DE2627137A1 - METHOD OF TREATMENT OF CRUSHED OATS - Google Patents

Description

Patent attorneys: Dr, Ing.Walter Abltz Dr. Dieter S =. Morf Dr. Hans-Α. Browns

a Munich 88, Pienzanaae «ir. 28

June 16, 1976 DC-0109

DU POHT OF CAlTADA LIMITED Montreal, Canada

Method of treating crushed oats

The invention relates to a method for treating comminuted material Oats, with the help of which the crushed oats are separated into different fractions •will. In particular, the invention relates to such Treatment or work-up process in which the crushed Oats in a so-called "flour fraction", a so-called "bran fraction" and an oil as well as in secondary products, including an essentially rubber-free flour, separated will.

For the purposes of the invention, the term "groats" relate

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to the core of the oat, the term "flour" to the endosperm of the oat and the term "bran" to the oat bran to which endosperm may be bound as explained below. "Rubber materials"("gum") are to be understood as meaning, in particular, water-soluble rubber materials _o

A wide variety of valuable products are made from oats, such as flour, starch, protein isolate, protein-rich flour, Bran, gums and oil, extracted. The use of traditional grain processing methods. comes across in all of However, oats often encounter difficulties. This applies, for example, to grinding, because of the oil content procedural problems related to the oat arise. If the oats are not de-oiled before the grinding process, the conventional milling methods also yield oil-containing ones Flours and bran, which can then become rancid when stored.

The gums can be used together with etv / as protein and Starch can be partially removed by treating the oats with water. A dilute aqueous solution falls of rubber materials, which must be processed before disposal or for rubber production. The protein can be extracted from the crushed oats with aqueous solutions, especially alkaline solutions. Here you can however, any gums contained in oats also get into the extracts. The solutions obtained can be viscous and pose procedural problems, in particular with regard to the separation of the solids from the aqueous solutions.

The composition and properties of cereal grains The water-soluble rubbers obtained are manufactured by B.L. D'Appolonia described in a treatise which on the occasion of the 58th annual meeting of the American

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Association of Cereal Chemists. (November 1973) Symposium on "Industrial Uses of Cereals" was presented.

Canadian patent application no. 245 163 (submitted on February 4, 1976) describes a method for separating acid-soluble protein from crushed oats and methods for the production of starch, rubber materials and the like with the help of appropriate processes. Methods for separating oil from crushed material Oats are known and are also discussed in the aforementioned Canadian patent application. A procedure for the isolation of protein from powdered oil seeds with the help of liquid fluorocarbons is from the U.S. Patent 3,869,438 is known.

Process for the solvent-extractive milling of corn, Wheat, rye and sugar millet grains, with the bran removed from the whole kernel of these cereal grains and the whole, ground kernels are then comminuted, as well as for the separation of the cereal kernels mentioned Paser, protein, endosperm and / or starch fractions obtained are in CA-PSs 864 538, 905 909 and 905 910.

It was the object of the invention to provide a method for the treatment or processing of crushed oats (in particular for the production of flour and / or protein) to make available, which is less than the known method with due to the oil and gum content of the oats Is fraught with problems.

There has now been a method of separating a flour fraction, a bran fraction and oil from crushed oats found in which the rubber materials do not pose any significant procedural problems and which is an im

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provides essential guinini-free flour.

The subject matter of the invention is thus a method for separating an essentially rubber-free flour from Oats, which is characterized by "that one

(a) Crushed oats with an oat oil extraction from the oats "capable organic solvents mixed and

(b) A substantial amount of gum from the mixture of the crushed oats and the solvent Separates flour, v / whether the flour fraction separated from the mixture is at least 20% by weight of the crushed oats matters.

In a preferred embodiment of the method according to the invention, one starts from comminuted, peeled (peeled) Oats from.

In a further embodiment, the comminuted is mixed Oats and the solvent under controlled conditions which are capable of producing a non-uniform To effect distribution of the crushed oats in the solvent.

In yet another embodiment, the controlled conditions include discontinuing mixing immediately before separating the first fraction from the second fraction.

Another embodiment consists in that the solvent and the crushed oats are continuously and mixed under controlled conditions.

According to another embodiment, the comminuting

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th oats continuously to solvent and separates the rubber-free flour continuously from the mixture of the crushed Oats and the solvent.

The crushed oats used in the process according to the invention are preferably peeled or peeled oats. Methods for peeling or peeling oats are known. The hulled oats, often referred to here as "groats", are crushed in order to facilitate the extraction of oil and the separation of the crushed groats obtained into a flour fraction and a bran fraction. A useful crushed grits can be by conventional comminution methods, for example by grinding through a pin or Ha mm ermühle "by means of corrugating rolls or other shearing methods produce. Suitable grain sizes of the comminuted groats are given in the examples below.

