DE1467499A1 - Process for the extraction of oil from vegetable matter - Google Patents

Description

John Charles Oavanagh December 1st ^ e

Raymont Arthur öouohe
Adelaide "! Terrace
Perth / Western Australia

Process for extracting oil from vegetable matter

The invention relates to a method for extracting oil from vegetable matter, the vegetable matter a multi-stage extraction with the aid of a countercurrent, hydrophilic, organic solvent or be subjected to such a solvent mixture. The process is aimed at extracting vegetable matter such as rice bran, soybeans, peanuts, maize (grain) To obtain germs, coconut meat and the like. Oil and / or to produce improved protein-containing substances from them.

Usually the oil is obtained by pressing the vegetable matter and / or by extraction with a solvent won. Due to the relatively low oil content of some substances, the oil yield in the pressing process is 1 comparatively low, especially since certain amounts of oil remain in the pores of the vegetable matter when pressed and cannot be detected. In order to obtain a higher oil yield, an extraction must therefore be carried out with the aid a solvent can be made. Used for vegetable raw materials with a low oil content, such as rice bran and soybeans require extraction with the aid of a solvent anyway, so it will be pressed.

VI _ 2

809902 / 07.8

waived and the oil is obtained exclusively by extraction using a solvent.

A petroleum hydrocarbon, such as e.g. Hexane, is used. The extraction is generally carried out in devices that use the countercurrent process work. The commonly used hydrocarbon solvents are only used to extract the oil and otherwise have no appreciable influence on the substances subjected to extraction. The resulting from the procedure, Flour product freed from the oil therefore essentially corresponds to the starting product} an improved or a product that has been remunerated in any way is therefore not obtained with this method of operation.

The invention is based on the object of creating an improved extraction method with which a According to ind, the resulting oil yields high oil yields Substances have improved properties.

According to the invention, in an extraction process the aforementioned type of Y / as water content of the extraction liquid set in the first stage so that in In this first stage the material subjected to extraction comes into contact with a mixture of the solvent and a substantial amount of water, and that in subsequent stages the material is in contact with the solvent is located, which contains increasingly less water, the amount of solvent and water and the number of stages can be set so that in the first stage only a minimal amount of oil differs from the

- 3 -

809902/0780 _BAD original

Separating extraction liquid as a separate phase and that essentially no oil separates in a separate phase in at least the last extraction treatment. The oil which is separated off in a separate phase in the remaining stages is transferred from one stage to the next on the way of the extraction liquid severed.

The extraction treatment of the vegetable matter is carried out with the help of a special solvent, preferably in a greater number of stages are carried out through which the solvent is countercurrent to that subjected to the extraction Material is passed through. The material subjected to the extraction is accordingly fed to the first treatment stage and finally from the last treatment stage discharged while fresh, i.e. new or pure! solvent of the last treatment β stage is added and is discharged from the first treatment stage. Each stage consists of a container in which the material is in contact is stirred with the solvent and then again substantially by the solvent is released. Centrifugal force is particularly suitable for separating the extraction liquid from the extraction material working decanters or a countercurrent washing filter. In general, it is best to work in the two to use the decanter in the first extraction stages and the filter in the remaining stages. on the other hand however, a decanter can also be provided for all stages of the process. The separated Solvent is returned to the tank of the previous (lower atomic number) stage, while the extraction material to the container of the following

809902/0780

H67499

(in the ordinal number, higher) level is fed. Before the extract! Ons liquid reaches the container of the previous stage, any oil is separated, which is present as a separate phase in the extraction liquid. The separated oil can then be fed to separate storage containers or else poured together to form a product depending on the oil quality of the various stages and the economic conditions of the process. The material leaving the last treatment stage is freed from the oil after the solvent has been removed this creates a flour-like product. The solvent leaving the first stage of the process, i.e. the Extraction liquid resulting from the whole process can, in addition to some other components, still contain some oil in solution contain. The procedure can be found in the flow diagram shown in the drawing.

In the method according to the invention, a hydrophilic solvent such as acetone, or an essentially hydrophilic mixture of solvents, eg a mixture of ethyl alcohol, ethyl acetate and acetone or a mixture of ethyl alcohol, ethyl acetate and isopropyl ether is used. . When using mixtures of the geeignetesten for the respective use proportions of the various mix components can be readily gestures by experiments determined we "In the former mixture has a volume ratio of 1: 1 t 1 is particularly suitable, while in the second-mentioned mixture a volume ratio of 4- r 2: suitable. In contrast to other processes, the material subjected to the extraction is not subjected to the treatment in its normally dry state, but in the moist state. If dry material is used, which

809902/0780

has no self-sufficiency, then (before the actual Treatment) the material water in an amount of about 20 to 70 Grew .- #, based on the moistened material, added. On the other hand, the water can also be made of the material and. the solvent existing Mixture in the first treatment stage or to the the extraction liquid flowing into the first treatment stage can be added. It is essential that the solvent or the solvent mixture on the one hand be so strong is hydrophilic in that it is miscible with a substantial amount of water and that it is otherwise 3? Ett or oil in relatively pure form if it dissolves or it contains little or no water. In addition, the solvent or mixture should have a boiling point or have a boiling range that is lower than the boiling point of water.

