CA2042828A1 - Mid-fraction production by fractional crystallization with stearin and olein fraction recycling to interesterification - Google Patents
Mid-fraction production by fractional crystallization with stearin and olein fraction recycling to interesterificationInfo
- Publication number
- CA2042828A1 CA2042828A1 CA 2042828 CA2042828A CA2042828A1 CA 2042828 A1 CA2042828 A1 CA 2042828A1 CA 2042828 CA2042828 CA 2042828 CA 2042828 A CA2042828 A CA 2042828A CA 2042828 A1 CA2042828 A1 CA 2042828A1
- Authority
- CA
- Canada
- Prior art keywords
- fraction
- topping
- olein
- bottoming
- fractional
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0008—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
ABSTRACT
The invention relates to a method for the production of mid-fraction by fractional crystallization of fatty substances, in which:
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a bottoming fractional crystallization treatment providing the mid-fraction and an olein bottoming fraction;
iii) the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal-lization treatment.
The invention relates to a method for the production of mid-fraction by fractional crystallization of fatty substances, in which:
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a bottoming fractional crystallization treatment providing the mid-fraction and an olein bottoming fraction;
iii) the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal-lization treatment.
Description
: ~ ~
~, 1 Mid-fraction production by fractional crystallization with stearin and olein fraction recycling to interesterification The present invention relates to a method for the produc-tion of mid-fraction by fractional crystallization of fatty substances, including fats and glyceride oils. In particular, the invention relates to the production of mid-fraction by tapping fractional crystallization and bottoming fractional 10 crystallization, in which the stearin topping fraction and olein bottoming fraction ~ormed as byproducts are mixed and interesterified, and the interesterified mixture is recycled as additional feedstock.
Natural glyceride oils and fats comprise a great many dif-15 ferent triglycerides, the physical prop~rties of which to alarge extent are determined by the chain lengths and the de-grees of unsaturation of the fatty acid moieties. To make natu-ral glyceride oils or fats more suitable for particular appli-cations it is often required to separate them into fractions 20 characterized by fatty acid glyceride distributions which are homogeneous with respect to the melting behavioux.
The fractional ~rystalliization may be carried out on the oils and ~ats as such (dry fractionation) or after mixing with ~ a solvent (solvent fractionation~. In the fractional crystalli-25 zation treatment the oil is cooled to a temperature at whichonly a higher melting triglyceride fraction crystallizes, fol-lowed by separation of the crystallized solids (stearin fracti-on) from the liguid fraction (olein fraction) e.g. by filtrati-on or ce~trifugation.
In the production of mid-fraction the oil or fat is first sub~ected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping frac-tion. This olein topping fraction is subjected to a bottoming fractional crystalliza~ion treatment at a lower crystallization 35 temperature, providing the aimed mid-fraction and an olein bottoming fraction.
It is understood that the topping fractional crystalliza-tion treatment and the bottoming fractional crystallization treatment may comprise more than one consecutive fractional . .
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" , . .. .
crystallizations in which the olein fraction and/or stearin fraction are passed to the next or former fractional crystalli-zation.
Mid-fraction is a desired starting oil or ~at blend for 5 producing margerines. Mid-fraction possesses a good consistency and a good melting performance imparting the margerines obtai-ned good organoleptic properties and a suitable consistency at a temperature within the range of 15-~5C. However, the produc-tion o~ mid-fraction inevitably results in the formation of two 10 byproducts, namely a stearin topping fraction and an olein bottoming fraction. These fractions are generally less valua-ble, ~io that the method for the production of mid-fraction is not optimal from an economic point of view.
The invention is based on the ~inding, that when the feed-15 stock comprising fatty substances, used for the production ofmid-fraction has a fatty acid composition of the triglycerides which is similar to that o~ the mid-fraction produced, and the stearin topping fraction and the olein bottoming fraction are mixed and this mixture is randomly interesterified, this inter-20 esterified mixture should have a fatty acid composition similarto that of the ~eedstock and may be recycled, substantially avoiding the formation of byproducts.
- Accordingly, tha present invention provides a method for the production of mid-fraction by fractional crystallization of 25 ~atty substances, in which:
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment pro-viding a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a ~ottoming fractional crystallization treakment providing the mid-fraction and an olein bottoming ~raction:
iii)the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal lization treatment.
A requisite ~or the method according to the invention is, that the stearin topping ~raction and the olein bottoming ~,j s .
.. .
':
. ". :: . ; . , ,, , , , ,-, . :. , . . , .; , ~ ~ . ~ . .... . .. .
. ..
',:' ' ' ' ," ',' ', . ~ ~ ,': ;' . ' ', -~ 3 fraction are subjected to a random interesterificati~n. There-fore, the method according to the invention is not suitable for the production of mid-fraction comprising specific symmetrical or asymmetrical triglycerides.
