Note: Descriptions are shown in the official language in which they were submitted.
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The i~lve~tion relates to a proces~, for purifying
i phosphatides and the phosphatide product obtained by said
¦ process.
I Conventionally phosphatides are obtained from beans,
in particular soya beans and other phosphatide-containing
materials. In the processing of beans the phosphatides
; are, for nstance, obtained by pressing or solvent
; extraction of the beans and by separating the phosphatides
from the resulting crude oils by a treatment with water or
i 10 aqueous solutions.
.'
I The aqueous sludge obtained contains phospholipids,
; a certain proportion of oil, fatty acids, carbohydrates,
¦ proteins, mineral salts, sterols, some remainders of the
j bean shelIs and occasionally other materials. The sludge
¦ 15 may be dried to obtain a yellow to black mass with a wax-
i like consistency. The phosphatides may be subjected to
'¦ various treatments such as removal~of the oil, replace-
ment of the oil by another oil~ hydroxylat~on and hydro-
i - lysis, either by en~ymatic action or by acidic or alkaline
hydrolysis. :~
Until now, however, it has been very difficult to
I remove from the phosphatides some of the materials which
i ,
i render them less suitable for certain applications.
~ U.S. Patent Specification 2,201,064 describes a
.~j ,:-
91 25 purification process in which dried phosphatides are
. r dissolved in hexane. Bel~ian patent 590,731 describes a
~ purification process in which dried crude phosphatides
.j . .
are treated with e.g. hexane and e.g. acetone which may
contain up to 10% of water.
!
These prior art processes do not yield atransparent ~i~
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495Sl
phosphatide product.
It has now been found that a purified phosphatide
product is obtained when phosphatides are subjected to the
combined action of a hydrophobic liquid and an a~ueous
liquid. The two liquids are separated and the purified -
phosphatide product is recovered from the hydrophobic liquid.
According to the process of the invention a
transparent phosphatide product is obtained.
Surprisingly it has been found that the presence
of an appreciable amount of a polar organic solvent, dissolved
in the aqueous liquid, adversely affects the purification. It
is therefore a special feature of the instant invention to
carry out the process while less than 30% by weight, preferably
less than 10% of the aqueous liquid consists of an organic
polar solvent.
`(~ The process of the invention produces a purified
phosphatide product which is transparent. Moreover, much of
the disagreeable ~ff-flavour normally associated especially
, . . .
with conventional hydrolysed phosphatides appears to have been
removed during the purification treatment.
.
The hydrophobic liquid to be used in accordance
with the present invention may be any hydrophobic liquid
in which phosphatides are soluble. Examples are aliphatic,
I preferably saturated hydrocarbons, preferably alkanes such
.j '
as heptane, hexane and pentane~ Cyclic alkanes such as
cyclohexane are also suitable. Aromatic compounds such as
benzene may also be used. Hexane is -
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preferred. The aqueous liquid will normally be water which,
however, may contain some proportion of another liquid or
other liquids dissolved or dispersed therein.
¦ One preference as stated above ls the absence of
substantial amounts of po]ar organic liquids from the
i aqueous liquid. The presence of substantial amounts of
polar organic liquids tends to make the subsequent
`¦ ' ! separation of hydrophobic liquid and aqueous liquid more
difficult. Moreover, it has been found that polar organic
liquids cause the recovery of the phosphatide product from
the hydrophobic liquid to be more troublesome and affect
¦ the quality of the product adversely. Smaller quantities,
; on the contrary, do not exhibit these undesirable
characteristics, and may even facilitate the separation of
hydrophobic liquid and aqueous liquid.
~ Another preference is the presence in the aqueous
; liquid of a minor amount of a bleaching agent. A suitable
~ ~ . , .
agent is H202. Suitable quantities are 0.5-5%, preferably
0.5-2% by weight, based on the aqueous liquid.
` 20 The t~rm "phosphatides" as used herein denotes a
mixture of phopholipids and other materials (other than ;
water) çomprising non-lipid materials as is, for instance,
~ . :
i obtained in the aqueous sludge described above, possibly
after one or more of the treatments also described above.
Such products are also often referred to as "lecithin". -
The amount of aqueous liquid to be used in accordance
with the process of the invention is preferably between
5 and 150% by volume of the phosphatides, more preferably
between 50 and 100%.
The amount of hydrophobic liquid to be used in the
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process of the invention is preferably between 200 and
¦ ,l 2000% by volume of the phosphatides, more preferably
! between 400 and 600%.
The process is preferably carried out while the amount
(by volume) of hydrophobic liquid is about 1 to a~out 3
times, preferably about twice, as large as the amount (by
volume) of phosphatides plus aqueous liquid.
- The sequence in which the two liquids are added to the
phosphatides is immaterial. In a preferred embodiment
the hydrophobic liquid is added to the aqueous sludge
described above containing the phosphatides, optionally
after some other treatment like, for instance, hydrolysis
of the phospholipids. This procedure has the advantage
that the need for an intermediate drying step is obviated.
The manner in which the two liquids are separated is
not essential. Centrifuging is preferred.