That which is subjected to the countercurrent process according to the invention Material is therefore in contact with a mixture of solvent at the start of the extraction process and water, in which the proportion of water is relatively large and about 10 to 30 vol .- ^. In the course of the In a further process, the material comes into contact with a solvent, which is increasingly less water until it finally reaches the final stage of treatment in which it is in contact with new or pure solvent which has no or very little water * ser contains.

In the first and second process stage, the solubility of the oil in the solvent is due to the water content of the solvent, the oil is therefore in

809902/0780

These first stages not only go in solution with the solvent, but it "forms a separate phase that is either." sinks to the bottom of the solvent or floats on the solvent or in the form of in the solvent distributed droplets is present. In the case of the method according to the invention, this is carried out in a separate Phase present oil is separated from the extraction liquid after this has left the one stage and before it is then fed to the next (lower in the ordinal number) stage. The procedure is accordingly based on the Amount of water and solvent in relation to the oil content of the material and the number of stages so that there is only a minimal amount in the first stage separates the amount of oil in a separate phase. In the subsequent treatment stages in which the solvent contains increasingly less water, the solubility of the oil in the solvent is considerably greater, so that in this Effective oil extraction is taking place in the area. It is advisable to adjust the procedure so that at least there is no free oil in the last two stages. In this way, with the inventive Process achieved an extremely effective oil extraction.

The oil that was in solution in the solvent in the last extraction stages and then in the increasing Dilution of the solvent with water / water as it passes from stage to stage in countercurrent flow from the Solution that was driven out and formed a separate phase is relatively pure and is in a porm which is extremely desirable.

809902/0780

The oil present in the separate phase can in some or separated and recovered in all stages before the solvent is countercurrent to the next (in the level preceding the ordinal number. In general, most of the oil is obtained in stage 2} it becomes separated before the solvent enters stage 1. The solvent in stage 1 is therefore almost completely oil-free and contains about 10 to 30 vol .- #

Water.

Accordingly, level 1 has no oil extraction] function $ Their puncture consists primarily in removing substances that can be dissolved in aqueous solvents, such as sugar, rubber or Resin substances, pigments and other components which are soluble in the aqueous solvent to extract and to be discharged with the liquid leaving stage 1. These substances therefore remain in the process according to the invention do not return as impurities in the oil and also do not arrive with the oil passing through the individual stages Material in the farinaceous end product. A particular advantage is therefore that one and the same The countercurrent flow of solvent has an extraction function on the one hand and supplies a high-quality oil, on the other hand, however, the function of removing the other components from the material, such as Has sugar, gum, pigments.

With certain raw materials, a certain amount of oil is already used withdrawn from the raw material by the aqueous solvent in the first stage of the process. This is in this In some cases, the amount of oil that is unavoidable goes with the aqueous solvent into the outflowing extraction liquid. The aqueous solvent also has the

809902/0780

146749S

A tendency to dissolve part of the free fatty acid component of the oil contained in the material, which thus also goes into the outflowing extraction liquid. If necessary, the oil leaving with the extraction liquid can be recovered later. However, this oil is generally of inferior quality - it contains more free fatty acids than the oil separated off in the intermediate stages.

■ Those present in addition to the oil, from the aqueous "solvent Components removed in step 1 generally consist of polyose and taste and odor substances.

In certain cases, specific components, such as antitryptic digestive inhibitors (antitrypUo digestive inhibitor) and urease when using soy

\ beans, Gossypol when using cottonseed and JLflatoxin when using peanuts that are infected with cob mold (aepergillus flavus).

The liquid leaving the extraction process is treated so that any that is present in a separate phase oil comes to the separation. The phase on the surface of the liquid (i.e. the phase with lower

specific weight) consists of oil and small amounts of solvent, while settling at the bottom Pha'se (ie, the phase with a higher specific weight) of solvent / water with the dissolved low j herein components. It is generally found that the "free fatty acid" content of the oil is partly in the phase settling to the bottom and partly in the floating phase. The separated oil is accordingly partially refined and contains less free fatty acid than conventional crude oil. The two phases mentioned

809902/0780

are separated from each other by Sohwerkraft decanting or by spinning. The floating phase will then preferably in a vacuum extraction column, heated to remove the small amounts of solvent and to obtain the oil in a relatively pure form. The solvent is then reused. The ones on the ground The settling phase is a distillation, preferably a fractionation or a rectification treatment so that the solvent is distilled off and condensed for reuse, while the Water and usually in connection with a small amount of oil with a high content of free fatty acids remaining by-products as a residue. The oil mentioned corresponds to that oil which is in the the first stage was kept in solution at high water content in the solvent; it can be regained if this is desired for economic reasons. The aqueous residue can be concentrated by evaporation or subjected to some other treatment to recover the usable components contained therein.

The separated from the between every two stages of the extraction liquid oil can be added to the oil, which was separated from the outgoing extract ionsflüssigkeit and as mentioned above, freed of the solvent. Instead, the two amounts of oil produced can also remain separate from one another, with both amounts of oil being freed from the solvent and used as independent process products.