As feedstocks any fatty substance may be used, such as semi-solid glyceride oils and fats of vegetable, animal or marine origin, such as fully or substantially hydrogenated palm oil, palm kernel oil, tallow, butter fats, fish oils, sunflower oil and their solvent or dry fractionated stearin or olein 10 fractions. Preferred ~eedstock components comprise hydrogenated palm oil, hydrogenated palm kernel oil, fractionated palm oil stearin, sunflower oil, such as palm oil hardened to a melting point of 58C (Cl6 40-50%;Cl8 60-50%), hardened palm oil stea-rin (C76 50-85%;Cl8 50-15~), hydrogenated palm kernel oil har-15 dened to a melting point of 39C (Cl2 45-55%; Cl4 12-18%; Cl6 5-10~; Cl8 12 25%), hydrogenated palm kernel oil stearin har-dened to a melting point of 41C ~Cl2 50-60%; Cl4 15-25%; Cl6 5-10~; Cl8 5-12%~ and sunflower oil hardened to a melting point of 69C (Cl~ 5-10%;Cl8 95-90%). Using these feedstock 20 components any practical distribution of fatty acids in trigly-cerides of mid-fraction may be formulal:ed.
Using these hardened feedstock components, for mid-fracti-on obtained by solvent fractionation, preferably the mid-fraction obtained has a H3 (>C50 ) of less 25 than 13, prefera~l~ less than 11, and a H2 M value (C44 ~ C46 ~
C48 ) which is as large as possible, generally higher than 60, pref~rably higher than 64, and a H3 ~H2 M value which is as large as possible, generally larger than 70.
For mid-fraction obtained by dry fractionation the H3 value 30 is generally less than 16, preferably less than 15. The H2 M
value i~ generally larger than 45, preferably larger than 50.
The H3 +H2 M value is generally larger than 65.
The interesterification used in the method according to the invention comprises any suitable interesterification pro-35 cess, by which the fatty acids o~ the triglycerides are random-ly ex~hanged. Any prior art interesterification process might be used, such as the proces disclosed in EP-A-76,682. Preferred is a catalyst comprising an alkaline metal or hydroxide. Prefe-rably the catalyst system comprises sodium or sodium hydroxide, .. . .
,}. :
' ' ' , ,,: ' ' ' ' :, ,' ' , ':, ' ~, ,",; . ~ ' , ' '.. : . '~ ' ' ' ' . ~ ','. ' ' , ', . . ,' . .:, ,. . . : . ' ' .- , , ., .
.. . . . . ..
, . .. . :
... . . . . .
glyceride and water in a weight ratio of 1/2/3 to 1/2/7. The catalyst is generally added in a concentration of at least 9.03% by weight sodium hydroxide based on the oil. The informa-tion of the European patent application EP-A-76,682 is included 5 by re~erence.
For an optimal distribution of the fatty acids over the triglycerides, used in the feedstock, it is preferred that the feedstock as well as the stearin topping fraction and olein topping fracti~n are subjected to the interesterification.
Depending on the separation efficiency, the solid particle content, the crystallization temperature and the cooling rate used in the fractional crystallization of the topping fractio-nal crystallization treatment and bottoming fractional crystal-lization treatment, these treatments may comprise more than 15 one, such as two consecutive fractional crystallizations.
When the topping fraction of crystallization treatm~nt comprises two or more consecutive fractional crystallizations, a higher midfraction yield may be obtained when, according to a preferred embodiment the stearin topping fraction originates 20 from the second consecutive topping fractional crystallization, and the olein topping fraction originates from the first conse-cutive topping fractional crystallization.
When the bottoming fractional crystallization treatment comprises two consecutive fractional crystallizations, it may 25 be preferred for obtaining better midfraction quality when the olein bottoming fraction originates from the first consecutive bottoming fractional crystallization, and the mid-fraction originates ~rom the second consecutive bottoming fractional crystallization~
I~ the olein topping or bottoming fraction comprises a relatively high solid content, it is preferred that this frac~
tion is partly recycled to the topping or bottoming ~ractional crystallization treatment whereby the fraction is diluted.
Preferably the recycling ratio of the recycled olein fraction 35 is about 10-60%, more preferably 25-50%.
The consecutive topping and bottoming fractional crystal-lizations may be carried out as countercurrent ~ractional crys-talllzations, such as disclosed in the earlier European patent application to be included.
....
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: , . . , ~ ' . , :: , :, . . -.. . . . . . . . . . . . .
., .
... . . . .. . .
-~ 5 Impurities present in the feedstock or formed during the production of mid-fraction, such as partly saturated triglyce-rides or diglycerides, may accumulate in the recycled stearin topping or olein bottoming fractions. Therefor~, it is prefer-5 red that intermittantly or continuously a minor part of thestearin topping fraction and/or olein bottoming fraction is not recycled but disposed. The disposed fraction may comprise up to about 5% by weight of the recycled olein topping or bottoming ~raction. Alternatively these impurities may be removed inter-10 mittantly or continuously from the recycled fractions, forinstance by adsorption.
