DE2548916A1 - PROCESS FOR DECAFFEINIZATION OF VEGETABLE MATERIALS - Google Patents

Description

P «tu \ -. 49 \ Vi \ t

; DS MC nc r. ·.:. η 22 '"'

VV der.mayjrüruLs -13 O C / O O 1 C

Tel. (Ü C-) i.0 o, 2Ö Z D H 0 ι?

Societe des Produits Nestle S.A. in Vevey / SWITZERLAND

"Process for decaffeinating herbal products Materials"

The invention relates to the decaffeination of vegetable materials.

There has long been a need for the decaffeination of vegetable materials, especially those for the Manufacture of beverages such as coffee and tea. Ordinary decaffeination generally uses organic Solvents, such as trichlorethylene or chloroform, are used, which solvents either with the vegetable Material or an aqueous extract thereof are brought together. If there is a sufficient amount of caffeine in the solvent has been transferred, then the obtained caffeine solution is separated, so that a further treatment of the decaffeinated Material or extract is made possible.

609823/0630

These organic solvent based decaffeination techniques have some drawbacks. It is particularly important for the consumer that by using the previously used for decaffeination The solvents used often result in a loss or denaturation of valuable taste and flavor Aroma components of the drink to be produced later occurs. So the decaffeination had often result in products that are not of very high quality exhibited.

Since the solvents used up to now are themselves harmful, there were also concerns about to associate them with plant materials from which food products are made. These concerns have led to the development of complex and costly process technologies in order to achieve complete solvent separation from the finished products.

According to the invention there is now a method for the production of a decaffeinated vegetable material suggested which is carried out by mixing a liquid, what can be seen, with a caffeinated material vegetable material brings together this fatty material and the vegetable material during a sufficient period Keeps in contact time to convert caffeine from the vegetable matter to the fatty matter, and the resulting, caffeinated fat stuff of. the decaffeinated vegetable matter.

As used herein the term "fatty material" refers to any animal or vegetable fats or Oils or mixtures thereof, or fractions thereof, contained within

609823/0630

of the temperature range (to be discussed below) assume a liquid form suitable for the separation of Caffeine from caffeinated compositions is suitable. These bold materials usually exist consisting essentially of esters of fatty acids (usually glycerol esters) and can either be in their original form Form or in other forms resulting from conventional treatments known in the art. In addition, the fatty materials used should be considered for other components of the vegetable material Be caffeine nonsolvent.

For example, the fatty materials can be in the form of unsaturated or saturated fats or oils. Similarly, unrefined or conventionally refined oils, as well as oils with or without such customary additives, such as antioxidants and preservatives, in the process according to the invention be used. It is preferred, however, that the fatty material be substantially free of surfactants which can either be naturally present or added. These materials can be emulsions stabilize, which when stirring the liquid components that are used in the method according to the invention, and thus process stages such as separating through Can make centrifugation difficult.

The fats used in the fiction, contemporary method Materials include commercially available oils and greases. Numerous such oils and fats are commercially available. Of these materials, however, the edible ones are very preferred since such fatty materials are used do not pay particular attention to the separation of plant materials that are then used in food

6098 2 3

medium processed is required.

These fatty materials are capable of any desired degree of decaffeination of a vegetable To effect material. Although substantially complete removal of caffeine is usually preferred a lower degree of decaffeination can be achieved as required. In any case, however, will Receive an equivalent amount of caffeine as a valuable, tradable by-product.

The fatty materials are used to extract caffeine from a wide variety of plant materials, and most often from coffee or tea. However, in order for decaffeination to proceed easily, it is desirable that water is present. It is believed that this fact is because it is favorable is when the caffeine is initially in a water-solubilized or partially water-solubilized form, thereby facilitating access to the fatty material used as the decaffeinating solvent. The assumption such a mechanism in the method according to the invention however, is intended to be illustrative only and in no way restrict the scope of the invention,

Caffeinated herbal materials that are produced by the Process can be decaffeinated, suitably either in aqueous liquid or used in solid form. If a solid form is used then water should still be present, too when it is bound within the solid. Accordingly, so are aqueous solutions of plant materials, as well Plant materials with a considerable moisture content

content for decaffeination according to the invention is preferred .