Some examples of the method according to the invention are explained below

- 10 -

809902/0780

Example I - rice bran

The extraction was carried out in an eight step countercurrent process in the manner described above The solvent was a mixture of 4 parts by volume of ethyl alcohol, 2 parts by volume of ethyl acetate and 1 part by volume Isopropyl ether used. On each 250 g of level 1 supplied hot bran was added about 500 g of water. In addition, level 1 was added for every 250 g Rice bran is supplied with an amount of 1.575 1 solvent level 8. In this example, some of the oil was in "free" state (i.e. as a separate phase) in which the. Stages 2 and 3 countercurrently flowing through solvent before. This oil was separated and the extract liquid draining off from step 1 (i.e. that from the overall process excreting liquid) added. This exiting liquid was described in the above Treated wisely.

Two batches of rice bran were used, i.e. a total of 500 g rice bran, with the following values determined became"

oil yield: 77 g

Free fatty acid content in the oil: $ 1.8>

Yield of flour product 299 g

Protein content of the flour product: $ 18.5

(Oleic acid)

(in bone-dry condition)

(Nitrogen times 6.5 of the bone-dry flour product)

Yield of by-products (without

oil) in the bone-dry state: 64 g of oil together with by-products: 6.5 g Content of free fatty acids in the

oil provided with the by-products: 23.0

809902 / Ö780

- 11 -

U67499

Part of the oil obtained in the above-mentioned example (ie the main amount of oil of 77 g excluding the oil containing the by-products) was stored in a glass container closed with a rubber stopper, the glass container being opened from time to time during the storage period of three months. No change in the color of the oil could be found here. In a comparative analysis, the value of $ 1.8 already determined during the production of the oil was obtained for the free fatty acid content. Even after a storage time of a further eleven months, the free fatty acid content remained unchanged at 1.8 Ji.

The flour product was practically deodorant and tasteless it was in a purified form. After three months of storage of the flour products in a screw top jar with polyvinyl insert, whereby the jar was opened frequently, 1 (LbB the flour product no change in appearance and also see no deterioration. After a further eleven months, no deterioration could be determined either will.

If the by-products are concentrated by evaporation to a mass of 65 Ji solids and 35 % water, the result is a dark brown syrup, the odor of which is very reminiscent of molasses (sweet-bitter odor).

Example II - soybeans

An eight-stage was used to extract the soybeans Used current system. The solvent consisted of a mixture of equal parts by volume of ethyl alcohol,

- 12-

809902/0780

Ethyl acetate and acetone. Lots of {4.50 g soybeans each were treated as follows:

300 g of water and stage 2 extraction liquid (900 g) were mixed with the added soybeans (450 g). DievJS.o jabohnen wjardjew; = ± ife dä & Bßjr ^ iösungsmit'tel-water mixture and then stirred for about five minutes * hot (50 ° 0). Then the solids were separated from the liquids. The solids containing approximately an equal percentage by weight of liquid were then treated in the subsequent stages of the GNöfeenetromsystem. The average temperature in each stage was 50 ° 0 plu
each level 5 minutes,

Level was 50 ° 0 plus minute 5 ° 0, the dwell time in

The liquid (extraction liquid of stage 1) contained about 30% by weight ->$> water and other components in solution. The solvent was recovered by distillation re ■>, while the other components (by-products) were concentrated to an aqueous extract. _Λ

After stage 3 and before stage 4, the solids were majfc ^ rjtal by means of a high speed circulating disintegrator (disintegrator) in the presence of the solution, -um ₁ ^^, d $ .§ ,, grg ^ en ^^ ilchen, to 'one size

Only 900 g of fresh solvent were added to the Solids of stage 7 added so that stage 8 er * ■ wu, rde. Water was only used in stage 1 of the system added. Because of the döi that occurs with the counter-flow

- 13 -

809902/0780

Η67499

The water content of the extraction liquid in stages 1 to 8 was about 30; $ 10 5.5 | 4.5; 4.1} 4.0 | 4, Oj 4.0? 6, the water content of the fresh Solvent was 4 #.

When operating the counter-current system, in that of levels I, *, 3 and 2 to levels 4, 3, 2 and 1 flowing solvent and in the extraction liquid leaving stage 1 the oil in a separate Phase on * After levels 5, 4, 3 and 2 it was then off the solvent carried out an intermediate separation of the oil, namely by the fact that the oil under the action settled under its gravity in the solvent and then withdrawn. The largest amount of oil was obtained from the solvent withdrawn from stage 4. Aue of the solvent withdrawn from stage 1 was the Oil is separated from the surface of the solvent by decanting (the solvent here has a greater water content and a correspondingly higher specific weight). The oil obtained from the intermediate stage solvents was added to the oil obtained from the solvent in stage 1, then the solvent was deposited by means of steam distillation and the oil was dried at 120.degree.

In order to achieve a mass balance between the supplied material and the supplied substances, this was the end. the countercurrent treatment of the last batch of soybeans' ^ duroh passed all stages, and distilled the entire \ liquid in order to determine the oil contained in it · Dae oil was separated from the solvent. dried at 120 ° 0 and added to the oil obtained during the countercurrent treatment. The total amount of oil recovered was 320 g with 2250 g of soybeans, which is a yield of

-U-

809902/0780

$ 14.2> equivalent to that of soybeans. The oil was of high quality, apparently resin free, and contained 0.22% of free fatty acid in the form of oleic acid.