The method accordin~ to the invention for the production of mid~fraction will be illustrated hereafter by way of non li-miting examples. The two processes used are shown in the an 15 nexed single drawing in which each box refers to a fractional crystallization and the subsequent separation of the stearin fra~tion from the olein fraction.
In a batchwise process it is possible to use only one crystallizer and various storage tanks in which the olein and 20 stearin fractions obtained in the topping fractional crystalli-zation treatment and bottoming fractional crystallization tre-ament are temporarily stored.
EXAMPLE I
Mid-fraction was produced according to method A. Feedstock (F) comprising 47% fully hydrogenated palm oil and 53% fully hydrogenated palm kernel oil was subjeoted to interesterifica-tion ~I) using 0.02% by weight metallic sodium.
In the two consecutive countercurrent fractional crystal-30 lizations 1 and 2 (crystallization temperature 44C and 40C,respectively) of the topping fractional crystallization treat-ment the solid particle content (SPC) was 11~. In the two con-secutive fractional crystallizations 3 and 4 (crystallization temperature 35C and 31C, respectively) of the bottoming frac-35 tional crytallization treatment the SPC was 17%. The stearintopping fraction and the olein bottoming ~raction were recycled to the interestification and mixed with the feedstock in a ra~io of 60/40. Initially the mid-fraction had a H3/H~M value of 12/55 and after steady state of 12/54.
's .... . . . . . . ...
.:: . :
:
For comparison purposes in each fractional crystallization the separation efficiency was kept at 0.5.
Table 1 shows the fatty acid composition (%) of the mid- ¦
fraction and of the feedstock. l~
1 :
Table 1 1, .
Fatty acid composition (%) of the midfraction and the feed after 10 cycles of intPresterification and fractionation.
Chain length Feed Mid in carbon ~' numbers : 8 2.2 2.1 15 10 2.0 2.2 12 26.2 26.0 14 8.9 9.0 1~ ~5.5 25.7 18 34.5 34.7 20 20 0.3 0.3 EX~MPL~
Feedstock comprising 7~ fully hydrogenated, dry fractiona-ted palm oil stearin, 33% fully hydrogenated palm oil and 60%
25 fully hydrogenated palm kernel oil was used for the production : :-of mid-fraction using method ~
In the fractional crystallization of the topping fractio- -nal crystallization treatment SP~ was 8%, and in the fractional : - .:
cry~tallization of the bottoming fractional crystallization :
30 trea~ment SPC was 18~. The topping ætearin fraction 1 and the bottoming olein fraction 2 were recycled to the esterification ; :
and mixed with the feedstock in a ratio of 71/29.
At a separation efficiency of 0.5 the mid~fraction had a ..
H3/H2M value of 15/45.
The ~atty acid composition (%) of the mid-fraction obtai~
ned and of the feedstock is shown in Table 2. ; ~
: ' " ' .
.. ..
Table 2 i '-.
Fatty acid composition (%) of the mid-fraction and the feed after 10 cycles of interesterification and fractionation. ~ :
Chain length Feed Mid in carbon 1.-numbers ~ 2.9 2.7 10 10 2.3 2.2 1~ 29.3 29.4 1~ 9.6 9.1 16 24.6 25.0 18 31.3 31.6 EXAMPLE III
The same process as used in Example II was used, but the olein fractions were recycled at a recycling ratio of 50% on ~ :
the f2ed. In the topping fractional crystallization treatment 20 SPC was 5.4% and in the bottoming fractional crystallization ~.
treatment SPC was 12%. The mid-fraction obtained had a H3/H2M
value of 15/45.
EXAMPLE IV
Feedstock, ~omprising 1,5~ fully hydrogenated sunflower -.
oiI, 46,5% fully hydrogenated palm oil, 26% fully hydrogenated palm kernel oil and 26% fully hydrogenated palm kernel stearin was processed according to method A. In the topping fractional crystallization treatment the SPC in the crystallizations 1 and 30 2 was 8%. In the bottoming fractional crystallization treatment the SPC of ~he fractional crystallizations 3 and 4 was 16%. The stearin topping fraction and olein bottoming fraction were recycled and mixed with the feedstock in ratio of 62/38. At a separation eff.iciency of 0.5, the H3/H2M value of the mid-frac- :
35 tion was 12/49.
Table 3 shows the fatty acid composition (%) o~ the mid-fraction and of the feedstock. -................................................................... .
. ~ : . ., .. . . .. ~ .. . . . , . , ~ . . :
. ,' ' , . , . . ~ , .: ,' : : .. ~ :
,. . . . .
, ,~ 8 Table 3 Fatty acid composition (%) of the mid-fraction and the feed after 15 cycles of interesterification and fractionation.
1.