Aqueous extracts of tea or roasted ground coffee are well known and can be prepared by methods conventional in the art. Since these extracts are later converted into beverage products, they should
usually be treated so as to minimize exposure to conditions that could result in loss and / or
Degradation of valuable flavor components as a result
can have. A special class of constituents in these beverages, the so-called volatile substances or aromatic substances, are particularly sensitive in this regard.

They are therefore preferred at the beginning of the procedure
separated and only at the end or near the end
the actual beverage production reunited with the more stable components.

This separation and preservation of the volatile or aromatic constituents of vegetable materials can be carried out by methods known per se in the art. For example, it is customary to steam off aqueous extracts, thereby obtaining an aqueous condensate which contains the aromatic and volatile constituents. These isolates are then kept under low temperature until they are re-combined with the components extracted from the plant material, for example
by mixing immediately before drying or adding to the dried material itself, with a second brief drying then following in the latter case. Accordingly, if aqueous extracts with fatty materials are decaffeinated, then the aqueous solution of the vegetable material is preferably free of its usual volatile constituents.

609823/0630

Another liquid vegetable material that can be decaffeinated by the method of the invention is from an aqueous extract of the vegetable material that is specially made for the purpose of decaffeination and does not form part of a later beverage product. This embodiment of the invention Process is particularly suitable for vegetable materials, such as coffee, which is normally roasted or otherwise must be treated to form many of the desired beverage ingredients.

For example, in this embodiment of the invention Method uses an aqueous extract of green coffee beans. Such beans can be extracted with water v / ground to remove its caffeine components. The resulting However, extract contains relatively little of the normal coffee beverage components, namely these water-soluble components are largely only formed during the subsequent roasting of the beans.

Making these extracts is pretty straightforward. All that is required is that the green beans be placed in contact with an amount by weight of water sufficient to dissolve the caffeine content. The beans typically contain 2 to 3 wt -.% Caffeine, depending on their origin, usually the dissolution is accomplished by a countercurrent flow of beans and water. However, this stage can also simply consist in slurrying the beans in water / water or an equivalent liquid, the contact time, usually 10 to 60 minutes, being sufficient to achieve the desired degree of decaffeination.

609823/0630

Even when green beans are extracted with water, some valuable beverage ingredients go into the watery one Phase. A technique by which a substantial loss of these desired components can be avoided, consists in using a closed circuit of the aqueous extraction medium. With this technique the aqueous medium rapidly takes the maximum concentration of the various water-soluble ingredients, including Caffeine, made from the green beans. During the subsequent selective separation of the caffeine from the medium, a recyclable aqueous extraction medium obtained, which in terms of those water-soluble constituents of green beans that are not decaffeinated by the Medium are removed, rapidly approaches the dynamic equilibrium.

Due to this dynamic equilibrium, the returned free extraction medium is released upon renewed contact having green coffee beans essentially just removes the caffeine from it. So it can be in a short time System in which only caffeine is separated from the green beans.

Both the circulatory extraction medium and the aqueous extract discussed in detail above are essential aqueous solutions containing both caffeine and various water-soluble 'constituents of vegetable materials contain. Accordingly, the inventive technique of treating the liquid vegetable materials with fatty Caffeine removal material can be applied to both in essentially the same manner. So becomes a liquid vegetable material mixed with a suitable volume of a liquid, water-immiscible fatty material,

609823/0 6J0

keep it in the mixture until the caffeine is in the fatty material has migrated, and then separated with a correspondingly reduced caffeine content. These Stages can be carried out fairly easily because of the fact that both phases are liquids are. This fact allows an easy and thorough mixing with stirring, while the immiscibility of the two Phases (aqueous and fat) an essentially complete separation by many known techniques, such as e.g. decanting, enables.

