§
RBD palm oil refined under classical conditions.
A: 200 7C, 1 mbar, 1.5% steam, 60 min.
B: 220 7C, 1 mbar, 1.5% steam, 60 min.
C: 260 7C, 3 mbar, 1.5% steam, 60 min.
D: Dual temperature: 200–220 7C, 1 mbar, 1.5% steam, 60 min.
E: Dual temperature: 220–240 7C, 3 mbar, 1.5% steam, 60 min.
Tab. 13. Characteristics of palm oil chemically refined 8.4 Feedstock for fractionated products
without bleaching earth [9].
For usage of palm oil in dry fractionation, it is clear that its
Crude Degummed Degummed, properties (mainly related to its TAG composition) should
palm and neutralized and not be modified during refining. Crude palm oil has nor-
oil neutralized deodorized
mally a PPO content below 5% which should stay at that
palm oil palm oil
level before fractionation. Production of palm mid frac-
FFA (as palmitic) [%] 2.56 0.06 0.03 tions (CBE) mainly consists in a maximum increase of
M [%] 0.08 0.01 0.01 symmetrical oleo-dipalmitin: POP; enrichment in asym-
I [%] 0.03 0.02 0.003 metrical PPO due to intra-esterification during the deo-
Carotene [ppm] 580 579 1.0 dorization is of detrimental effect for the palm mid fraction
DOBI 3.1 – – quality [36]. The effect of deodorization time and temper-
Phosphorus [ppm] 16 3 0
ature has been extensively studied by Willems and Padley
Tocopherols [ppm] 733 679 566
[12]. The change of the ratio is significant if the oil is sub-
Induction period at 100 7C [h] 49 34 44
jected to temperatures around 270 7C for long residence
times. To avoid these intra-esterification problems, deo-
nated, chemically refined high-quality crude palm oil. Its dorization temperatures and residence times need to be
carotenoid content is announced to be above 800 ppm, limited; for this reason, chemical refining or physical
with a vitamin E concentration superior to 900 ppm. refining at low pressure and shorter residence times are
Same quality oils are available in the Latin American mar- preferred.
ket, like Sioma Oil (produced by Danec S.A. in Ecuador),
which is a more unsaturated variety of palm oil, obtained Also, a tailing effect which depends on the deodorization
from the hybrid palm. conditions can be observed in the solid fat content profile
of oleins [36]. This tailing effect observed in palm olein
subjected to 280 7C for 4 h is significant compared to
8.3 Production of white soaps from palm refining at 250 7C for 2 h; it is once again produced by
intra-esterification of the fatty acids promoted at high
Production of white soaps from palm oil is not evident: temperatures and resulting in early crystallization of palm
the main problem is the too dark color (.5R 5”1/4) which olein during storage.
is usually achieved during the saponification step [44].
Good results (saponification color of 3R 5”1/4 or lighter)

can only be expected when a crude palm oil of high 9 Refined palm oil quality
quality is used for refining and if the refining procedure is
performed under optimized conditions. Recent research 9.1 Effect of crude oil quality on color reversion
has shown [33] that very good saponification colors
(around 2.5R 5”1/4) can only been obtained from a very It is clear that good-quality refined palm oil cannot be
light RBD palm oil (0.6R 5”1/4) that can only be produced produced from low-quality oils. Crude palm oil with a very
from crude palm oil having a DOBI above 3 (Tab. 14). low DOBI can be processed using a higher bleach-

Tab. 14. Production of white soaps with low saponification color through physical refining of palm oil
[33].
Crude palm oil (DOBI: 3.3)

Refining conditions RBD oil color Saponification color
(R 5”1/4 Lovibond) (R 5”1/4 Lovibond)
Bleaching with 1.5% BE and refining at 280 7C 0.9 3.6

Bleaching with 1.5% BE 1 0.4% AC and refining at 280 7C 0.7 2.8
Bleaching with 2.5% BE 1 0.5% AC and refining at 280 7C 0.6 2.5
BE: Tonsil Optimum 210 FF.