Chain length Feed Mid in carbon ', numbers 8 1.8 1.8 10 10 1.7 1.8 12 27.5 27.4 14 10.3 10.4 16 25.6 25.3 18 33.1 33.3 ~ :
EXAMPLE V
A feedstock comprising 42% hydrogenated palm kernel stea-rin, 53% hydrogenated palm oil and 5% hydrogenated sunflower oil, was subjected to sol~ent fractionation in acetone in a 20 r~tio o~ 1/5 wt/wt. In the topping fractional crystallization :.
treatment SPC was 29% and the crystallization temperature about 30C. In the bottoming fractional crystallization treatment SPC
was 33% ~on present fat) and the crystallization temperature : :
was about 20C. The stearin topping fraction 1 and the olein 25 bottoming ~raction 2 were recycled and after removal of the :
acetone, mixed with the feedstock in a ratio of 47.5/52.5, andthereafter interesterified. The fatty acid composition o~ :
the mid ~raction resembles closely the composition o~ the ~eed-stockj see Table 4.
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'l ~- 9 ~ ;
Table 4 .
The fatty acid compositio~ (%) of the mid-fraction and thP
feedstock after 10 cycles of interesterification and fractiona-tion.
~
Chain lengthFeedstock Mid :
in carbon :
numbers 8 l.l 1.3 10 10 1.2 1.3 `
12 23.8 23.8 14 10.0 9.4 16 28.0 28.5 18 35.5 35.7 The H3/H2M value of the mid-fraction was 14/59. From time to time it was:necessery to remove diacylglycerols by adsorp-tion on silica. The time period between the removal procedures of these impurities was depending on th~ composition of the fePdstock. , ' ~ ~
EXAMPLE VI . -A feedstock romprising 85% palm oil and 15~ solvent frac- :
tionated palm oil stearin was used in method B. The mid-fracti-on obtained had a constant composit:ion of 1.2%S3 , 67%S2 0, 25 6.3%S2 Li and 25,5~ others.
EXAMPLE V~II
Midfraction was produced according to method C. Feedstock comprising 43% fully hydrogenated palm kernel oil was subjected 30 to interesterification (I) using O.OZ% metallic sodium. In the two consecutive countercurrent fractional crystallizations 1 and 2 (crystallization temperatures of 44 and 48C, respective-ly) of the topping fractional crystallization treatment the ~:
solid particle content (SPC) was 18.5%. In the bottoming frac-35 tional crystallization 3 (crystallization temperature of 38~
of the bottoming fractional crystallization treatment the SPC
was 30%. The stearin topping fraction and the olein bottoming fraction were recyaled to the interesterification and mixed with the feedstock in a ratio of 50/50. In the steady state the . , .
', ' . : :' ,~. , .
'l '-- 10 , , ~
H3/H2M ratio was 12/52. For comparison purposes the separation !J
efficiency was kept at 0.5. Table 5 shows the fatty acid compo-sition (%) of the midfraction and of the feedstock. Usually, method C may be used in systems in which the SE is still high ?~
5 at a high SPC.
Table 5 Fatty acid composition t%) of the feed and of the midfrac-tion after 10 -cycles of interesterification and fractionation 10 (method C~. :
Chain lengthFeedstock Mid in carbon l~ .
numbers I ::
8 2.2 2.1 : -2.1 2.0 ;~
12 27.1 27.4 - .
14 8.g 9.2 . ~
16 25.5 26.1 : .
18 33.5 33.3 0.3 0.3 , '. ' ~ ~ . ' . ~, .
~,
~, 1 Mid-fraction production by fractional crystallization with stearin and olein fraction recycling to interesterification The present invention relates to a method for the produc-tion of mid-fraction by fractional crystallization of fatty substances, including fats and glyceride oils. In particular, the invention relates to the production of mid-fraction by tapping fractional crystallization and bottoming fractional 10 crystallization, in which the stearin topping fraction and olein bottoming fraction ~ormed as byproducts are mixed and interesterified, and the interesterified mixture is recycled as additional feedstock.
Natural glyceride oils and fats comprise a great many dif-15 ferent triglycerides, the physical prop~rties of which to alarge extent are determined by the chain lengths and the de-grees of unsaturation of the fatty acid moieties. To make natu-ral glyceride oils or fats more suitable for particular appli-cations it is often required to separate them into fractions 20 characterized by fatty acid glyceride distributions which are homogeneous with respect to the melting behavioux.
The fractional ~rystalliization may be carried out on the oils and ~ats as such (dry fractionation) or after mixing with ~ a solvent (solvent fractionation~. In the fractional crystalli-25 zation treatment the oil is cooled to a temperature at whichonly a higher melting triglyceride fraction crystallizes, fol-lowed by separation of the crystallized solids (stearin fracti-on) from the liguid fraction (olein fraction) e.g. by filtrati-on or ce~trifugation.
In the production of mid-fraction the oil or fat is first sub~ected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping frac-tion. This olein topping fraction is subjected to a bottoming fractional crystalliza~ion treatment at a lower crystallization 35 temperature, providing the aimed mid-fraction and an olein bottoming fraction.
It is understood that the topping fractional crystalliza-tion treatment and the bottoming fractional crystallization treatment may comprise more than one consecutive fractional . .
,, ., . , , ~ .