Of particular importance for the effectiveness of the decaffeination are the caffeine dissolving properties of the fatty material. These properties depend on each selected material and the temperature during mixing with the liquid vegetable material. This The effect can be based on the distribution coefficient for caffeine between equal volumes of fat and water Phase during mixing and at equilibrium. The affinity of fat material for caffeine a given temperature results from the following relationship:

Distribution coefficient - caffeine concentration in the fat phase distribution _coefficient - caffeine concentration in the aqueous phase

So higher distribution coefficients mean higher ones Ability to decaffeinate.

In the following Table I are exemplary data for various bold materials indicated at different temperatures. The data show the equilibrium that goes through simply mixing equal volumes of fatty material and aqueous caffeine solutions is obtained. It will care pointed out that the fat material used in each case only

3 / 0-6-9-6

represents a representative of commercially available products. So are depending on the history of a particular material expect certain changes in the partition coefficient. With these dates and with those in this description However, additional information provided may include the properties and the optimal conditions can easily be determined for the use of other fatty materials within the scope of the invention.

TABLE I Solubility Properties of Fatty Materials

fat material temperature

Safflower oil

Soybean oil

Corn oil

Peanut oil
Coffee oil

Triolein (oleic acid ester of glycerin)

olive oil
Pork fat

20 ⁰ C 10 ⁰ C

20 ^W C 10 ° C

20 ° C

15 ° C

10 ⁰ C

5 ° C

10 ° C 23 ° C

23 ° C 23 ° C 65 ⁰ C

Caffeine distribution coefficient with equal volumes of aqueous and fatty phases

0.064 0.067

0.064 0.059

0.064 0.064 0.071 0.085

0.067 0.140

0.085 0.076 0.197

609823/0630

The contact time between the fatty and vegetable phases is largely unimportant. It's only for a few minutes the approach to equilibrium is required. The optimal temperature for decaffeinating one however, certain fatty materials within the scope of the invention should be determined prior to use. Exemplary data are given in Table I, but further determinations can also be made by well known Techniques are carried out. The best temperature in the process according to the invention can be used after the selection of the fat material can be determined by a simple experiment.

When determining the optimal temperature, the choice of a particular material draws the limits of what is possible Variations after itself. So define the freezing point of the aqueous vegetable material and the solidification point of the fat material the lower limit for usable temperatures. There should be a breakdown at the other end of the range of the taste that can occur when the flavor and aroma components are exposed to higher temperatures get abandoned. Normally, however, the decaffeination can be done within a range of 0 to 50 ° C, with Aqueous extracts 10 to 30 C are preferred. If these components are negligibly absent, then even higher temperatures can reach the point of instability of the plant material concerned.

Once a specific fat material and temperature has been selected for the decaffeination stage are only left to consider the degree of decaffeination. This one will generally influenced at least in part by the ratio of vegetable matter to fatty matter.

609823/0630

usually a proportion of fatty material admits aqueous vegetable material of approximately 20: 1 only partially decaffeinated in a single contacting step. For example, with this ratio distribution coefficients of 0.035 and 0.085 result in decaffeination of about 40> i or $ 65 · An increase the ratio of fatty matter to vegetable matter naturally increases the degree of decaffeination and vice versa.