The crushed groats are added to a solvent for the oil contained in the oats. The solvents used should be suitable for use with food (for example those remaining in the products Contained non-toxic), do not cause the formation of toxic substances in the product and the product's nutritional value not noticeably decrease. Furthermore, the solvents must be able to separate the flour and bran fractions to effect. The type and amount of solvent remaining in the products must be included comply with the relevant health regulations. Examples of suitable solvents are pentane, hexane, heptane, cyclohexane and alcohols having 1 to 4 carbon atoms as well as mixtures thereof; "Hexane" or "heptane" also apply in the context of the invention to those in the food industry solvents called "hexane" and "heptane", respectively. The preferred solvent is hexane. The invention

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is generalized below with regard to usage of hexane as a solvent and the separation of essentially rubber for a flour from crushed groats explained.

Before separating the crushed groats into the flour and the bran fraction can be useful »the solvent (hexane) and the crushed groats for a while Mix thoroughly to allow the extraction of the oil from the crushed groats (i.e. the de-oiling of the crushed Grits) to facilitate. Mixing is preferably carried out with stirring, "for example by creating a slurry the crushed groats and hexane.

According to the invention, the flour fraction can be separated from the bran fraction by several methods. At a discontinuous embodiment, the crushed groats and the hexane are used to extract the oil from the crushed Mix thoroughly for a while. The mixing process can then be regulated so that the The mixture of the crushed groats and the hexane is separated into a flour and a bran fraction »as follows is explained in more detail. On the other hand, you can also cancel the mixing process; in this Ealle inclines Bran fraction to a relatively rapid sedimentation, whereby a separation of the flour fraction from the bran fraction of the mixture is made possible. The flour fraction should be added as soon as practically possible after the mixing is stopped be separated because the flour contained therein also tends to sedimentation, whereby the separation of the bran fraction is made more difficult and / or its effectiveness is impaired. In the embodiment of the invention Procedure, which includes the termination of the mixing process, the above-mentioned sequence of steps is preferably one

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times or several times (for example by adding hexane and mixing again) with it high degree of separation of the crushed groats into flour and bran is achieved. Optionally, the mixture of the The crushed groats and the hexane are separated into the fractions by sieving. The clear mesh size of the used Sieves mainly depends on the desired degree of separation. A fine-meshed one is preferably used Sieve, for example one with a mesh size of about 48 μ (300 Tyler mesh) or less; the exemplary Use of a sieve with a mesh size of 44 μ (325 Tyler mesh) is described below. The bran fraction remaining on the sieve can be used as such or further comminuted as follows is explained. The clear mesh size of the sieve is preferably chosen so that the one passing through the sieve solid portion of the flour fraction is white and essentially bran-free.

According to a further embodiment, in particular in the case of continuous Execution of the process, the separation of the mixture of the crushed groats and the hexane by carefully controlling the mixing of the crushed groats with the hexane, especially immediately before and during the separation of the flour from the bran fraction. Such regulation of the mixing process is important for achieving a non-uniform distribution of the crushed groats in the hexane and the separation the crushed groats into the fractions. If mixed too effectively, a "uniform" mixture will form of the crushed groats and the hexane, and there is no in situ separation of the crushed groats into the Flour and bran fraction. The separation can, however, be carried out by part of the mixture of the comminuted Groats and hexane branches off, the flour fraction

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(e.g. with the help of a sieve) and the bran fraction is returned. If the density is insufficient, the distribution is the crushed groats in hexane non-uniform and the crushed groats tend to separate into fractions only if there is insufficient mixing between periods Periods with higher mixing intensity can be switched on.

It is possible to choose between the above-described states of uniform mixing and insufficient mixing Adjust the mixing process so that a non-uniform distribution of the crushed groats in the hexane is achieved continuously and in particular two fractions of crushed groats can be produced in the hexane. The first (usually above contained) fraction contains as the main solid component Flour. The second fraction (usually at the bottom) has bran as its main component. As follows is explained, you can regulate the mixing process so that the two fractions in terms of color and the general appearance - with the exception of near the interface between the two fractions - clearly from each other lift up. The two fractions can be separated from each other. One method of separation is the partial Separation of the flour fraction, subsequent addition of hexane to the remaining fractions and subsequent further fractions Separation of a flour fraction from the bran fraction, as described above with reference to the termination of the mixing process including embodiment has been explained. A preferred method of separation is that one of the mixture Hexane and crushed groats are continuously mixed with hexane and at the same time hexane and part of in particular the flour fraction removed. With the aid of the latter separation method, anything suspended in the bran fraction can be removed Separate the flour. It can be useful to separate the flour fraction from the bran fraction or afterwards to seven and any oversized grain for the purpose of another

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Treatment turn to slam the bran fraction. The bran fraction can also be separated. The in the invention Process separated bran fraction can consist of bran particles with adhering endosperm. To Separation of any hexane can further crush the bran fraction and either turn the mixture of crushed Oats and hexane are added or separated into a flour and a bran fraction for further separation Hexane mixed and separated into further flour and bran fractions. There can be bran fractions with different Endosperm content can be obtained.