AC: activated carbon.
ing earth dosage (up to 5–6%) to produce acceptable FFA tive stability index (OSI) values indicated an optimum
and color in refined products, but such a product has very around 120 7C, in agreement with other work [13, 32]. It
poor quality. As such, it cannot be called a refined product may be argued that by increasing the bleaching earth
that could meet the requirements of the customers. As dosage or by altering other refining parameters, oil of any
seen above, carotenoids in crude palm oil are easily DOBI value could be adequately refined. However,
removed during adsorptive bleaching and/or deodoriza- another study showed [47] that the oxidative stability of
tion. The amount of carotenoids in the crude oil does not low DOBI refined palm oil is always lower, as compared to
determine the residual color of the refined oil, which is refined palm oils with DOBI above 2.3.
probably due to unknown high-molecular-weight com-
pounds [45]. Every step in palm oil refining is important, A bleachability test has been developed [33] at laboratory
and great care is taken in order to produce a stable scale by which the final color of palm oil could be pre-
refined palm oil with minimal chances of color reversion. dicted. Six crude palm oils from different origins with an
Although in most cases the color reversion is rectifiable, it initial FFA content between 1.9 and 7.2% were prepared.
means extra costs. Color reversion during processing is Afterwards, the samples were bleached at 260 7C for
normally associated with poor quality of the crude oil or 50 min at a pressure of 3 mbar, with the addition of only
with improper degumming and bleaching processes. The small amounts of steam (to ensure good mixing and heat
reversion could be due to colored pigments present in the transfer). The low DOBI values combined with elevated
crude oil or as a result of the oxidation of carotenoids levels of fatty acids and peroxides in some samples gave
during deodorization; oils derived from badly damaged an indication that these oils were difficult to bleach (final
palm fruits contain brown pigments from decomposed color 5”1/4 above 3) (Tab. 15). Moreover, a direct rela-
protein and carbohydrates that are resistant to bleaching. tionship between the DOBI and the final color of the heat-
Moreover, oxidized crude oils may contain colored com- bleached palm oil was observed [33]. A heat-bleached
pounds of quinoid nature developed from oxidation of palm oil with color below 2R can be produced when crude
colored materials. It seems that oxidation not only devel- palm oil had a DOBI above 2.5. These observations con-
ops new pigments but also stabilizes the pigments firmed earlier findings [47] that DOBI values are a good
against their removal by adsorption [16]. indicator for palm oil refinability. It was also shown [33]
that the bleaching temperature did not affect the final
It has been shown that bleached oil color cannot be used color after heat-bleaching. These observations confirm
to predict the final deodorized oil color and quality; in that the bleached oil color cannot be used to predict the
order to determine the effect of the bleaching temperature refined oil color.
on the final oil quality, a simple test has been developed
[46]. Palm oil was bleached at 95, 105, 120 and 135 7C
with 2.5% bleaching earth. Bleached oil colors decreased 9.2 Maximum retention of tocopherols and
as the temperature increased, while the heat-bleached tocotrienols
(refined) oil colors did the opposite. It was assumed that
the rise in refined oil red color could be due to color for- The influence of the bleaching conditions on the toco-
mation caused by both oxidized fatty acids and oxidized pherol and tocotrienol retention of physically refined palm
carotenoids: elevated temperatures would increase the oil has been reported (Tab. 16) [34]. The total quantity of
formation of the color bodies. Although the refined oil identified tocopherols/tocotrienols increased during
color rose with increasing bleach temperature, the oxida- bleaching in correlation with the bleaching earth quantity,

Tab. 15. Relationship between initial FFA content and DOBI of crude oils of different qualities (1–6)
and final color of refined oils after a bleachability test at laboratory scale (260 7C, 3 mbar, 50 min) [33].
1 2 3 4 5 6
FFA (as palmitic) [%] 7.21 4.32 3.54 4.91 2.79 1.90
DOBI 1.34 1.76 2.02 2.23 2.67 3.13
Peroxide value [meq O2/kg] 2.33 3.79 3.15 3.54 0.36 1.03
Oil grade bad poor poor poor fair good
Lovibond (5”1/4) 3.1R/33Y 3R/35Y 2.2R/20Y 2R/20Y 1.3R/15Y 1.4R/15Y
Tab. 16. Effect of bleaching and deodorization conditions on residual tocopherol and tocotrienol contents (ppm) of palm oil
(bleaching conditions: 110 7C, 50 mbar, 20 min; deodorization conditions: 250 7C, 3 mbar, 2.5 h) [34].
Crude Bleached RBD