However, the device with which the contact with the rich material is carried out also influences the degree of decaffeination. As described above, decaffeination can be carried out using one-step decaffeination take place, whereby a certain weight of fatty material comes into contact with a certain weight of aqueous extract If these materials are kept in contact for a sufficient amount of time that the caffeine distribution equilibrium is reached, and then the extract is separated. The effectiveness of decaffeination can be however, aureh increasing the number of stages can be increased. Accordingly, in a preferred embodiment of the method according to the invention, the decaffeination is carried out in several stages, with the vegetable material contacted with successive servings of the fatty material until the desired degree of decaffeination has been achieved;

This preferred embodiment of the invention Method can be carried out simply by adding servings of the caffeinated composition certain fatty material contacted, the fatty phase and the aqueous phase for a sufficient time keeps in touch, thus making an essential transition of caffeine

609823/0630

in the fat material takes place (such a transition corresponds to usually more than $ 70 of the equilibrium distribution), the aqueous and the fatty phase are separated and then this sequence of steps with further servings of decaffeinated bold material repeated.

Yet another preferred embodiment of the invention Process includes countercurrent decaffeination. Here, an initially caffeine-free fatty material is used successive volumes of vegetable matter passed through it, the latter volumes being related to the caffeine content are arranged in reverse order. Fresh, fatty material first touches those volumes of plant material that is already the most decaffeinated and only then those with a higher caffeine content. If in this procedure the first Volume of the vegetable material has reached the desired degree of decaffeination then it is simply left out while creating a new volume that has the highest caffeine content connected downstream to a constant number of volumes in the stream and a correct order to maintain contact with the greasy material.

It is particularly pointed out that aqueous solutions or extracts of vegetable material, for example May contain 2 to 60 wt-i total soluble solids, Usually, however, it is preferred that the solutions to be decaffeinated contain a concentration of soluble Solids from 10 to 50? have before they start with the as a solvent for caffeine-acting fatty material. Such concentrations will be preferred so that the following liquid volumes, when decaffeinating, be kept small

and so the amount of water that is later removed by an extract when it dries into a solid form is small must become.

Concentration can be achieved by methods known per se in the art. Because the aqueous extract is to later release the dried beverage product, it is also preferred here that the concentration under conditions is achieved, which result in the least possible detrimental effect on the taste. Accordingly it is preferred to use techniques such as vacuum evaporation or freeze concentration in which the extract does not have to be exposed to higher temperatures for a long time.

The present invention also encompasses a method in which fatty material is used for direct decaffeination of solid vegetable materials is used. Examples of such pests are the green coffee beans can be used in ground, comminuted and preferably whole form. Can of roasted coffee beans can also be used. However, the volatiles should be removed first to avoid undue loss to avoid valuable beverage ingredients. Accordingly, the decaffeination of whole greens is done Beans most preferred. The following discussion of this embodiment is therefore particularly aimed at although, of course, other vegetable materials can be treated in a similar manner.

The use of solid vegetable materials represents a particularly preferred embodiment of the invention to the extent that certain disadvantages are avoided, which are associated with aqueous solutions of vegetable matter

609823/0630

rials are connected. Thus, the separation of the fatty material from the caffeinated composition is achieved facilitated by the fact that the fatty material remains liquid and the vegetable material in solid Form. The separation of the beans and the fatty material can be conveniently accomplished by simply draining the Beans can be achieved. If centrifugal forces are used to facilitate this separation, then a fairly simple machine could be used.

In addition, when separating the green coffee beans from a liquid fatty material, the degree of separation can be increased be close to 10C #. On the other hand, even the most sophisticated methods of separating immiscible liquids yield one certain retention of one liquid in the other; no such problem is encountered here. If once most of the fatty material has been separated from the beans, then allowing a second physical Cleaning stage, such as the passage of a steam jet through the beans, an essentially 100% separation of the retained fatty material. It however, even this additional step can be made unnecessary. Because of the done after decaffeination Roasting and extractive treatment of the beans will have little effect on the taste of what is later produced Beverage product even with an incomplete separation obtained if a substantially tasteless fatty material is used.