The flour can be separated from a solution of the flour fraction by conventional methods for separating a pesticide to be isolated. The flour can be centrifuged off from the flour fraction, for example. Because the hexane dissolved oil it may be useful to clean the flour after separation by washing any adsorbed oil to free. The oil can be obtained from the oily hexane solution by separating off the hexane. The Bran can be obtained from the bran fraction by separating off any hexane contained in this fraction. at These processes, the hexane is preferably recovered and to separate the flour and bran fractions from the crushed groats reused. Optionally, the oily hexane solution can be at least partially used to separate the Flour and bran fractions from the crushed groats can be used.

Although the separation of the flour and bran fractions was generally described above as a one-step process, it can be carried out - possibly in a more effective manner - in several stages. For example, you can Separate the flour and bran in several steps. With such an approach, flour fractions, which flour

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-to,

with different protein contents, as well as separated bran fractions with different properties will. This can be beneficial for "certain end-uses.

The oil obtained in the process according to the invention can be obtained in cloudy form. It can then be useful to clean the oil. The oil can be cleaned by conventional methods or by mixing with isopropanol (especially _{isopropanol containing H 2} O ₂ ), stirring and separating (for example centrifuging off) any pesticides. As explained below, a clear, brown oil can be obtained. The solids retained by the centrifuge presumably contain considerable proportions of phospholipids and are suitable, for example, as emulsifiers.

The flour separated with the aid of the method according to the invention is essentially free of rubber and, moreover, virtually oil free. The gum and oil content of the flour are given below. Those contained in the bran fraction water-soluble gums can also be obtained. The obtained with the aid of the method according to the invention Products can be used either as such or as raw materials for other products in the food industry.

The main ingredients in flour are starch and protein. The flour can be classified according to air classification or air classification methods be separated into fractions with different starch and protein content. By extracting the flour with Protein and starch concentrates can be obtained from acidic or alkaline aqueous solutions. As in more detail below is explained, can be a high proportion of the contained in the flour Protein by slurrying the flour in such

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extract aqueous solutions. The pH of the aqueous Solutions "is in the EaIle alkaline solutions preferably at least 9> O (especially about 11.0) and, in the case of acidic solutions, preferably about 2.0. Examples of for Alkalis suitable for pH adjustment are sodium and potassium hydroxide. Examples of acids that can be used are phosphoric, hydrochloric and citric acids. As mentioned, they are in oats contained rubber materials (especially water-soluble rubber materials) by the method described above separated with the bran fraction, while the flour obtained is practically free of gum. The extraction of the protein from the flour can thus be carried out in the context of the process according to the invention at low solution viscosities, which is of great advantage in terms of process technology and, in particular, with regard to product separation. The solids contained in the solution obtained in the protein extraction can be isolated therefrom, for example by centrifugation. It can be useful washing or reslurrying the solids with water to separate adsorbed solubilized protein, and to isolate the solids again. The latter consist mainly of starch. When the strength is one If it contains a small amount of bran and the like, it can be useful, for example, by sieving, washing or air sifting clean.

The solubilized protein can - for example by isoelectric Precipitation - to be obtained. The solution of the solubilized Protein is treated with alkalis (e.g. sodium hydroxide) or acids (e.g. phosphoric acid) as required pH value of about 3.5 to 4 »5 adjusted. The protein precipitate can, for example, by centrifuging the solution be separated. The protein can also be obtained by freeze-drying the solubilized protein solution. This method is particularly suitable for isolating

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acid-soluble protein, especially from solutions "in the pH value »at which the protein should be soluble. the Properties of the protein including its color can vary from the method used to extract and separate the protein Protein. The protein obtained by extraction with alkalis or acids is probably in hot, acidic aqueous solutions stable. The acid-soluble protein obtainable from the flour in the tea described is To be preferred to the material available directly from the de-oiled groats. When the protein with another substance (e.g. flour) is to be mixed, it is preferably extracted from the flour with the help of an acidic solution and then freeze-dried, since the protein obtained in this way is whiter than that obtained by electrical precipitation is won.

The protein can also be extracted from the flour with the help of practically neutral aqueous solutions. One such Protein can be precipitated in hot water.

The products obtained according to the invention have a high economic value. The bran fraction can e.g. with or cline protein additive in pastries or as a filler for Meat products or animal feed are used. The flour is suitable as such or in protein-enriched form Form, e.g. for pastries or food for small children or as cake flour. The rubber materials can (e.g. with hot water) extracted from the bran and obtained as a binding or thickening agent for the food industry. The oil is suitable, for example, as a vegetable (edible) oil.

The following examples are intended to explain the invention in more detail without, however, restricting it.

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♦ 79-

Example 1_

Shelled Hinoat Oats (obtained from Agriculture Canada, Ottawa, Ontario) is made using a CASELLA grain mill ground (comminuted) using a sieve with circular openings of a diameter of 2.5 mm. 250 g of the The ground groats obtained are placed in a vertical cylinder 6.3 cm in diameter and height of 40.6 cm given. 600 ml of hexane are then added to the cylinder and the mixture is added over the course of 20 minutes at room temperature by stirring the consistency of a slurry. After you have stopped stirring, you lift it up The bran-free layer on top is removed. The process is repeated four times, adding 500 ml of hexane each time. The bran layer is then centrifuged to separate off the hexane and the bran fraction at room temperature dried in vacuo and weighed.