The solid residue from Step 8 was obtained by heating in a forced-circulation air oven at 65 ° 0 and then Heating under vacuum (755 mm) at 65 ° C from the solution

from /

funds exempt. A total / 1470 g dry solids was won in this way. The solids were then screened into three screen classes, which were then separated have been subjected to an analysis for the crude protein and the residual oil. Here & sxsioh results in the following values:

Parliamentary group /
weight
(G) N χ 6.25 =
Crude protein + 44 hashes 78 21.6 -44 + 60
Bunny 141 46.0 - 60 hashes 1251 61.1

Peat oil

0.78

1.49 1.47

The analysis of the solids revealed that the antitryptic digestive inhibitor and urease, both substances normally found in soybean meal: were removed from the flour without the aid of a "roasting process" used to eliminate or render them harmless. The shell accordingly had a higher protein content, since heat damage to the proteins could be avoided. ^e

- 15 -

809902 / Ö780

The aqueous extract obtained after recovery of the solvent from the liquid of stage 1 was formed a thick yellowish emulsion. This emulsion was in hot and cold alcohol and in an excess of hexane solvable.

, 'Jt; ■ ■■■■.; ■ · -: ■ ■ · ... · ■ · · ■

Two products were obtained by dissolving in hexane, and

although '"" ■■ "' '■ ·, ■■ /

1 · a water-soluble material in an aqueous layer and> - '

2. a hexane-soluble material (most likely Resin fabrics and Leeithine) in a Hexansohicht.

These materials were recovered separately, leaving 217 g of solids in the aqueous extract and 16 g of resin solids (Gum) in the hexane extract.

All of the substances produced in this process were

Exploits

- 22 ^ 0 g soybeans 1 470 G Trooked solids 320 oil 217 Solids in the aqueous
extract 16 Solids in the hexane extract 243 Water content and Yersuohs-
losses (difference determination) 2 250 G

Since the normal water content of the soybeans was approximately $ 10, the water difference value used for the experiment was correct.

- 16 -

809902/0780

f * S »'· ■ ·. ■.' ■ '». ■

Example III - cottonseed

To extract the cottonseed kernels (meat) was an additional stage countercurrent solvent system is used. The solvent consisted of a mixture of ethyl alcohol, ethyl acetate and isopropyl ether in a volume ratio of 4 ι 2 t 1.

10 batches of 200 g of cottonseed each were as follows processed:

4-20 g of water were added to the cores, which were placed in a Centrifugal mills were ground so that they had a thin, creamy consistency. This amount of water was required to achieve an effective crushing jsu. The comminuted material was with 1,300 g of liquid the Level 2 mixed and stirred while hot (50 ° 0 + 5 °) | after solids and liquid were separated from one another with a stirring time of 5 minutes. The solids that approximated contained in the same proportion of liquid were then treated in the subsequent stages of the Q-co-flow system. The residence time of the substances in each stage was 5 minutes, the substances at the same time at a temperature of 50 ° ö + j> were stirred. The liquid (liquid of level 1) contained approximately 33 G-ew.-jt water and other components in solution. The solvent was recovered from the stage 1 liquid by distillation, the soluble Components have been thickened to an aqueous extract.

Between extraction stages 3 and 4 the solids were in the presence of the solvent by means of a

- 17 -

809902 / D7ßn

U67499

high speed rotating crusher crushes the coarse parts on one for oil extraction to bring more effective size.

Irish solvent was only added to the stage 7 solids in an amount of 1300 g, thereby level 8 was formed. The only water addition to the system was when the kernels were wet-ground before Mixing them with the liquid of stage 2 (whereby level 1 was formed). Due to the equilibrium established in the countercurrent, the Percentages of water in the total liquid in the order of levels 1 to 8 to about 33 | 10 | 5j 4,2j 4 »1 $ 4tO | 4, Oj 4.0, the fresh solvent being 4 wt .- # Contained water.

During the operation of the countercurrent system, this became separated in a separate phase in the stage 2 leaving solvent oil, so that this Solvent entered stage 1 in an oil-free state. The contact of the solvent with the in step 1 The cores present did not yield any extraction of the step leaving liquid therefore did not contain any oil in one separate phase. The oil separated from the liquid leaving stage 2 was steam distilled freed from the solvent and dried at a temperature of 120 ° 0 under vacuum (755 mm). The oil pointed "was light yellow in color and of excellent qualityj its free fatty acid (oleic acid) content was 0.34 #.

The total oil yield from 2000 g of seeds was 440 g. That at the end of the countercurrent treatment in the liquids of stages 2 to 8 in solution was not

809902/0780

won. Its amount was about 50 to 100 g.

The solid residues were removed by heating to 65 ° O in freed from the solvent in an oven operating with air circulation. From the amount of 2000g seeds a total of 1048 g of solids were obtained ^ these were sieved, whereby the following three products were obtained:

weight
(a) for the ur $ Protein
(η χ 6.25) Residue
Oil 0 140 Cores Pods and
Pasern 244 7.0 61.0 3.83 Middle product
(-30 + 100
Meshes) "Flour"
(-100 mesh) 664 12.2 69.5 0.52 33.2 1048 52.4

An analysis of the "flour" for free G-ossypol showed that this toxic component had been almost completely removed. A salary of only $ 0.005 was found.