To make them easily accessible for decaffeination, the green coffee beans should contain some moisture. The beans usually naturally contain 8 to 10 wt. all moisture, although higher amounts of at least about 20 wt -.% loading

609823/0630

be preferred. However, the upper limit of moisture content is quite variable. Decaffeinating a caffeinated composition largely or entirely consists of green beans, is preferably carried out in the absence of free liquid water to help with Separation problems occurring in liquid mixtures and the possible loss of valuable components of the Avoid vegetable matter dissolved in this water. Accordingly, it is preferred in this embodiment of the method according to the invention that the Green beans contain between about 20 and 60 wt. 5t, preferably between about 40 and 60 wt. Ji, of water.

The incorporation of water into the green beans can be done easily. So can the beans simply immersed in water and kept in it for several hours until it has absorbed the desired moisture content to have. They can then easily be separated from the excess water, for example by centrifugation. By using heat and / or pressure, this incorporation or this "swelling" of the beans can be accelerated will. For example, if beans are soaked in water at a temperature of about 80 to 90 ° C, then they absorb the desired moisture content much faster. When using steam with about 2 at even less time, usually about 1 to 30 minutes, is sufficient to achieve the desired moisture content to achieve.

Once the beans are swollen to a suitable moisture level, then they are placed in or in a bath a stream of fatty material is introduced until the desired degree of decaffeination has been achieved. here the time of mixing is important because the

609823/0630

transition of caffeine from the beans takes place much more slowly than from a dilute solution. Accordingly, it is desirable that times of at least 30 minutes be provided for this stage with longer times for a more complete decaffeination required are.

In processes that result in a high degree of decaffeination, it is also important to ensure that the moisture content of the swollen beans does not drop significantly during treatment. Contact between swollen beans and fatty material can result in lower moisture levels due to a transition from water from the beans to the fatty material. If this decrease goes to a moisture content below the preferred range of 40 to 60% , then there is a corresponding decrease in the effectiveness of the decaffeination.

It is therefore preferred that the fatty material used for decaffeination contain a small amount of water. 0.9 to 1.2 wt .-% and in particular about 1 wt -.% Water, based on the fatty material commonly used in this preferred embodiment of the method according to the invention. This amount acts to maintain a balance between the amount of water in the beans and that in the fatty material, so that overall there is no migration of water from the beans into the fatty phase or vice versa. On the one hand, this prevents excessive removal of water from the beans and, on the other hand, it reduces the total amount of water that is present during decaffeination, thereby avoiding excessive losses of water-soluble components in the beans that are not caffeine.

609823/06 ^ * 6- ^

Here, too, a multi-stage process can be used in contrast to a single-stage contacting of the rich material be carried out with the vegetable material in the manner described above. So make a direct current and in particular countercurrent extraction with fatty material, particularly favorable features of a preferred embodiment of the method according to the invention.

One aspect in which the decaffeination of swollen Green beans are considerably different from the decaffeination of aqueous caffeinated solutions is in the Influence of temperature on the effectiveness of decaffeination, if during decaffeination there is contact with fat Material takes place with an aqueous caffeinated solution, then, as already stated above, have temperature differences no major influence on the effectiveness of the decaffeination during such contacting. In the However, treating firm beans will speed up the decaffeination process by increasing the temperature the caffeine separation increased enormously.

So, for maximum caffeine separation efficiency, decaffeination of the beans is preferred performed at as high a temperature as possible. A breakdown of the fatty materials usually occurs a temperature of about 150 ° C, which is why this temperature is usually a practical maximum limit for decaffeination. Longer contact times at very high temperatures can also be a factor result in certain degradation of flavor components. Accordingly, it is preferred that the decaffeination of green beans within a temperature range of approximately 50 to 120 ° C.

609823/0630

relates to another aspect of the present invention the regeneration of the caffeinated fatty material so that it can be reused in a decaffeination process can be. This regeneration is achieved in a very effective manner by removing what is separated Caffeinated fatty material contacted with water, a transition of the caffeine into the aqueous phase and allowed then separates the fatty material so that it can be used again for further decaffeination. The regeneration sequence is largely a reverse of the steps described above for decaffeination. In addition, however, it readily allows the caffeine to be isolated from the regenerated aqueous phase.