The hexane fractions are sieved through a sieve with a mesh size of 44 μ (325 Tyler mesh). The ones from Particles retained by the sieve are added to the bran fraction. Then the flour is centrifuged from the hexane solution. The oil is recovered from the solution by evaporating off the hexane.

The centrifuged flour is used to separate any adsorbed oil mixed with hexane to form a slurry and then centrifuged again and vacuum-dried. The white flour obtained has a very mild taste.

The bran obtained in the manner described above is reused in the CASELLA grain mill a sieve with circular openings with a diameter of 0.5 now ground. 112 g of the doubly ground bran are

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treated three times with hexane according to the procedure described above for the ground groats. The bran and flour fraction obtained in this way are dried. A 55 g sample of the bran fraction is wet-ground in a disc or puck mill and treated again with hexane. A bran and a flour fraction are obtained, which are dried.

The following results are achieved (all percentages relate to weight):

Sample weight, extract- protein- 3? Solid-

g th pro salary, keitsgedukt, % * fo ** halt, #

ground groats 20.5 9 »84"

First separation (250 g of ground grits treated)

Flour 89.6 35.8 20.5 9.38

Oil 12.3 4.9

Bran 149.5 59.8 22.3 8.46

Second! Separation (112 g of double-milled bran treated) Flour 28.7 25.6 19.6 12.29

Bran 82.9 74.0 7.31

Third separation (55 g of beater milled bran treated)

Flour 5.1 9.3 29.9 14.84

Bran 49.6 90.2

* The percentages relate to the weight of the treated Materials.

** Value obtained by Kjeldahl analysis for nitrogen times 6.25.

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This example shows that the protein content of the flour can be varied.

example

A sample of peeled Hinoat oats is made with the aid ground in an Alpine CONTRÄPLEX 250 CW pin mill. Because of the values obtained by grinding (with the aid of the pin mill) wheat are believed to be $ 90 of that obtained Pass the crushed groats through a sieve with a mesh size of 44 μ (325 Tyler mesh). 200 g of the crushed groats are placed in a column which has a height of 38.1 cm and a diameter of 6.3 cm and is arranged so that hexane is fed into their bottom and with the help of a near the Head located overflow can be deducted. The column is equipped with a stirrer, its blades are near the bottom of the column. 2000 ml of hexane are passed through the column within about 2 hours. During this period the stirrer is adjusted so that the mixture of crushed groats and hexane is about 7.7 cm below the overflow into a flour fraction and a bran fraction is separated.

The bran is separated from the hexane in the column and vacuum dried. The flour drawn off through the overflow with the hexane is centrifuged off from the hexane and dried. Tom Hexane the oil is then separated off.

The following results are achieved:

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3C-0109 Weight,
δ extract
tth product 2627137 sample 200 Protein-
, io salary, $ crushed gruel 128.0 64.0 23.9 Secret 62.7 31.4 28.75 bran 12.8 6.4 20.65 oil

Example 3

A sample of the husked Hinoat oats is prepared with the help of a CÄSBLLA granulator using a circular sieve Milled openings with a diameter of 2-5 mm. the Ground gruel is placed in the cylinder described in Example 2 and with it for 30 minutes at room temperature 600 ml of cyclohexane slurried. Then you hold the Stirrer on and lifts off the bran-free layer on top. This process is repeated three times, each time 500 ml of cyclohexane are added.

The flour fraction obtained from the upper, bran-free layer is passed through a sieve with a mesh size of 44 µ (325 lyler mesh) poured. Those retained by the sieve Particles are added to the class fraction. The bran, flour and oil are made according to the above Methods separated and dried.

The following results are achieved:

sample weight
G , extract
tes Pro
dukt, fo 16 - protein
salary t Damp
activity
salary, $> ground grits 250 783 20.5 9.8 Throat 73.4 29.4 17.4 5.2 bran 145.7 58.3 23.9 6.5 oil 14.5 5.8 - S09S53 / 0

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example

The procedure of Example 3 is repeated except that methanol is used as solvent instead of cyclohexane. The following results are achieved:

Sample weight, extract- protein- moisture-

g tes product, salary, keitsge- i "% holding, $>

ground grits 250 29.8 20.5 9.8 flour 74.5 58.1 19.0 9.4 bran 145.1 4.4 25.6 4.1 oil 11.1

A very white, odorless flour with a mild taste is obtained.

B ice ρ i e 1

A sample of peeled Hinoat oats is obtained using a CASELLA grain mill using a circular sieve Milled openings with a diameter of 2.5 mm. 500 g of the ground groats are then placed in a 2000 ml beaker mixed with 1000 ml of hexane. The mixture forming a slurry is then mixed with the aid of a mechanical Stirrer for 30 min. Mixed at room temperature. Then the stirring speed is reduced by the To effect separation of the mixture into a flour fraction and a bran fraction, and sucks the flour fraction through a sieve with a mesh size of 44 μ (325 Tylermesh). The portion retained by the sieve is returned to given the beaker. This process is repeated four times, adding 1000 ml of hexane each time. The flour will centrifuged from the extracted solution and dried.