0.5% 0.75% 1.00% from 0.5% from 0.75% from 1.00%
acid-activated acid-activated acid-activated acid-activated acid-activated acid-activated
clay clay clay clay clay clay
a-tocopherol 190 220 233 223 147 125 150

a-tocotrienol 131 155 162 156 140 112 147
g-tocotrienol 339 291 286 250 213 201 251
d-tocotrienol 113 127 135 206 51 69 62
Total 773 794 815 834 551 506 610
which is in accordance with earlier observations [48] pletely inseparable from the quality of the crude oil. The
where regeneration of the free form from dimeric or high acidity of crude palm oil places physical refining as
esterified compounds was assumed. This release does the first option, mainly for economical reasons but also for
not seem to be indiscriminate, as the g-tocotrienol con- environmental issues. The latest developments in the
tent decreases with increasing bleaching earth quantities. refining technology have been driven by the increased
An average tocopherol and tocopherol retention of 80% attention to the nutritional quality. Optimizing the deodor-
was obtained after steam refining, which is quite high. The ization technology and the process conditions for max-
relative concentration of single tocopherols/tocotrienols imum retention of the natural characteristics will be an
was modified by steam refining, probably due to differ- important challenge for the future.
ences in volatility among various forms and to different
stabilities under the refining conditions [47]. The development of vacuum systems (ice condensing)
capable to reach low operating pressure (around 1 mbar)
More recently, the influence of bleaching and deodoriza-
is very important [49] because it allows a reduction of the
tion conditions on total tocopherol and tocotrienol reten-
deodorization temperature without affecting the vapor-
tion has been studied [33] (Tab. 17). In this case, an
ization efficiency.
increase of tocopherol and tocotrienol contents was not
observed during bleaching. Pre-treatment with active
carbon decreased the b-carotene contents of the Even if single-temperature deodorizers are still the most
bleached and of the refined oil. Low quantities of steam economical for palm oil, working at different tempera-
did not modify the b-carotene content of the refined oil, tures (dual temperature) is an asset to reach the best
while affecting the final acidity and improving tocopherol compromise between the required residence time for
and tocotrienol retention. deodorization (performed at low temperature) and heat
bleaching and final stripping at higher temperature for a
brief period.
10 Future developments in palm oil refining
Furthermore, a design including a structured packing for
It becomes clear that good-quality palm oils are made in oil stripping, able to reduce steam consumption and
the plantation and not in the factory. Indeed the quality of operating costs, perfectly fits with the requirements of a
a fully refined palm oil is highly dependent on and com- high-acidity oil like palm oil.

Tab. 17. Effect of pre-treatment and deodorization conditions on tocopherol and tocotrienol contents of palm oil [33].
Pre-treatment conditions$ Deodorization conditions FFA (as b-Carotene [ppm] Tocopherols and
palmitic) before and after tocotrienols [ppm] before
[%] deodorization and after deodorization
Acid pre-treatment and bleaching with 260 7C, 3 mbar, 0.2% steam, 50 min 0.09 107/2.0 808/684
1.5% BE (95 7C, 30 min)
260 7C, 3 mbar, 1% steam, 50 min 0.03 107/1.5 808/496
Acid pre-treatment, bleaching with 260 7C, 3 mbar, 0.2% steam, 50 min 0.08 87/1.0 797/659
1.5% BE (95 7C, 30 min) and treatment
with 0.4% AC (80 7C, 30 min)
260 7C, 3 mbar, 1% steam, 50 min 0.03 87/1.0 797/487
$
Crude palm oil: FFA, 5.3% (as palmitic); DOBI, 2.5; b-carotene, 459 ppm; tocopherol and tocotrienol content, 972 ppm.
BE: Tonsil Optimum 210 FF; AC: activated carbon.
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Crude Palm Oil Refining Process by Gibon 2007

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Eur. J. Lipid Sci. Technol. 109 (2007) 315–335 DOI 10.1002/ejlt.

Véronique Gibon Palm oil refining

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Carotenoids (and in particular b-carotene) are known for

3.1 FFA content

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Fig. 2. Two-stage counter-current bleaching with pre-filtration.

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

ing earth and potentially toxic spent activated carbon.

5.2.5 Packed (fixed)-bed bleaching

Packed- (or fixed-) bed bleaching is used in some re-

Fig. 4. Multi-stage modular bleaching (Combiclean) [29].

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

In the physical refining of crude palm oil, full reduction of

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

5.2.9 Catalytic properties of bleaching earths 5.2.10 Irradiation bleaching

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Fig. 5. Continuous vertical deodorizer (De Smet) [38].

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Fig. 6. Packed column stripper (Alfa-

Fig. 7. Modular single-vessel stand-alone deodorizer (Qualistock-De Smet) [38].

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

FFA (as palmitic) [%] 3.8 0.08

FFA 87.4 98.1

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Good results (saponification color of 3R 5”1/4 or lighter)

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Crude palm oil (DOBI: 3.3)

Bleaching with 1.5% BE and refining at 280 7C 0.9 3.6

BE: Tonsil Optimum 210 FF.

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

Crude Bleached RBD

a-tocopherol 190 220 233 223 147 125 150

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.ejlst.com

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