When the fatty material is regenerated, the effectiveness of the caffeine transfer to the aqueous phase is again increased by the same parameters of temperature, the caffeine distribution coefficient the material in question and the weight ratio of the fatty material to the water, as discussed above for the separation of the caffeine from an aqueous solution of the vegetable material became.

Since the breakdown of flavorings during the regeneration is not a problem, since components of the end product are not present, the temperature can be kept higher during the regeneration in order to improve the effectiveness of the caffeine transfer into the aqueous phase. If, for example, the solubility of the caffeine in water increases more rapidly with increasing temperature than in the fatty material, then it is advantageous to ^{carry out the regeneration at a temperature up to 100 °} C. (and even above if pressure is used to avoid evaporation). If against it

609823/0630

lower temperatures favor this transition, then these should be used.

Since it is desired here to convert ₃ caffeine from the rich material in an aqueous phase, the relatively greater solubility of caffeine in water allows the use of low proportions of fat to an aqueous phase, even for a substantially complete conversion. In addition, if it is desired to keep the amount of water used in regenerating the fatty material low, a multi-stage regeneration sequence comprising cocurrent or countercurrent extraction of the fatty material with water can be employed in the same manner as described above in order to make the regeneration of the fatty material more efficient.

When the fatty material was regenerated by removing caffeine with water, it was found that the separated Fatty material can contain about 1 wt. i £ of water, too when the separation of these immiscible liquids is carried out by such effective means as centrifugation will. This water is preferably removed from the fatty material before re-contacting with vegetable matter removed to avoid dilution of liquid vegetable materials. The removal of the im bold Trapped water material can be removed by such measures as relaxation of the ti'llati on under vacuum or equivalent known techniques can be performed.

As stated earlier, certain preferred embodiments are based of the method according to the invention for decaffeinating solid vegetable materials on the Using a greasy material that contains a small amount of • washer. In the practice of these embodiments

609823/0630

this dilution factor is negligible. Therefore can the regenerated fat material, which contains absorbed water, is used directly for further decaffeination will. Alternatively, the water content of the fatty material can be adjusted, for example by the fact that one adds water or that one carries out a partial stripping, depending on what to achieve an optimal Water content is required.

While it is desirable to have water in the fatty material, it is preferred to have the retained Remove water and then add the desired amount of water to the dry fatty material. This sequence of stages ensures an optimal water content and avoids the difficulties and / or interruptions necessary for the determination the water content in the regenerated fatty material and its adjustment are necessary.

The invention is illustrated in more detail by the following examples. Unless stated otherwise, the percentages relate to weight.

EXAMPLE 1

An aqueous extract of roasted ground coffee beans is steam stripped to remove volatiles. 10 kg of the stripped extract having a concentration of soluble Peststoffen of 19% and a temperature of 22 ⁰ C which are then added to 179 kg of maize oil with 60 ⁰ C. The resulting mixture is stirred for 30 minutes and then passed through a centrifugal separator at a rate of 3.16 kg / min. The liquid separated from the oil in the centrifuge shows a decaffeination

609823/06

degree of

By repeating this treatment with more corn oil, the degree of decaffeination can be increased successively be decreased until an essentially complete ^ Removal of the caffeine has been achieved.

EXAMPLE 2

A tea extract with a concentration of soluble solids of 27.6 / s and with a temperature of 22 ° C is used mixed with corn oil in a volume ratio of 1:20 and stirred for 10 min. The mixture then undergoes centrifugal separation was subjected to a tea extract showing 63 # decaffeination. Another treatment results in an even greater degree of caffeinization.