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This gives 118 g _f 1 weii3es flour having a protein content of 20.3 ° i and mild taste.

20 g samples of the flour are then mixed in the form of a slurry for 30 minutes with 100 ml of distilled water. _{The pH of the water is adjusted to 11 f} 0, 9 »0, 2.6 or 1.5 either with sodium hydroxide solution or with phosphoric acid, as required. The slurry is then centrifuged. The supernatant liquid is separated off and the solid material for separating off the adsorbed protein in the form of a slurry is mixed with 100 ml of water for 30 minutes and centrifuged again. The solids (mainly starch) are dried. The supernatant liquid is combined with the one previously obtained and the pH of the solution obtained is adjusted to 4.5 either with sodium hydroxide solution or with phosphoric acid. The precipitated protein is centrifuged off from the solution and vacuum-dried.

The following results are achieved:

pH of the
solution

11.0
9.0
2.6
1.5

Starch, g

15.60 15.67 14.48 14.60

Protein content of starch, fo

0.93

7.4

3.2

1.7

Protein fraction,

4.10
2.74
3.30
4.16

Protein content of the protein fraction, #

89.5 38.4 90.8 83.7

All protein fractions are white; however, the fraction extracted with the acid solution is whiter than that which is obtained with the aid of the alkali solution.

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Example 6

The dried bran fraction from Example 5 is equipped with a crusher, reduction rollers and sieves Yersuchs wheat mill, which was constructed to simulate a technical wheat milling process. There are four fractions, i.e. Bran (bran), "coarse bran" (coarse shorts), fine shorts, and flour. There are no procedural problems whatsoever during the grinding process on. The flour obtained is white and has a mild taste.

The following results are obtained (based on frozen data on dry material):

Share (related

Sample genes on the protein,? S oil, fo raw ash, bran fraction), ^ fiber, fo%

bran 19.4 30.2 1.60 3.32 3.92 "Rough
bran ¹¹ 30.6 31.1 3.01 2.85 4.15 "Fine
bran ¹¹ 9.5 24.6 2.28 2.44 3.02 flour 19.8 15.4 1.07 0.70 1.23 Flour* 24.5 0.48 0.43 1.12

* To compare the results for the flour from Example 5.

example

174.3 g of obtained by extraction of Hinoat oats, cloudy and green oil for 15 min. with 500 ml 2-propanol mixed. The solution obtained is centrifuged and the clear, brown one at the top is decanted Layer. The 2-propanol is removed with the aid of a hot ion evaporator. The oil obtained (125.5 g) is clear and Brown.

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«5 * 0 *

Example 8

To show the distribution of the water-soluble gums in the products of Example 2? mixes are determined in each case 20 g of ground grits "flour and Eleie in the form of a slurry with 80 ml of distilled water" at 25 ⁰ C. Then "If the viscosity of the solution using a Brookfield Viskosimeters-, Model LVF, spindle no. 1 bei60Dpm ,

The following results are achieved:

Sample viscosity, gps *

ground jelly 400 flour 8th Eleie # * - Water*** 2.5

* As indicated on the viscometer.

** Cannot be determined due to the pasty nature of the solution.

*** Only water for comparison.

Example 9

De-hulled oats are added with the help of a 0ASELLA grain mill a sieve with circular openings with a diameter of 2.5 mm and then again in the same mill Ground using a 1mm sieve. 250 g of the ground groats are placed in a vertical cylinder of one diameter of 6.3 cm and a height of 40.6 cm. 600 ml of hexane are then poured into the cylinder and the mixture is stirred a slurry-forming mixture for 30 minutes at room temperature by. The stirring speed is then adjusted so that the slurry is divided into a flour fraction and

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separates a bran fraction. The flour fraction is siphoned off or. sucked off. Repeat the extraction process four times, adding 500 ml of hexane each time.

The bran is extracted from the bran fraction and dried. The flour is centrifuged from the flour fractions, again mixed in the form of a slurry with 500 ml of hexane, centrifuged from the hexane solution and dried. Oil is obtained from the hexane solutions.

The oil content of the ground groats, the flour and the Bran are determined by oxhlet extraction with hot hexane .

The following results are achieved:

Sample extracted oil content,

Product, * ground grits - 5.6 flour 43.0 0.08 oil 6.1 - bran 47.4 0.89

Example 10

Unhulled Hinoat-oats (groats) is crushed by means of a commercially available Ha m mermühle. 200 g of the ground oats are mixed in the form of a slurry for 30 minutes with 400 g of n-heptane (boiling point 97 to 98 ^° C.) and then sieved through a sieve with a mesh size of 44 μ (325 Tyler mesh). The sieve residue is again mixed thoroughly in the form of a slurry for 30 minutes with 400 g of n-heptane. The residue obtained on further sieving is in the form of a slurry during

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Mix with 400 g of n-heptane for 30 minutes, after which one again sifts. The resulting sieve residue (hereinafter referred to as "bran") is oven-dried overnight in a vacuum. The bran is pale yellow in color

t.