The nitrogen solubility in 0.02 If sodium hydroxide according to the method Lyman, Ghang Cough (J. Nutrition 49, 679, 1953) was 81.3 ^ and was therefore higher than most usual cottonseed flours. This value leaves the good Recognize protein quality. The removal of the free Gossypol by dissolving (instead of chemical bonding with a Amino acid (lysine) also improves the quality of the protein flour compared to the products made in the usual way.

- 19 -

809902/0780

U67499

In the G-egenstroinsystem a special lot of 200 g treated, with the solids from each stage being examined for their residual oil content and for free gossypol the following values resulted

step oil content
(56 the dry
Solids) free
Gossypol (Jf) * 1 32.4 0.03 2 14.3 0.01 3 6.4 0.01 4th 2.3 0.01 5 1.2 0.01 6th 0.8 0.01 7th 0.7 0.01 θ 0.6 less than 0101

original kernels 0.84

These results show the high effectiveness of the process (ie the system working with an aqueous solvent) with regard to the removal of further components, such as the toxic g-ossypol, from the solid product as well as suitable for human consumption. When the oil yield from the extraction liquid of stage 2 was checked, it was found that the gossypol and colorants of the crude oil were practically completely removed. It was therefore not only the flour but also the oil resulting from the process of improved quality.

- 20 -

809902/0780

H67499

The aqueous extract, which arose on the recovery of the solvent from the liquid of step 1 was concentrated, whereby a thick "pitchy ¹¹ layer was separated during the concentration of the aqueous solution. This was separately from the aqueous concentrate is obtained, consisting mainly of Polyose and water-soluble dyes, with the following extracts

"pitch-like" material Polyose material

103 g H2 g.

The overall material balance was taken into account of the oil held in solution in the liquid of the final batch.

The following output was determined:

Solids 1048 G oil 444 β Extraktetoffβ (solid
total fabrics) 223 G 1715 β Not shown 285 β 2000 £

(Own water, loss of attempts, oil in solution)

Example IV - peanuts

The extraction of the peanut kernels was carried out in a two-stage process Grepenstromsyetem carried out. The solvent consisted of

809902/07 8 0

- 21 -

a mixture of ethyl alcohol, ethyl acetate and isopropyl ether in a volume ratio of 4 t 2 ι 1.

Four batches of 250 g cores were processed as follows »

520 g of water were added to each 250 g of kernels, the kernels being ground to a thin cream-like paste which had a total water content of $ 70. This slurry was mixed with 1620 g of liquid of stage 2 and stirred for five minutes while hot (50 ° C ~ 5 °), then the contaminants were separated from the liquid. The pesticides, which had approximately the same amount of liquid, were then treated further in the subsequent stages of the countercurrent system. The residence time in each stage of the system was five minutes, the substances being stirred at a temperature of 50 ° ± 5 ° 0. The liquid (lye of stage 1) contained approximately 33 # water and other components in solution as well as oil, which formed a separate phase. The liquor or liquid from stage 1 was distilled to recover the solvent. The oil and the other components were retained in the aqueous extract.

Between the extraction stages 3 and 4, the solid was comminuted in the presence of the solvent in order to make it suitable for to largely unlock the oil extraction.

A total of only 1620 grams of solvent was added to the entire system. The solvent became the solid Stage 5 fed, whereby stage 6 was formed. Water was only added to the kernels before they did entered level 1 of the system.

- 22 -

809902/0780

-22- H67499

At the countercurrent equilibrium that was established in the order of steps 1 to 6 for the water content in the lye or liquid are roughly the following Percentages! 33} 10; 5} 4.2} 4.1} 4.0, the fresh solvent containing 4 wt% water.

In stages 1 to 3 the oil separated into two phases off, but in level 3 only when it cools down. The oil separating from the cold stage 3 liquid was drawn off and combined with the oil from stage 2. Then the solvent was removed by steam distillation and the oil is then dried at 120 ° 0 under vacuum (755 mm). The resulting oil was almost as clear as water and contained $ 0.30 free fatty acid (oleic acid). The total oil yield was 401 g from a total of 1000 g of kernels. The amount of oil remaining in solution in the final liquor and not recovered can be estimated at perhaps up to 100 grams.

The solid residues were desolventized in an oven with circulating air at 65.degree. she were almost pure white in color, tasteless and odorless and suitable as protein food for people. That The total weight of the dry product was 379 g | this was sieved into three products, as can be seen in the following table

Protein oil content

I JjI X υ

Cj-ί oVjxxfO "ι * f * Q (rPWi Γ * lr \ " fc V

/ -η _q q \ / ν drier drier

⁽ '- ^ö * ^b * ^b * ^J ^ ^g; solid pesticide

13.5 68.7 22.9 68.6 342.6 70.9

+ 60 stitches

- 60 + 100 stitches

- 100 meshes 342.6 70.9 0.17

- 23 809902/0780

-23- H67499

From the aqueous extract, 97 g of concentrate in the form of a thick syrup was obtained, mainly 79 g of pesticides Contained polyose and flavor components.