EXAMPLE 3

Green coffee beans are decaffeinated using a circulating aqueous medium that has reached an equilibrium soluble solids concentration of 29% and is at a temperature of 22 ° C. Decaffeination is carried out by passing the aqueous medium countercurrently through a column of green beans with substantially decaffeinated beans being removed from the column at one end and fresh green beans being added at the other end. Performed within the circulating aqueous system, and at a point outside of the column v / ith the aqueous medium by means of a centrifugal extractor, the coffee oil with ^ 0 ⁰ C is added in a ratio of 1:21 to caffeine from the aqueous extract to separate. In this system, heat exchangers are used to control the temperature

609823/0630

to keep these two liquids at the specified value.

One third of the caffeine in the medium can be removed with a single pass of medium and Cl through the centrifuge. A second pass of the I-iediura and another equal portion of oil increase the decaffeination of the medium to over 60 / °. After roasting, grinding and extracting separate samples of decaffeinated beans obtained after the first and second passes, both samples of aqueous extracts are found to be essentially caffeine free.

EXAMPLE H

Green coffee beans are exposed to steam at 110 ° C until they have a moisture content of k5% of the total weight. Samples of 10 kg are placed in separate extraction chambers. Each of the samples is decaffeinized for 4 hours at 95 ° C. with kaiso1, which is passed through the chambers at a rate of 1.1 kg / min.

In one experiment, labeled "A", oil is passed through only one chamber. Then it will regenerated by extraction with water to remove the caffeine content, whereupon the water is separated and the oil is returned to a continuous flow of a decaffeinated corn oil to maintain the swollen beans in the chamber.

On a second attempt, labeled "3", four chambers connected in series so that the corn oil flows through each. The regeneration and the return The oil will only be carried out after it has gone through all four

609823/0630

Through chambers. A chamber, namely into which the oil runs first, is separated after 1 hour and a new chamber is added at the downstream end. In this way and after a start-up period of 6 st Obtained a system in which the four chambers have beans with different caffeine content, due to the The fact that they were exposed to the inflowing decaffeinating oil for a different period of time.

The caffeine content of the beans from experiment "A" and from a chamber that follows all four stages of experiment "B" the start-up were analyzed. Despite the fact that each of these beans is under essentially decaffeinated under the same physical conditions the corresponding decaffeinations are noticeably different. While the attempt "A" beans are one Some decaf failures show that those of the attempt did "B" underwent a 92 $ decaf. It is therefore clear that a multi-stage extraction increases the degree of decaffeination significantly increased.

EXAMPLE 5

An aqueous extract of roasted ground coffee beans is steam stripped to remove volatiles. 200 g of the stripped extract, which has a soluble solids concentration of $ 18.4, are then mixed with 2 kg of safflower oil and stirred at 20 ° C. for 30 minutes. This mixture is then centrifuged to break the emulsion and then decanted. The separated extract shows a degree of decaffeination of 56%.

609823/0630

EXAMPLE 6

The procedure of Example 5 is repeated with the modification, that 2 kg of soybean oil is used in place of the safflower oil. The extract shows after separation a decaffeination level of $ 56.

EXAMPLE 7

The procedure of Example 5 is repeated using 2 kg of peanut oil in place of the safflower oil. In addition, throughout the process the extract and maintained at lu ° C and not at 20 ⁰ C 01 are. The separated extract shows a degree of decaffeination of $ 56.

EXAMPLE 8

Green coffee beans are mixed with coffee oil in a countercurrent extraction zone with four chambers decaffeinated in the manner described for experiment "B" in example 4. Every Chamber contains 6.6 kg of beans expressed as dry weight. The 01 is kept at 105 ° C and the extraction is carried out during a total extraction time of 6 hours (1.5 hours for each cycle). It becomes an overall oil / bean weight ratio of 120: 1 used.

After each passage of the circulated oil through all four chambers of the extraction zone, the oil becomes regenerated by aqueous extraction of the caffeine and then stripped to remove the water content. A predetermined one The volume of water / water is mixed into the oil before it is returned.