The portions that pass through the sieves during the individual sieving are combined and the mixture becomes centrifuged. The solution of n-heptane and oil is then decanted off. The solids obtained from the centrifuge are mixed with 200 g of n-heptane to remove any adsorbed oil in the form of a slurry. Thereafter It is centrifuged again and the n-heptane solution is decanted again from. The oil is obtained from the combined n-heptane / oil solutions by evaporating off the n-heptane with the aid of a rotary evaporator isolated. Then the oil is dried in the yakuai oven over night. It's green and cloudy.

The solid material obtained from the centrifuge (hereinafter referred to as "shell") is placed in a vacuum furnace over Haeht dried. It's colored white.

The protein content is determined according to Example 1. Thereby are achieved the following results:

Grits oil

Flour bran

Total yield 93 * 1

weight »G Share ("be
moved to the
Grits), $> Proteins
stop, $> , 4 200 19th - 15, 1 7.6 , 6 102, 2 51.1 18th 68, 8th 34.4 23

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Example 11

De-hulled Hinoat oats (groats) are crushed with the help of a BEUHLER laboratory rolling mill with corrugated rollers. The fractions obtained from the rolling mill are combined and have the following grain size distribution:

Grain size, mm wt. %>

(Tyler mesh)

> 1.68 (> 10) 5.0

> 1.41 (> 12) 7.2> 1.00 (> 16) 18.0

> 0.841 (> 20) 16.1> approx. 0.679 (> 25) 10.2 <approx. 0.679 (<25) 43.5

242.4 g of the crushed groats are in the form of a slurry during 30 mn. mixed with 484.8 g of hexane. Afterward the slurry is sieved through a sieve with a mesh size of 44 μ (325 Tyler mesh). Of the Sieve residue ("oversize grain") is mixed again as a slurry for 30 minutes with 484.8 g of hexane. The slurry is again sieved and the resulting sieve residue again in the form of a slurry during Mixed with 484.8 g of hexane for 30 min. The residue obtained from further sieving (hereinafter referred to as "bran" called) is washed with 200 ml of hexane and dried overnight in a vacuum oven. The bran obtained is pale yellow colored.

The fractions ("undersize") that pass through the respective sieve in all of the aforementioned sieves are combined and centrifuged. The solid material obtained from the centrifuge (hereinafter referred to as "flour ¹¹ ") is used to separate any adsorbed oil in the form of a slurry

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200 ml of hexane mixed. Then the flour is centrifuged off and dried over soft in a vacuum oven. The flour is very white in color.

From the solutions containing hexane and oil, which were decanted from the aforementioned centrifuged solutions, the oil is obtained with the help of a rotary evaporator. The oil is kept in the vacuum oven overnight. Ss is green in color and cloudy.

The residual oil content of the flour and bran fraction is through Determined Soxhlet extraction with hot hexane as the solvent .

The following results are achieved:

Proportion (weight, reduced to residual oil protein crushed content, content, te grits), # <fo fi *

crushed

Groats 242.4 18.3

Kehl 119.7 49.4 0.01 15.1

Bran 107.9 .44.5 1.66 24.2

Oil 14.7 6.1

With the help of an automatic Kjel-Poss analyzer certain total nitrogen χ 6? 25.

Example 12

A 25 g sample of the bran fraction obtained according to Example 11 is 40 min. At 50 ⁰ C with! Barrels extracted. The solution obtained is centrifuged, the aqueous solution is decanted from the solids and doubled

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809853/0783

Volume of methanol. The raw rubber substances precipitated as a result are centrifuged from the liquid and overnight dried in a vacuum oven. The amount of dried raw gums obtained based on the bran is 9.5 wt. #.

The procedure is repeated using the flour fraction from Example 11, using dried raw gums in an amount of 0.5 wt. ~ $, based on the flour. When separating crushed oats into one Bran, flour and oil fraction according to example 12, the gums thus remain mainly with the bran, during the flour is essentially gum-free.

Example 13

In order to show that further flour can be separated from the bran fraction of Example 12, the bran is again using a CASELLA grinder with a sieve ground circular openings with a diameter of 0.5 nm. 50 g of the regrinded material are in shape a slurry for 15 min. Mixed with 200 g of hexane. The slurry is then sieved through a sieve with a mesh size of 44 μ (325 Tylermesh) . The sieve residue is in the form of a slurry mixed with a further 200 g of hexane for 15 min. Then sieve again and dry the sieve residue (bran) overnight in a vacuum oven. The finer parts in the hexane are centrifuged and the pesticides (flour) separated and dried in a vacuum oven overnight. That The flour obtained is white, while the bran is pale yellow in color.