'.,':'",' ~' ' ,' ~ , ' ' ,,; ',, . '".". ,,'. ' ,,, '', , ' ,~ ' .", .,', ; ,' , :, , '; , ' , , .,. ' .~ , ;,. " : ;: ',, ,, : , , " , . . .
" , . .. .
crystallizations in which the olein fraction and/or stearin fraction are passed to the next or former fractional crystalli-zation.
Mid-fraction is a desired starting oil or ~at blend for 5 producing margerines. Mid-fraction possesses a good consistency and a good melting performance imparting the margerines obtai-ned good organoleptic properties and a suitable consistency at a temperature within the range of 15-~5C. However, the produc-tion o~ mid-fraction inevitably results in the formation of two 10 byproducts, namely a stearin topping fraction and an olein bottoming fraction. These fractions are generally less valua-ble, ~io that the method for the production of mid-fraction is not optimal from an economic point of view.
The invention is based on the ~inding, that when the feed-15 stock comprising fatty substances, used for the production ofmid-fraction has a fatty acid composition of the triglycerides which is similar to that o~ the mid-fraction produced, and the stearin topping fraction and the olein bottoming fraction are mixed and this mixture is randomly interesterified, this inter-20 esterified mixture should have a fatty acid composition similarto that of the ~eedstock and may be recycled, substantially avoiding the formation of byproducts.
- Accordingly, tha present invention provides a method for the production of mid-fraction by fractional crystallization of 25 ~atty substances, in which:
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment pro-viding a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a ~ottoming fractional crystallization treakment providing the mid-fraction and an olein bottoming ~raction:
iii)the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal lization treatment.
A requisite ~or the method according to the invention is, that the stearin topping ~raction and the olein bottoming ~,j s .
.. .
':
. ". :: . ; . , ,, , , , ,-, . :. , . . , .; , ~ ~ . ~ . .... . .. .
. ..
',:' ' ' ' ," ',' ', . ~ ~ ,': ;' . ' ', -~ 3 fraction are subjected to a random interesterificati~n. There-fore, the method according to the invention is not suitable for the production of mid-fraction comprising specific symmetrical or asymmetrical triglycerides.
As feedstocks any fatty substance may be used, such as semi-solid glyceride oils and fats of vegetable, animal or marine origin, such as fully or substantially hydrogenated palm oil, palm kernel oil, tallow, butter fats, fish oils, sunflower oil and their solvent or dry fractionated stearin or olein 10 fractions. Preferred ~eedstock components comprise hydrogenated palm oil, hydrogenated palm kernel oil, fractionated palm oil stearin, sunflower oil, such as palm oil hardened to a melting point of 58C (Cl6 40-50%;Cl8 60-50%), hardened palm oil stea-rin (C76 50-85%;Cl8 50-15~), hydrogenated palm kernel oil har-15 dened to a melting point of 39C (Cl2 45-55%; Cl4 12-18%; Cl6 5-10~; Cl8 12 25%), hydrogenated palm kernel oil stearin har-dened to a melting point of 41C ~Cl2 50-60%; Cl4 15-25%; Cl6 5-10~; Cl8 5-12%~ and sunflower oil hardened to a melting point of 69C (Cl~ 5-10%;Cl8 95-90%). Using these feedstock 20 components any practical distribution of fatty acids in trigly-cerides of mid-fraction may be formulal:ed.
Using these hardened feedstock components, for mid-fracti-on obtained by solvent fractionation, preferably the mid-fraction obtained has a H3 (>C50 ) of less 25 than 13, prefera~l~ less than 11, and a H2 M value (C44 ~ C46 ~
C48 ) which is as large as possible, generally higher than 60, pref~rably higher than 64, and a H3 ~H2 M value which is as large as possible, generally larger than 70.
For mid-fraction obtained by dry fractionation the H3 value 30 is generally less than 16, preferably less than 15. The H2 M
value i~ generally larger than 45, preferably larger than 50.
The H3 +H2 M value is generally larger than 65.
The interesterification used in the method according to the invention comprises any suitable interesterification pro-35 cess, by which the fatty acids o~ the triglycerides are random-ly ex~hanged. Any prior art interesterification process might be used, such as the proces disclosed in EP-A-76,682. Preferred is a catalyst comprising an alkaline metal or hydroxide. Prefe-rably the catalyst system comprises sodium or sodium hydroxide, .. . .
,}. :
' ' ' , ,,: ' ' ' ' :, ,' ' , ':, ' ~, ,",; . ~ ' , ' '.. : . '~ ' ' ' ' . ~ ','. ' ' , ', . . ,' . .:, ,. . . : . ' ' .- , , ., .
.. . . . . ..
, . .. . :
... . . . . .
glyceride and water in a weight ratio of 1/2/3 to 1/2/7. The catalyst is generally added in a concentration of at least 9.03% by weight sodium hydroxide based on the oil. The informa-tion of the European patent application EP-A-76,682 is included 5 by re~erence.
For an optimal distribution of the fatty acids over the triglycerides, used in the feedstock, it is preferred that the feedstock as well as the stearin topping fraction and olein topping fracti~n are subjected to the interesterification.