609823/0 6-313

Five different experiments are carried out using the above procedure. These attempts differ Essentially, adding varying amounts of water to the stripped, decaf, fatty material. The data for the continuous operating conditions of each experiment are as follows:

Try water in oil on no. salary rights rhal-

the Bohten water charge salary

Decaffeine loss type of

ation on feast
fabrics,
the no
caffeine
are Coffee beans 2.52 "MiIds"
1.33? caffeine 91% 1.1% It 91% ι, ΐί It 692 2.4 ^ "Robusta"
2.15% caffeine 91% 5.2% It

55%

555?

51%

0.37

1.00

1.00

0.75

1.20

These data indicate that proper moisture levels indicate optimal decaffeination with minimal loss other bean ingredients permitted. The effectiveness of decaffeination decreases when the concentration of the Water in the fatty material falls during decaffeination. It can also be seen that although the effectiveness of the Decaffeination remains higher with higher water contents in the fatty material, but that also higher contents of water result in an increased loss of non-caffeine solubles from the beans in the system.

60982 3/0630

Claims (1)

PATENT CLAIMS 1. A method for producing a decaffeinated vegetable material, characterized in that one is a liquid, what se immiscible, fatty material contacted with a caffeinated vegetable material, the fatty material and the vegetable Material keeps in contact sufficient time to convert caffeine from the vegetable material into the fatty material and the obtained caffeine-laden fatty material from the decaffeinated one separates plant material. 2. The method according to claim 1, characterized in that the caffeinated vegetable material consists of a aqueous extract of tea or roasted ground coffee. 3. The method according to claim 2, characterized in that prior to contacting the aqueous extract with the fatty Material volatile substances are separated from the extract. 4. The method according to claim 1, characterized in that the caffeinated vegetable material consists of an aqueous extract of green coffee beans. 53. The method according to claim 4, characterized in that the decaffeinated aqueous extract of green coffee beans following contact with the fatty one Material is returned for further contact with green coffee beans. 609823/0630 6. The method according to any one of claims 2 to _5} characterized in that the aqueous extract has a concentration of soluble Peststoffen from 2 to 60 wt -% has.. 7 · The method of claim 6, characterized in that ₃ the aqueous extract has a concentration of soluble solids content of 10 to 50 percent - has.%. δ. Process according to one of Claims 2 to 7, characterized in that the aqueous extract and the fatty material are brought into ^{contact at a temperature between 0 and 50 0} C and then kept at this temperature. 9 · Method according to claim 1, characterized in that £ the caffeinated plant material consists of green or roasted coffee beans. 10. The method according to claim 9 »characterized in that volatile substances before decaffeination of the roasted coffee beans are separated. 11. The method of claim 9 or 10, characterized in that the beans are swollen with water prior to contacting the beans with a rich material until they have a total moisture content of 20 to 60 wt -.% Have. 12. The method according to any one of claims 9 to 11, characterized characterized that the beans and the fatty material at a temperature between 30 and 150 ° C and then kept at this temperature. 609823/0630 13 · Method according to one of claims 9 to 12, characterized marked j that the for contacting the beans The fat material used has a moisture content which is substantially related to the moisture content the beans are in balance. 14. The method according to any one of the preceding claims, characterized in that the separated, with Caffeine-laden fatty material is contacted with water to make up essentially the total amount of it contained therein To transfer caffeine into the aqueous solution, the caffeine-laden aqueous solution from the fatty Material is separated and the decaffeinated fatty material for further contact with caffeinated plant material is recycled. 15. The method according to claim 14, characterized in that that> before recycling the decaffeinated fatty material, the moisture content of the fatty material to a Value is set, which essentially corresponds to the moisture content of the caffeinated vegetable matter is in balance. 16. The method according to any one of the preceding claims, characterized in that safflower oil, soybean oil, Corn oil, peanut oil, coffee oil, triolein or pork fat is used. 982 3 / 0-6 ^ 4