The following results are achieved:

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609853/0783

DC-0109 Afc

Share

Weight, g put on the protein bran fractured, tion), $>

Bran fraction 50.0 24.2

Flour 10.0 20.0 16.3

Bran 35.6 71.2 27.3

Example 14

A 20 g sample of a flour with a protein content of 11.3 $ vjizxL in the form of a slurry with 80 ml of distilled Mixing water «The suspension is then adjusted to a pH of 2Q with dilute hydrochloric acid, and the pH is maintained it for 30 min. at room temperature and then centrifuged it. The supernatant liquid is then decanted off and the solids are mixed again in Γ · οηα a slurry with 80 ml of distilled water, after which the pH is adjusted to 2.0. Centrifuged after 30 min the slurry and the supernatant liquid combined with that previously obtained. Then you put the obtained solution with dilute sodium hydroxide solution to a pH value of 4-5. The precipitated acid-soluble protein will separated and freeze-dried. The solids separated in the first two centrifugations (hereinafter referred to as "Starch") are dried in a vacuum oven.

The process is by means of aqueous hydrochloric acid at 50 ⁰ C and with the aid of phosphoric acid (instead of hydrochloric acid) at room temperature and repeated 50 ⁰ C.

The following results are achieved:

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DC-0109 attempt
1 * attempt
2 2627 137 salt
acid salt
acid attempt
3 attempt
4th acid Room temperature
temperature 50 ⁰ G phosphorus
acid phosphorus
acid temperature 20.0 20.0 Room temperature
temperature 50 ⁰ C Weight of flour, g 20.0 20.0 acid soluble pro
tein: 1.3 1.4 Weight, g 99.4 99.4 1.8 1.8 Protein content,% 93.3 94.9 Strength: 16.8 16.8 Weight, g 1.6 1.6 16.7 16.9 Protein content, fo 91 91 1.2 2.2 on the starting point
material (flour) related
good yield, $ & 93 94

Both the acid-soluble protein and the starch are distinctly white in color.

To show the solubility of the acid soluble protein, 1 g of the protein from Experiment 3 is added to 99 g of water which has been adjusted to a pH of 2.6. Huh After stirring for 30 minutes, all undissolved pests are centrifuged off from the solution. The supernatant liquid is separated and analyzed for protein content. The solution contains 0.93 # protein, from which it can be seen that 99.7 9 ^ of the protein in the acid-soluble protein has gone into solution are.

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609853/0783

20-0109

eis ρ i e 1

15th

40 g peeled, using a standard hammer mill Crushed Hinoat oats are stirred in the form of a slurry for 15 minutes with 160 g of 2-propanol. The received The mixture is sieved through a sieve with a mesh size of 44 μ (325 Tyler mesh). The sieve residue will mixed again in the form of a slurry for 15 minutes with a further 160 g of 2-propanol. Then you sieve again and mixes the sieve residue again for 15 minutes with 160 g of 2-propanol. The one obtained from a new sieving Residue (hereinafter referred to as "bran") is dried overnight in a vacuum oven Fractions passing through the respective sieve are combined and centrifuged. The solvent will decanted off and the solid material (flour) dried over night in a yakuum oven. From the decanted solvent oat oil is obtained with the help of a rotary evaporator. The oil is dried overnight in a vacuum oven.

The throat and bran are made with the help of an automatic Ejel Foss protein analyzer for protein content analyzed.

The following results are achieved:

product

flour

bran

Weight, g

21.85

11.66

3.40

Share (based on the

Starting material), fo

54.6 29.2

8.5

Protein content,

1 °

13.5 21.0

colour

White

pale yellow

yellow

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609853/0783

Example 1_6

The procedure of Example 8 is followed using the bran and flour obtained according to Example 15 were repeated. However, a # 2 spindle is used in the viscometer.

The following results are achieved:

Viscosity, cps

flour 15th bran * Water** 6.5

* Too viscous to measure.
** Only water for comparison.

Furthermore, the procedure using the flour and bran obtained in Example 10 is repeated .

The following results are achieved:

Sample viscosity, cps

Flour 27.5

Bran *

* Too viscous to measure.

Example 17

Shelled Scott oats, which have a protein content of 17.4% by weight, are made using a CASELLA grain mill with a sieve with circular openings of a diameter

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DC-0109 -Jo.

ground measrs of 1 mm. 50 g of the obtained groats will be in the form of a suspension for 15 minutes at room temperature mixed with 150 g of hexane. Then you can see them Slurry through a 44 micron mesh (325 Tyler mesh) screen and mix the screen residue again in the form of a slurry for 15 minutes with 150 g of hexane. After another show he will be there residue obtained again for 15 min. with 150 g Hexane mixed »which is again looked at. The pale yellow colored sieve residue (hereinafter referred to as "bran") is dried over! laughs in the yakuum oven.

The fraction ("undersize" *) of all of them passing through the sieve Sieves are pooled and centrifuged. The hexane / oil solution is decanted. The solid material obtained from the centrifuge is used to remove the adsorbed oil mixed in the form of a slurry with 150 g of hexane. then It is centrifuged again and the hexane solution is decanted again. The oil is made from the combined hexane / oil solutions by evaporating off the hexane using a rotary evaporator isolated and dried overnight in a yakuum oven. It is colored green and cloudy.