Depending on the separation efficiency, the solid particle content, the crystallization temperature and the cooling rate used in the fractional crystallization of the topping fractio-nal crystallization treatment and bottoming fractional crystal-lization treatment, these treatments may comprise more than 15 one, such as two consecutive fractional crystallizations.
When the topping fraction of crystallization treatm~nt comprises two or more consecutive fractional crystallizations, a higher midfraction yield may be obtained when, according to a preferred embodiment the stearin topping fraction originates 20 from the second consecutive topping fractional crystallization, and the olein topping fraction originates from the first conse-cutive topping fractional crystallization.
When the bottoming fractional crystallization treatment comprises two consecutive fractional crystallizations, it may 25 be preferred for obtaining better midfraction quality when the olein bottoming fraction originates from the first consecutive bottoming fractional crystallization, and the mid-fraction originates ~rom the second consecutive bottoming fractional crystallization~
I~ the olein topping or bottoming fraction comprises a relatively high solid content, it is preferred that this frac~
tion is partly recycled to the topping or bottoming ~ractional crystallization treatment whereby the fraction is diluted.
Preferably the recycling ratio of the recycled olein fraction 35 is about 10-60%, more preferably 25-50%.
The consecutive topping and bottoming fractional crystal-lizations may be carried out as countercurrent ~ractional crys-talllzations, such as disclosed in the earlier European patent application to be included.
....
..... .
.. - . . ... . . . , , , . . ~ .. . .. . . .
.: . . : . . ,, , . . ~ :.
: , . . , ~ ' . , :: , :, . . -.. . . . . . . . . . . . .
., .
... . . . .. . .
-~ 5 Impurities present in the feedstock or formed during the production of mid-fraction, such as partly saturated triglyce-rides or diglycerides, may accumulate in the recycled stearin topping or olein bottoming fractions. Therefor~, it is prefer-5 red that intermittantly or continuously a minor part of thestearin topping fraction and/or olein bottoming fraction is not recycled but disposed. The disposed fraction may comprise up to about 5% by weight of the recycled olein topping or bottoming ~raction. Alternatively these impurities may be removed inter-10 mittantly or continuously from the recycled fractions, forinstance by adsorption.
The method accordin~ to the invention for the production of mid~fraction will be illustrated hereafter by way of non li-miting examples. The two processes used are shown in the an 15 nexed single drawing in which each box refers to a fractional crystallization and the subsequent separation of the stearin fra~tion from the olein fraction.
In a batchwise process it is possible to use only one crystallizer and various storage tanks in which the olein and 20 stearin fractions obtained in the topping fractional crystalli-zation treatment and bottoming fractional crystallization tre-ament are temporarily stored.
EXAMPLE I
Mid-fraction was produced according to method A. Feedstock (F) comprising 47% fully hydrogenated palm oil and 53% fully hydrogenated palm kernel oil was subjeoted to interesterifica-tion ~I) using 0.02% by weight metallic sodium.
In the two consecutive countercurrent fractional crystal-30 lizations 1 and 2 (crystallization temperature 44C and 40C,respectively) of the topping fractional crystallization treat-ment the solid particle content (SPC) was 11~. In the two con-secutive fractional crystallizations 3 and 4 (crystallization temperature 35C and 31C, respectively) of the bottoming frac-35 tional crytallization treatment the SPC was 17%. The stearintopping fraction and the olein bottoming ~raction were recycled to the interestification and mixed with the feedstock in a ra~io of 60/40. Initially the mid-fraction had a H3/H~M value of 12/55 and after steady state of 12/54.
's .... . . . . . . ...
.:: . :
:
For comparison purposes in each fractional crystallization the separation efficiency was kept at 0.5.
Table 1 shows the fatty acid composition (%) of the mid- ¦
fraction and of the feedstock. l~
1 :
Table 1 1, .
Fatty acid composition (%) of the midfraction and the feed after 10 cycles of intPresterification and fractionation.
Chain length Feed Mid in carbon ~' numbers : 8 2.2 2.1 15 10 2.0 2.2 12 26.2 26.0 14 8.9 9.0 1~ ~5.5 25.7 18 34.5 34.7 20 20 0.3 0.3 EX~MPL~
Feedstock comprising 7~ fully hydrogenated, dry fractiona-ted palm oil stearin, 33% fully hydrogenated palm oil and 60%
25 fully hydrogenated palm kernel oil was used for the production : :-of mid-fraction using method ~
In the fractional crystallization of the topping fractio- -nal crystallization treatment SP~ was 8%, and in the fractional : - .:
cry~tallization of the bottoming fractional crystallization :
30 trea~ment SPC was 18~. The topping ætearin fraction 1 and the bottoming olein fraction 2 were recycled to the esterification ; :
and mixed with the feedstock in a ratio of 71/29.
At a separation efficiency of 0.5 the mid~fraction had a ..
H3/H2M value of 15/45.
