DE1492974A1 - Process for the production of a plant phosphatide which is particularly suitable as an emulsifier for oil-in-water emulsions - Google Patents

Description

PATENT LAWYERS

DR. ING. A. VAN DER WERTH I 4 CJ ZC? / 4 DR. FRAN Z LEATHER ER

HAMBURG-HARBURG 8 MÖNCHEN 8

WtItTORfI * »TR. S »■ TIl. (0411) 77 0 * β | 1.UCILe-ORAHNSTR. 32 - TEL. (Οβίΐι 440S46

Munich, July 26, 1965

i / p

Sign in UNILLVEH N.V., iSuseumparic 1, Rotterdam, Holland

A method for producing a ale emulsifier door oil-in-^ acoer tBulsionon becondore £ £ he ~ eoi th Pflanzenphosphatids

The alβ byproducts in the production of vegetable oils by extraction with solvents resulting Pflanaenphoephatide, also called plant lecithins are recovered by DAB hydrating freed from solvent extracted Cl at temperatures between about 95 ⁰ C and 100 C of 1 to 5 y * water, the swollen ochleimetoffe by centrifugation separates from the main volume of the oil and then evaporates them in a vacuum

This Pflansenlecithine, eg "Gojalecithin contain about 50 to 70 / - Fhosphatide, 1 bia 2 ^ 'ater and 23-49 ü Cl. They are used, among other things, in the food and feed industry as Eaulgatoron in the production of water-in-oil bsw · oil-in-water emulsions «

It has now been found that the emulsification of these lecithins, in particular of 0.1alecithins, can be improved considerably for C / .t-uyatoEe, if the lecithm paste can be diluted with such lecithins before evaporation, organic or otherwise inorganic "Uuren at a temperature about 15 ° C and JO ⁰ O provides that a pH value between • chea ^ and 2" adjusts itself between 4.5 and 3.5, then by heating the acidic coal. to temperatures of -

H92974

at least

L IL O 60 breaks the emulsion, "the two phases mechanically, eg by decantation, centrifugation or öchwingßiebung, separated and then the phosphatide phase in a vacuum at temperatures not higher than 60 ⁰ C evaporating ·

Instead of lecithin glue you can also use the already thickened lecithin go out »if you have this before the acid treatment dispersed in the same or a larger area.

For the execution of the procedure we prefer low molecular weight organic acids, such as Λαοίαen-, Acetic, lactic and citric acids, which are best added to the lecithin dispersion in a 10M solution volatile, e.g. formic and acetic acid, have the advantage • any excess of the same when evaporating the lecithin preparation at the same time »it is removed by the vapor ·

The process is applicable to all plant phosphatides, as s.B · on those in! soybean oil, peanut oil, rubol and Sunflower oil

The end products of the process not only have a considerably improved smelling effect for oil-in-water emulsions than the untreated lecithin, but are also milder in taste with weak organic _{> vc} bases, ζ · Β · Xthanolamines, adjusts to the original pH value of 6 to 7

The vegetable lecithins produced by this process, in !! tight of. 1 to 10% of vegetable or animal fats added to increase the ability of the latter to emulsify. They are generally used as emulsifiers for

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Oil-in-water emulsions are very suitable, e.g. Feed fats, Baokfβtteν mayonnaise and mayonnaise-like products « They give such products a high emulsion stability

Ee was already known, phosphatides or oily Phosphatide mixture after dispersing in water with small amounts of water-soluble acids e.g. mineral acids, such as hydrochloric acid, sulfuric acid, phosphoric acid or glycerol phosphoric acid to be treated at a pH-ülfert between 4.0 and 1.8 and then to be dried. However, the dried phosphatides treated in this way showed a lower level Emulsifying power than the non-acid-treated phosphatides

The difference between the process according to the application the known working method is that, according to the invention, following the acid treatment, not only the water, but also most of the water-soluble accompanying substances of the lecithin are removed

Furthermore, to obtain relatively pure phosphatides, raw vegetable oils are initially used with precipitants such as alum or Tannic acid with the addition of alkali in dilute, approximately treated with a neutral solution to precipitate proteins. After removing the precipitated proteins, the oil became the Phosphatide with acidic, aqueous solution with a pH of about 2 to 6 like «

The process according to the application differs from this, however, in that an acid treatment is not carried out on the Eohöl but rather phosphatide slimes obtained by treating potash with water, which have a completely different composition «

It is also prepared by extracting vegetable flours or fish eggs with methyl alcohol, ethyl alcohol, ether or chlorohydrin obtained by precipitation old

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thinned cures lecithin cowonnen, on the other hand it is eioh with the registration process according to a p: an other Starting material, which also results from the fact that the The lecithin obtained there is soluble in Vaseor, in the Gogen-0ats see below the phosphatides of the molding process