The solid material obtained from the centrifuge (hereinafter referred to as "flour") is placed in the yakuum oven overnight dried. It's colored white.

The flour and bran are analyzed using a leech-Foss protein analyzer on the protein content.

The following results are achieved:

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609 8 53/0783

DC-0109 -3 * 1.

Weight, g protein, $>

Bran 17.4 25.1

Flour 25.1 17.1

Oil 2.7

609853/0783

Claims (29)

DC-0109. &. PATENT CLAIMS Q) Method of separating an essentially rubber-free Oat flour, characterized in that one a) crushed oats mixed with an organic solvent, which is used to extract oat oil from the oats, and b) separating an essentially rubber-free flour from the mixture of the comminuted oats and the solvent, the flour fraction separated from the mixture making up at least 20 percent by weight of the comminuted oats. 2. The method according to claim 1, characterized in that the oats in step (a) before the separation of the Essentially rubber-free flour de-oiled. 3 · The method according to claim 2, characterized in that The crushed oats are crushed, hulled or peeled oats. 4. Process according to Claim 3, characterized in that the organic solvent used is pentane, hexane, heptane, Cyclohexane, an alcohol with 1 to 4 carbon atoms or a mixture thereof is used. 5. The method according to claim 4, characterized in that the separation of the gum-free flour from the mixture performs as a discontinuous process. 6. The method according to claim 4, characterized in that the separation of the rubber-free flour from the mixture as a continuous process. - 32 609853/0783 7. The method according to claim 1, 3 or 6, characterized in that the solvent used is pentane, hexane, Heptane, cyclohexane or a mixture thereof is used. 8. The method according to claim 6, characterized in that the gum-free flour is substantially free of bran. 9. The method according to claim 1 to 8, characterized in that in step (b) the mixture of the comminuted Separates oats and the solvent into at least two fractions, one fraction being bran as essential Proportion of the solid component and a second fraction essentially gum free flour as the primary contains solid component. 10. The method according to claim 9 _f, characterized in that the second fraction is substantially free of bran. 11. The method according to claim 10, characterized in that bran, gum-free flour and / or oat oil are separated wins in a substantially solvent-free form. 12. The method according to claim 11, characterized in that you win bran and this is further crushed and mixed again with solvent and another Separation into fractions makes which bran as an essential solid component or rubber-free flour included as the main solid component. 13. The method according to claim 9 to 12, characterized in that that the separation of the mixture of the crushed oats and the solvent by sieving the Mixture through a sieve, which holds back almost all of the bran and that containing the gum-free flour Lets solvent through, performs. - 33 609853/0783 14. The method according to claim 9, characterized in that the crushed oats and the solvent are mixed together under controlled conditions, whereby one the regulated conditions are chosen so that a non-uniform (uneven) distribution of the crushed Oats in the solvent is achieved. 15. The method according to claim 14, characterized in that the regulated conditions include an interruption of the mixing process immediately before the fractions are separated. 16. The method according to claim 15, characterized in that the mixture is immediately after the interruption of the Mixing process to facilitate the separation of the fractions incorporated additional solvent. 17. The method according to claim 14, characterized in that additional solvent is continuously incorporated into the mixture and the gum-free flour continuously separated from the mixture. 18. The method according to claim 14, characterized in that the bran is separated from the solvent, further crushed, chopped up, mixed again with solvent and mixed in an essentially gummy st off free flour as the main one fraction containing solid component and a further fraction separates. 19. The method according to claim 1,9 or 13, characterized in that crushed oats are used, which by processing peeled or peeled oats with the help of a pin or hammer mill or fluted rollers was obtained. 20. The method according to claim 1, 9 or 13, characterized in that the solvent used is hexane. - 34 609853/0783 3X3-0109 Ί 21. The method according to claim 1, 9, 12, 13 or 17, characterized characterized in that in an additional stage a protein-rich fraction of gum-free flour separates. 22. The method according to claim 1, 9 »13 or 14, characterized in that that in an additional step an acid-soluble protein fraction of gum-free flour separates 23. The method according to claim 9, characterized in that a starch fraction of Separate gum-free flour. 24. The method according to claim 9, 12, 13 or 14, characterized in that that in an additional stage the gums (gum) from the bran fraction or bran separates. 25. The method according to claim 22, characterized in that the separation of an acid-soluble protein fraction therein consists in mixing the rubber-free flour with an acidic aqueous solution, the undissolved solid substances separated from the aqueous solution and recovered the soluble protein from the solution. 26. The method according to claim 25, characterized in that the protein is removed from the solution by freeze drying wins. 27. The method according to claim 25, characterized in that the protein is obtained from the solution by isoelectric precipitation. 28. The method according to claim 26 or 27, characterized in that that the acidic aqueous solution is a dilute solution of hydrochloric and / or phosphoric acid. - 35 - 609853/0783 DC-0109 Ιό Ι ι id / 29. The method according to claim 24, characterized in that the rubber materials are separated from the bran in that this is mixed with water, the bran is separated from the water and the gums are extracted from the water. - 36 - B0S853 / 07R3