The following material composition was determined!

Fixed products 379 g .Oil 401 g Extract solids 79 g rest 141 g

(Own water, oil in solution and experimental losses)

Since the intrinsic water content is between 4 and 7 f <> and the solution contains up to about 10 i » oil, the calculation works.

An additional extraction of peanut kernels was carried out at a rate of 4 parts / million aflatoxin B1 extremely toxic product of the piston mold (aspergillus flavus). A report by the "Tropical products Institute ", London, showed qualitatively low or negative aflatoxin values for the flour obtained and in quantitative terms values that were below 0.007 parts / million B1.

With the method according to the invention, a high quality oil can therefore be obtained at the same time Effectively remove the toxic components of the solids.

Example V - Corn (corn) germs

Corn (grain) germs were subjected to extraction in an eight-stage countercurrent system. The germs were in

- 24 -

809902/0780

brought a state that they had in iahlen wet "Au & they ie containing 50 to 53 $> water. A mixture of equal parts by volume of ethyl alcohol, Äthylaoetat and acetone was used as solvent.

Lots of 250 g of trooked germs each were prepared as follows processed »

The germs added with water (250 g) were 15 minutes kept under the action of the water for a long time, so that the moist germ almost regressed. You moistened Lot was mixed with 800 g of lye or liquid of stage 2 and in a rotating at high speed Son's oath (Waring Blendor) crushed. You mix was then stirred hot (50 ° C + 5 °) for five minutes | then the pesticide was separated from the liquid. That in a separate phase in the liquid The oil present (liquor of stage 1) was then separated off, the solvent liquor being separated out. Recovery of the solvent was not aimed at in the experiment, nor was it determined of the extracted components.

The solid was then treated further in the subsequent stages of the system. The normal extraction temperature was 50 ° 0 + 5 ° and the residence and etiour time in each Level five minutes.

Only Θ00 g of fresh solvent was used for the solid added to stage 7, whereby stage 8 was formed. The addition of water to the system consisted only of the water used to regress the troubled germs.

- 25 -

80990 / »/ η 7 ft Π

-25- -U67499

In practice, it will be advisable to remove the moist germs from the filter directly to the process. The oil equilibrium that was set in the oil flow brought about the The sequence of steps 1 to 8 approximates the following water content (in £) ι 35 | Hj 7J 5 J 4.3 * 4.1J 4.0} 4.0, the fresh solvent containing 4 wt .- ^ water.

In stages 1 to 7, the oil fell in a separate phase on (in stages 6 and 7 only when cooling down). When removing the oil from the liquid in stage 2, in stage 1, if at all, only a little oil is extracted or in a separate one Phase formed.

The resulting oil was by separating the oil phase from the aqueous solvent lye obtained in each stage. The oil was removed from the solvent by means of steam distillation freed and dried at 120 ° 0.

The following yield resulted from 1750 g of dry germs:

Oil 840 g

Pest residue 721 g

Heat 189 (inherent humidity, losses

and soluble components.)

The oil recovered was of high quality and an analysis "- of the shell yielded about 23% raw protein (S χ 6.25) with an oil content of around 3.6? 6. This high one The residual oil content shows that either before the extraction, the material is broken down considerably further by crushing it must be carried out or a renewed comminution carried out in an intermediate stage of the extraction must become.

- 26 -

809902/0780

The advantage of the method with the direct use of a moist vegetable material is that at the same time With the production of a high-quality oil, a dry flour is obtained, which is excellent as a protein substitute suitable. The oil obtained was obviously of a higher quality than that obtained with the previous processes Oil.

Example VI - Coconut Meat

"Coconut meat" means the moist meat of the coconut before it is dried to form copra. Its moisture content is about 50 fi and its oil content approximately 33 pounds.

To extract the fresh coconut meat, a eight-stage counterflow system used. The solvent consisted of a mixture of ethyl alcohol and ethyl acetate and isopropyl ether in a volume ratio of 4 ι 2: 1. Lots of 500 g each were processed as follows:

Coconut meat was shredded and mixed with 750 g of stage 2 liquor to form stage 1.

bi

This mixture was heated for five minutes / a temperature of

50 ° 0 + 5 ° stirred and it became the pestilence afterwards separated from the liquid. Some of the coconut oil formed a separate part in the stage 1 liquid Phase. The solid was then treated in subsequent stages of the system. The normal extraction temperature was 50 C + 5 and the residence and stirring time was 5 minutes.

- 27 -

809902/0780

-27- H67499

Between extraction stages 2 and 3, the solid became finely comminuted by means of a disintegrator running at high speed in the presence of the solvent ..

Fresh solvent was only used in an amount of 750 g of level 7 pesticides were added so that level 8 was obtained. No water was added to the system, since the natural coconut meat has about 50 # inherent moisture owns. The approximate water content (in Ji) in the liquids of levels Ϊ to 8 were öleiohgewioht 37 | 15 »8 | 5.5 | 4.4 | 4.2 | 4.1 | 4.0 #, where the; fresh solvents have a water content of 4 Grew .- ^ on- ' pointed.