The ~atty acid composition (%) of the mid-fraction obtai~
ned and of the feedstock is shown in Table 2. ; ~
: ' " ' .
.. ..
Table 2 i '-.
Fatty acid composition (%) of the mid-fraction and the feed after 10 cycles of interesterification and fractionation. ~ :
Chain length Feed Mid in carbon 1.-numbers ~ 2.9 2.7 10 10 2.3 2.2 1~ 29.3 29.4 1~ 9.6 9.1 16 24.6 25.0 18 31.3 31.6 EXAMPLE III
The same process as used in Example II was used, but the olein fractions were recycled at a recycling ratio of 50% on ~ :
the f2ed. In the topping fractional crystallization treatment 20 SPC was 5.4% and in the bottoming fractional crystallization ~.
treatment SPC was 12%. The mid-fraction obtained had a H3/H2M
value of 15/45.
EXAMPLE IV
Feedstock, ~omprising 1,5~ fully hydrogenated sunflower -.
oiI, 46,5% fully hydrogenated palm oil, 26% fully hydrogenated palm kernel oil and 26% fully hydrogenated palm kernel stearin was processed according to method A. In the topping fractional crystallization treatment the SPC in the crystallizations 1 and 30 2 was 8%. In the bottoming fractional crystallization treatment the SPC of ~he fractional crystallizations 3 and 4 was 16%. The stearin topping fraction and olein bottoming fraction were recycled and mixed with the feedstock in ratio of 62/38. At a separation eff.iciency of 0.5, the H3/H2M value of the mid-frac- :
35 tion was 12/49.
Table 3 shows the fatty acid composition (%) o~ the mid-fraction and of the feedstock. -................................................................... .
. ~ : . ., .. . . .. ~ .. . . . , . , ~ . . :
. ,' ' , . , . . ~ , .: ,' : : .. ~ :
,. . . . .
, ,~ 8 Table 3 Fatty acid composition (%) of the mid-fraction and the feed after 15 cycles of interesterification and fractionation.
1.
Chain length Feed Mid in carbon ', numbers 8 1.8 1.8 10 10 1.7 1.8 12 27.5 27.4 14 10.3 10.4 16 25.6 25.3 18 33.1 33.3 ~ :
EXAMPLE V
A feedstock comprising 42% hydrogenated palm kernel stea-rin, 53% hydrogenated palm oil and 5% hydrogenated sunflower oil, was subjected to sol~ent fractionation in acetone in a 20 r~tio o~ 1/5 wt/wt. In the topping fractional crystallization :.
treatment SPC was 29% and the crystallization temperature about 30C. In the bottoming fractional crystallization treatment SPC
was 33% ~on present fat) and the crystallization temperature : :
was about 20C. The stearin topping fraction 1 and the olein 25 bottoming ~raction 2 were recycled and after removal of the :
acetone, mixed with the feedstock in a ratio of 47.5/52.5, andthereafter interesterified. The fatty acid composition o~ :
the mid ~raction resembles closely the composition o~ the ~eed-stockj see Table 4.
;::
' "" ..
~ ' '';'' ,, ,.. . . ,,..... . .. . .. -.
'l ~- 9 ~ ;
Table 4 .
The fatty acid compositio~ (%) of the mid-fraction and thP
feedstock after 10 cycles of interesterification and fractiona-tion.
~
Chain lengthFeedstock Mid :
in carbon :
numbers 8 l.l 1.3 10 10 1.2 1.3 `
12 23.8 23.8 14 10.0 9.4 16 28.0 28.5 18 35.5 35.7 The H3/H2M value of the mid-fraction was 14/59. From time to time it was:necessery to remove diacylglycerols by adsorp-tion on silica. The time period between the removal procedures of these impurities was depending on th~ composition of the fePdstock. , ' ~ ~
EXAMPLE VI . -A feedstock romprising 85% palm oil and 15~ solvent frac- :
tionated palm oil stearin was used in method B. The mid-fracti-on obtained had a constant composit:ion of 1.2%S3 , 67%S2 0, 25 6.3%S2 Li and 25,5~ others.
EXAMPLE V~II
Midfraction was produced according to method C. Feedstock comprising 43% fully hydrogenated palm kernel oil was subjected 30 to interesterification (I) using O.OZ% metallic sodium. In the two consecutive countercurrent fractional crystallizations 1 and 2 (crystallization temperatures of 44 and 48C, respective-ly) of the topping fractional crystallization treatment the ~:
solid particle content (SPC) was 18.5%. In the bottoming frac-35 tional crystallization 3 (crystallization temperature of 38~
of the bottoming fractional crystallization treatment the SPC
was 30%. The stearin topping fraction and the olein bottoming fraction were recyaled to the interesterification and mixed with the feedstock in a ratio of 50/50. In the steady state the . , .
', ' . : :' ,~. , .
'l '-- 10 , , ~
H3/H2M ratio was 12/52. For comparison purposes the separation !J
efficiency was kept at 0.5. Table 5 shows the fatty acid compo-sition (%) of the midfraction and of the feedstock. Usually, method C may be used in systems in which the SE is still high ?~
5 at a high SPC.