Recovery of the purified phosphatide product from
the hydrophobic liquid is preferably by evaporation.
The temperature and pressure at which the process is
carried out can vary within wide limits. Atmospheric -
pressure at ambient temperature is preferred.
The purified phosphatide product obtained is trans-
`~ parent and superior to the untreated one with respect to
odour, taste and oil-solubility. The product can
especially usefully be applied in food preparations like
margarine. Still another advantage of the purified
phosphatide product according to the invention is its
good oil solubility as compared with conventional products.
The advantages of the process according to the
invention are especially pronounced when the process is
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cL 540
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applied to phosphatides which have been hydrolysed by
pancreatin.
! The invention is illustrated by the following
- ~ examples.
EXA~PLE I
. _
100kg crude soybean phosphatide sludge containing
33% of water were homogenised with 200 1 hexane and
centrifuged. The transparent hexane phase emerging from
the centrifuge was evaporated in two stages, in the first
stage in a vertical evaporator, in the second stage in ~
a thin film evaporator. As compared with the phosphatides -
, ~ ,: .
recovered in the conventional way, i.e. by drying of the
sludge, the phosphatides obtained showed the following
properties.
conventionalprocess of
process the invention ~-
Acetone-insoluble 6 6
matter (1) % 3 3
Moisture (2) % 0.5 -~ 0.05
Colour/Gardner (3) 10 10 ;
Colour / Iodine (4) 20 18
Colour/Lovibond (5) 35 g + 3.6 r + 35 + 3.2
. .
Sugar (calc. on ~ ~ F ~ r :
; 25 saccharose) (6) ~ ' ' J 1 .
Transparency (7) % 12.8 84.5
Acid Value (8) 23 23
Phosphorus (9) % 1.93 2.0
. Iron (10) ppm 152 73
Composition with settles does not settle
(1) Acetone-insoluble matter determined according to
the Official and Tentative Methods of the American Oil
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cL 540
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9551
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' Chemists' Society.
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(2) Modified Karl Fischer Method according to the
Official and Tentative Methods of the American Oi'
Chemists' Society.
(3) Official and Tentative Methods of the A.O.C.S.
(4) Methods of the Deutsche Gesellschaft fUr Fett-
wissenschaft, Munster/Westf.
' (5) Methods of the A.O.C.S.
' (6) ditto
(7) Transparency was determined as follows:
The material is heated to 50C in a waterbath.
It is then dissolved with stirring in equal parts by
weight of xylol.
' Turbidity of the solution is measured in a turbidity
~- 15 measuring unit sold by B. Lange GmbH, Berlin, Germany.
The transparency of the solution is Tv = 100 - t,
wherein t is the measured turbidity.
The extinction of the solution is Ev ~ logLv~
' The transparency of the material is then calculated
from the formula
v . 2 = log
(8~ Methods of the A.O.C.S.
' (9) ditto
'' (10) Methods of the Deutsche Gesellschaft fur Fett- '
' ' 25 wissenschaft, Munster/Westf. '
EXAMPLE II ;
100 kg of crude soybean phosphatide sludge
'~ containing 55% of water were''t'reated as described in
Example I. The loss of sludge, calculated on the dry
matter, amounted to abt. 9.5% Analytical results:
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conventional process of the
.~ processinvention
Acetone-insoluble % ~ 67 67
~ matter
'! 1' 5 Moisture % o.6S 0.05
Colour/Iodine 24 22
, Sugar % 3.2 1.7
Transparency % 10 88
! I Acid Value 18 18
I , 10 Phosphorus % 1.962.04
Iron ppm 280 135
20% oil settlesdoes not settle -
~, j EXAMPLE III
i 15 10 kg of crude soybean phosphatides were homogenised -
with 10 l water. The sludge was then homogenised with401 -
¦ cyclohexane and the mixture was centrifuged. The white
; ., . .:
¦ solvent phase was evaporated. The phosphatides thus ~ ~
.
¦ obtained were transparent. Analysis showed that the
sugar content decreased to abt. 40~ and the iron content
¦ to abt. 55% of the starting value. The P-content had
risen by 0.04%. Colour, acetone-insoluble matter and acid
¦ value had remained substantially constant. -.
~I EXAMPLE IV
_j
10 kg crude soybean phosphatides were dissolved in 40 l - -
hexane. Subsequently 10 l water was stirred into the
o solution. After 10 min stirring the solution was allowed
to settle. After a resting period of 5 h and separation
- of the phases the hexane solution was evaporated. The
phosphatides thus obtained were transparent. The analyt-
i ical data corresponded to those of the preceding examples.
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EXAMPLR V
j ¦ 10 kg crude phosphatide sludge, which had been
hydrolysed enzymatically according to USP 3,652,397, were
homogenised with 20 1 hexane and centrifuged. The
hydrolysed phosphatides isolated from the hexane phase
: were transparent. The sugar and iron contents had been
reduced to about half the star~ing values.
The P-value had increased by 0.05%. The other
values (colour, acetone-insoluble matter, acid value) had
remainel constant.
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