The oil obtained in the separate phase in stages 1 to 4 (in stages 3 and 4 only when cooling) was removed from

the solvent lye is separated and so

won. The oil from all stages has been combined!

and by means of steam distillation from the solvent:

free and dried at a temperature of 120 ° C,

The solid product was dried in a circulating air oven at a temperature of 85 ° C. and then dried sieved into two products, namely over 100 hash and under 100 hash. The product under 100 hashes (Coconut wheat) was analyzed, whereby for the crude protein and residual oil content, the following values were obtained

Crude protein (Hx 6.25) = 35.1 Ji of dry

Test fabrics.

Bestöl * 0.30 Ji of the dry

Solid.

- 28 -

809902/0780

- ²⁸ - 'U67499

A total of eight lots were processed, the 7th lot for assessing the oil extraction and the 8th lot were divided into individual samples to determine the influence of the comminution. Game 8 was behind the Stage 2 is not shredded, but as chopped material as a whole through the individual process stages hindu led. In addition, 8 oil extraction samples were taken from the lot taken. The values determined for the application of the individual substances are therefore not true Indication of complete recovery. '■

In total, an amount of oil of 1,117 g was obtained, to which a further amount of oil of about 200 g must be added, which can be recovered from the solvent and was not extracted from the pesticide. The yield was therefore about 33 %. The oil was clear as water and of high quality. The free fatty acid (oleic acid) content was 0.09% and was of an acceptably improved quality with respect to the free fatty acid.

The total solids yield from the six lots was 385 g, which corresponds to a yield of 12.8%. 50 i »of which consisted of" flour "and 50 ° C. from a good over 100 mesh. The flour was tasteless, pure white, odorless and had a low paser content. It made one for all uses including human food suitable protein material.

The oil extraction observed in the last two batches indicated the need for fine grinding of the material. The following results were found here surrendered

. - 29 -

809907/078 (1

U67499

Lot 7th according to level 2
4th
6th
8th Lot 8th naoh level 4 ·
8th

Residual oil of the dry solid)

2.7 1.4

Residual oil of the dry solidsa)

19.8 9.0

After distilling off the solvent in the lye the aqueous extract remaining in stage 1 was concentrated to 168 g coconut syrup. This syrup contained polyose and other components. It had a pleasant scent of coconut.

The overall settlement was carried out taking into account the changes made during the Q-e overall process following list «

Solids 12.8 oil 33.0 Extract (estimated) 4.0 Self-moisture 50.0 Heat (difference value) 0.2

(dry solid)

This exemplary embodiment allows the method to be applied to a moist raw material and to the one that is established here Recognize the advantage of avoiding an!

- 30 -

809902/0780

-30- U67499

Example VII - Coffee grounds

"Coffee grounds" is to be understood as the moist solid residue that is present in the production of powder coffee after the extraction of the water-soluble coffee. The usual water content of the coffee grounds is $ 60 and the commercially available coffee grounds used in the following example had a water content of 62 fo . ■

The extraction of the coffee grounds was carried out in a six-stage Countercurrent process carried out. As a solvent was a mixture of ethyl alcohol, ethyl acetate and isopropyl ether in a VoIr ratio of 4 * 2 j 1 is used. Lots of TOO g each were processed as follows: '

The wet set was mixed with 1000 g of solvent from stage 2 mixed and for five minutes at a temperature of 50 ° 0 + 5 ° stirred. Then the solid was ^ " separated from the liquid. The solid that is about 'to? contained an equal amount of liquid, danii deri other Stages of the countercurrent system fed, in which he has five Was treated for minutes at a temperature of 50 ° 0 + 5 °. The liquid (lye from stage 1) was used recovery of the oil and other components in solution are retained. ■, .- ,. *.

No water was added to the system! the total water content therefore corresponds to the water content of the moist set. Fresh solvent was mixed in an amount of 1000 g only with the solid from stage 5, so that level 6 was formed. Der WassergetialV'dfer ^ Xäügen the Levels 1 to 6 were approximately 44} 16j 7.5j ί, Ί | 4V3j 4.1 #, the fresh solvent containing 4% by weight of water

- 31 -

809902/0780

-31- U67499

and the extraction system was in equilibrium.

After animal batches had been processed to achieve the equilibrium conditions, two batches were subjected to the procedure to determine the quantitative values. In stages 2 to 5 (in stage 5 only when cooling) the oil formed a separate phase, the oil content in stage 2 being extremely low and the main amount being separated off in stage 4. The oil was dark brown and had a faint coffee color. It contained 0.6 μl of free fatty acid (oleic acid) and was easy to separate out. The yield was 114.0 g, corresponding to 8.2 i "of the wet coffee grounds or 21.6 i" of the dry coffee grounds.

A hexane extraction of the liquor from stage 1 (before recovery of the solvent by distillation) produced a yield of 12.2 g of a waxy oil (which formed a solid wax at normal external temperatures of 20 to 25 ° C.). This wax was very dark brown to black in color and, like *, had a strong smell of burnt coffee. The Auebeute was 2.3 i "of the dry coffee grounds.