Table 5 Fatty acid composition t%) of the feed and of the midfrac-tion after 10 -cycles of interesterification and fractionation 10 (method C~. :
Chain lengthFeedstock Mid in carbon l~ .
numbers I ::
8 2.2 2.1 : -2.1 2.0 ;~
12 27.1 27.4 - .
14 8.g 9.2 . ~
16 25.5 26.1 : .
18 33.5 33.3 0.3 0.3 , '. ' ~ ~ . ' . ~, .
~,
Claims (14)
1. Method for the production of mid-fraction by fractional crystallization of fatty substances, in which:
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a bottoming fractional crystallization treatment providing the mid-fraction and an olein bottoming fraction;
iii) the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal lization treatment.
i) a fatty substances comprising feedstock is subjected to a topping fractional crystallization treatment providing a stearin topping fraction and an olein topping fraction;
ii) the olein topping fraction is subjected to a bottoming fractional crystallization treatment providing the mid-fraction and an olein bottoming fraction;
iii) the stearin topping fraction and the olein bottoming fraction are combined and subjected to interesterifi-cation, and the interesterified mixture of fatty sub-stances is recycled to the topping fractional crystal lization treatment.
2. Method as claimed in claim 1, wherein the feedstock and the mixture of stearin topping fraction and olein bottoming fraction are subjected to interesterification.
3. Method as claimed in claims 1 or 2, wherein the topping fractional crystallization treatment comprises at least two consecutive topping fractional crystallizations.
4. Method as claimed in claim 3, wherein the stearin top-ping fraction originates from the second consecutive topping fractional crystallization, and the olein topping fraction originates from the first consecutive topping fractional crys-tallization.
5. Method as claimed in claims 1-4, wherein the bottomng fractional crystallization treatment comprises at least two consecutive bottoming fractional crystallizations.
6. Method as claimed in claims 5, wherein the olein bottoming fraction originates from the first consecutive bottoming fractional crystallization, and the mid-fraction originate from the second consecutive bottoming fractional crystallization
7. Method as claimed in claim 1-6, wherein the olein top-ping fraction is partly recycled to the topping fractional crystallization treatment.
8. Method as claimed in claim 7, wherein the recycling ratio of the olein topping fraction is about 10-60%, preferably about 25-50%.
9. Method as claimed in claims 1-8, wherein the olein bot-toming fraction partly recycled to the bottoming fractional crystallization treatment.
10. Method as claimed in claim 9, wherein the recycling ratio of the olein bottoming fraction is about 10-60%, prefera-bly about 25-50%.
11. Method as claimed in claims 3-10, wherein the consecu-tive topping and/or bottoming fractional crystallizations com-prise countercurrent fractional crystallizations.
12. Method as claimed in claims 1-11, wherein the fractio-nal crystallizations are selected from solvent crystallization and dry crystallization.
13. Method as claimed in claims 1-12, wherein impurities are removed from the stearin topping fraction and/or olein bottoming fraction.
14. Method as claimed in claims 1-13, wherein a minor part of the stearin topping fraction and/or olein bottoming fracti-on, generally up to 5%, is disposed.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP90.109334.4 | 1990-05-17 | ||
| EP90109334 | 1990-05-17 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2042828A1 true CA2042828A1 (en) | 1991-11-18 |
Family
ID=8203992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 2042828 Abandoned CA2042828A1 (en) | 1990-05-17 | 1991-05-17 | Mid-fraction production by fractional crystallization with stearin and olein fraction recycling to interesterification |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0457401A1 (en) |
| AU (1) | AU7708291A (en) |
| CA (1) | CA2042828A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0651046A1 (en) * | 1993-11-02 | 1995-05-03 | N.V. Vandemoortele International | Method for dry fractionation of fatty substances |
| DK2173197T3 (en) * | 2007-07-25 | 2019-09-23 | Bunge Loders Croklaan B V | Course of action |
| WO2009080288A1 (en) | 2007-12-21 | 2009-07-02 | Loders Croklaan B.V. | Process for producing a palm oil product |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB590916A (en) * | 1945-02-13 | 1947-07-31 | Procter & Gamble | Process for improving fats and fatty oils for food and other purposes |
| DE3372902D1 (en) * | 1982-11-22 | 1987-09-17 | Unilever Nv | Margarine fat blend |
| GB2170506B (en) * | 1984-12-17 | 1989-08-23 | Unilever Plc | Edible fats |
-
1991
- 1991-05-09 EP EP19910201120 patent/EP0457401A1/en not_active Withdrawn
- 1991-05-15 AU AU77082/91A patent/AU7708291A/en not_active Abandoned
- 1991-05-17 CA CA 2042828 patent/CA2042828A1/en not_active Abandoned
Also Published As
| Publication number | Publication date |
|---|---|
| EP0457401A1 (en) | 1991-11-21 |
| AU7708291A (en) | 1991-11-21 |
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