Poicniol 1

200 g oojalocithinschleira consisting of 55 above water, 30; y Phosphatidon and 15% 01, 200 g of AIT were V.aseor vorrührt at 20 ⁰ C and then with 5.0 ml of 10 vorootst, iicer formic acid, whereby the pH of 6.4 has been reduced to 4.0. Ban has the Uiechung at 60 ⁰ C or \ 7? 4nnt, 1/2 hour boi corührt this temperature and then by centrifugation in an aqueous, sugar and acid-containing extract and a residue phosphatidhaltigen decomposed · latter v / urde in vacuo at 7O ⁰ C evaporated

Yield ι 33.5 β cinea Ihöophatid-Cl-Gemiecliee with a phosphatide content of 67 »4 } **

The emulsification of this product was determined in the following manner checked!

A solution of 1 ß the Präparatee in 9 ß one on & chmelepunkt JO ⁰ C cured Erdnußweichfettes was dissolved in a 100-al-liiechssylinder GQgoken in which 50 ml "/ ater were of 50 ⁰ C · The cylinder was capped and then within x 20 seconds 20 times pivoted with the iiand 180 ° the cylinder was then zun'ichct in a iV'aaserbnd of 50 ⁰ C and spiiter in an oven of the temperature detected and the time eleichon bostinurit in which 2 ^ al water had deposited "

DieHe half-life however, was only 1 to 2 minutes at Verv.-onduns dos v / ie prepared as described above preparation 775 hours, using a ten from non iure with &> treated Cchleim Üojaleoithine.

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Bfiupiel 2

In an analogous Weico as in Example 1, oojalocitixinechleim was baw with dilute acetic acid. "'Ilchaliuro to a pli-.Vert of 4.0 an ^ oßäuort and then, after separation of ^{the acidic water, evaporated at 70 0} C in a vacuum.

The determination of the half-life zoite under the same conditions as in Example 1 gave the following values

Acetic acid! 390 hours Lactic acid 400 hours

Example 3

200 Q oojalecithinachleim, zusoEuaensotsatzt as in ßoispiel 1, with a PLL Ivert of 6.5? .Urdcn at 20 ⁰ C with 10 pointer formic acid until a pH-v »4 ort acidified and then heated to 60 ⁰ C, After dom Brochon dor L & ulsion .vurde most of dos sugar and bitterstoffhaltißen Sauorwasaera separated by centrifugation and dor rest of the water removed by evaporation in vacuo at 70 ⁰ C.

In an otherwise identical experiment, the end product was mixed with as much lionoethanolamine before the remaining V.'assors was evaporated added that a pH of 6.5 resulted.

The bulging behavior of both preparations was determined according to the method given in Example 1. Lie ilalbwertzcit for the non-neutralized product was? ÜO hours, for the Q * neutralized with ethanolamine> Q hours

example

To clarify the procedure in accordance with the charge, go to known state of the art, as can be seen from dom UG-Iatent 2,391,462, the following comparisons were made executed

J · 200 g jojalecithin gruel, set with susazame similar to

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• -6-

in Example 1, having a pK of 6.4 were v.'ert according dor Voruchrift of said U - ^ - Patents "at 20 ⁰ C with so much 10Me; he added formic acid that screen, a pE of v.ert 4.0 or 5.5 and then freed from '.7aaaer by evaporation in vacuo at 70 ° C

Furthermore, according to the procedure of the application, 2CO g of desaelbon So ^ aleclthinschlolms were acidified at 20 ⁰ C with 10 ', ClQQr formic acid up to a pK -'. Vert of 4.0 or 5 * 5, whereupon the mixture was 1 / Heated for 2 hours to 60 C, most of the sour water containing sugar and leaves was separated off by centrifugation and the rest of the water was removed ^{in vacuo at 70 0 O.}

When testing the preparations obtained in the emulsification test according to Example 1, the following half-lives were observed:

pIl-iYtrt. 4.0 5.5

Half-lives, £ td

a) Preparations according to

U.S.P. 2,591,462 <r 0.01 <-: 0.015

b) preparations according to
the registration

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Claims (1)

492974 Claim Process for the production of a plant phosphatide which is particularly suitable as an emulsifier for oil-in-water emulsions, characterized in that the phosphatide mixture obtained by hydration of crude extracted vegetable oils at a ^{temperature between about 15 0} C and 30 ⁰ O is diluted with such values · or weak inorganic acid is added that a pH value of from 2 to 5, preferably from 3.5 to 4.5 is established, after which the hereby formed i & nulsion is broken by heating to temperatures of at least 60 ⁰ C, the acid-containing phase mechanically separated from the phosphatide-containing phase and finally the phosphatide-containing phase is evaporated ^{in vacuo at temperatures not above 80 ° C.} 909810/0600 BAD OfllGlNAL