■ · '■ "" - ^: · ■' ■ · - 'from, The illation by the solution at the JLttel-Deat / the lye of the Stage 1 obtained aqueous extract contained 7.0 g of solid (dry) were obtained by evaporation of the aqueous extract 9.0 g of dry material were obtained. The amount of total solids extracted was therefore 16.0 g, respectively a yield of 3.0 Jt of dry coffee grounds.

The solid residue from stage 6 was obtained by heating

to a temperature of 65 ° fXI in a 6th en with Luftslrkula- j tion freed from the solvent. The total weight of the

809902/0780

dry residue was 391, corresponding to a yield of 73.5 1 ° of the dry coffee grounds. This residue was tasteless and had a protein content of 14 #.

The compilation resulted in the following values in detail

mission

1400 g moist coffee grounds = 532 drier

Coffee grounds

yield weight
(κ) Percent of dry
Coffee grounds oil 114.9 21.6 ■ wax 12.2 .- ,, - -. : .2, -3 · · ■■ - - Solids back,
was standing 391.0 .- ".-. 73,5, ..,.," Pest in
extract 16.0 ■■■■■ '■ "· ■ --'- 3, -O ■' ■ ' Yersuchs-
soh fluctuations . - 3.9,. 532.0 100.0

This example leaves the application of the invention Procedure to detect moist plant material which a slightly "refined oil is obtained. This can be done with the previously available procedures in which in the first stage of work, drying is carried out will not be achieved.

, ._:,: ..,. ...,.: .. .Seis.pie.1 VJII. -r.Re.iskleie. · ..- ■. _; ■

To compare the oil extraction, two rice bran proles, who have been in the open air for several weeks and therefore were greatly decomposed, an extraction treatment

- 33 -

809902/0780

üö ν

-33- 'U67499

"subjected, and" was the one in a conventional manner and the other by means of the method according to the invention, wherein. a mixture of ethyl alcohol, ethyl acetate and isopropyl ether was used as the solvent. It was there a four-step extraction process with hexane in comparison set au a seohsstufigen extraction with the mixture mentioned, since stages 1 and 2 of the invention Process cannot be described as actual oil extraction stages. There was no oil yield, only the residual oil content is determined in order to obtain an indication of the relative degree of extraction.

The hexane extraction was carried out in three batches in countercurrent with 600ml solvent and 250g rice bran each Stage carried out. The oil obtained had a free fatty acid content of 17.4 Ji (oleic acid). The one after the Extraction remaining oil content of the flour was 12.1 J * of dry flour weight.

The extraction according to the method of the invention was carried out with four batches of 250 g · The first stage consisted of 250 g rice bran, 200 g water and 675 al solvent-lye of stage 2 · Fresh solvent was used only fed to stage 6 in an amount of 675 ml. The oil obtained in a separate phase in the liquor from stages 2 to 4 was separated off. This UI contained 2.7 * free fatty acid (oleic acid). The remaining oil content of the dry flour was 2.2 liters.

This example clearly shows the advantages of the process according to the invention in the production of oil with low Free fatty acid content, i.e. a partially refined one Oil, recognize.

Claimsι

- 34 -

809902/0780

Claims (6)

-34- U67499 patent claims 1. A method for extracting O ^ from vegetable matter, the vegetable matter being subjected to a multi-stage extraction using a countercurrent hydrophilic organic solvent or a solvent mixture, characterized in that the water content of the extraction liquid is adjusted in the first stage that in this first stage the substances are in contact with a mixture of the solvent and a substantial amount of water, and that in the subsequent stages the substances are in contact with solvent, which contains increasingly less water, and that furthermore the amount _a n Solvent and water and the number of stages are set so that in the first stage only a minimal amount of oil separates from the extraction liquid as a separate phase and that essentially no oil separates in a separate phase in at least the last extraction treatment, the i n the remaining stages in a separate phase separating oil is separated from the extraction liquid on its way from one stage to the next. 2. The method according to claim 1, characterized in that the hydrophilic solvent acetone or a mixture of Is ethyl alcohol, ethyl acetate and isopropyl ether or a mixture of ethyl alcohol, ethyl acetate and acetone. - 35 - 809902/0780 - 35 - U67499 3. The method according to claim 2, characterized in that the hydrophilic solvent a mixture of ethyl alcohol, Ethyl acetate and isopropyl ether in a volume ratio from 4 ι 2: 1 is. 4. The method according to claim 2, characterized in that the hydrophilic solvent is a hybrid of ethyl alcohol, Äthylace.tat and acetone in a volume ratio of 1 ι 1 χ ΐ. 5 × The method according to any one of claims 1 to .4, characterized in that the water content of the first stage is adjusted by the addition of "water to the materials so that the WaBsergetiält; about 10 to 30 volume - $> the Gresamt extraction liquid. 'of the first level. 6. The method according to one of claims 1 to 4, characterized in that that the water content of the first stage by adding * vöii'Ifasö'er to that of the "second stage to the first ^ ufe ^^ lfln ^ ind-en Extractiönsfiussigk'eit is adjusted so that * the täs ^ seigeiiaTt approximately 10 to 30 vol .- ^ of the total The extra fluidity of the first stage is V. 7 · Method according to one of the preceding claims, characterized geicenÄzeicJme't, 'that the substances during the extraction of a second shredding. BATH ORIGINAL
80990 2/0780