DE3435492A1 - METHOD AND DEVICE FOR PRODUCING AROMATIC RESINS AND OILS FROM HOP FLOUR - Google Patents

Description

Missing out and device

for the production of aromatic resins and oils

from hop flour

The invention relates to a method of mechanical Separation of a liquid concentrate of aromatic resins and oils from lupulin powder and a device for Carrying out the method and a product for use in brewing malt beverages.

It is well known that extracts from hops are used in the production of beer and ale to make these To give drinks their characteristic aroma and bitter taste. The substances to which this aroma and The taste is attributable to resins and essential oils contained in the lupulin glands (hereinafter simply referred to as "lupulin").

The brewing strength of hop substances for the production of Beer and ale is measured analytically and expressed as a percentage of the organic acids it contains, which as "Alpha acids" and are contained in the hops substance that is added to the wort.

Currently in the factory production of malt beverages Added strongest hop extract is a viscous, syrupy extract from lupulin that is obtained by solvent extraction is won. The extract obtained by solvent extraction or the concentrate obtained in this way contains up to 55% alpha acids, depending on the quality of the hops used and the type of extraction solvent.

Solvent extracts are also the most stable form of the hop product because they come in sealed metal cans stored, whereby the aroma-giving components are protected from oxidation.

Most solvent extracts contain a small amount of residual solvent, which some brewers do

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complain. Examples of such solvents are hexane and methylene dichloride. Carbon dioxide can be used as a solvent with no residue. However, extraction processes using carbon dioxide require very high pressure in order to generate and maintain the carbon dioxide in a liquid or fluid, gaseous state. Extraction using supercritical carbon dioxide requires the use of extractor vessels that can withstand pressures of 14 to 42 * 10 ⁶ Pa (2000 to 6000 psi-psig). Pumps and other ancillary equipment must also be provided with which to work under these extreme pressures. Consequently, the use of carbon dioxide as an extraction solvent requires a very high capital investment, even for a moderate output plant.

Lupulin is separated from hop cones in a variety of ways Way, which leads to different grades of lupulin powder or hop flour. A hop flour from high quality consists essentially of pure lupulin glands. Lower grades contain fibrous vegetable ' Substances of the broken scale leaves of the hop umbel. Examples of lupulin separation processes from hops can be found in U.S. Patents 2,833,652, 3,271,162, 3,390,000, 4,051,771, and 4,053,653. The alpha acid content of these processes obtained hop flour ranges from 15% to 37%. The method according to the invention can be used for different qualities of lupulin powder or hop flour, e.g. between 20% and 50% alpha acid.

In GB-PS 1 190 670 is a method for comminuting or Milling of hop flour into a paste composed of the resins and essential oils which are proposed has been proposed released by the mechanical crushing process. as well as from the cell material of the hop flour. Tests with this method have shown that it is only

is successful with high quality hop flour. The presence even small amounts of fibrous material made the resulting mixture too dry. If an essentially Pure hop flour with a high alpha acid content was used, a semi-fluid paste was created, which when heated too a free flowing liquid. However, if you used a hop flour of lesser quality with a low one Alpha acid content resulted in a dry product which was not fluid and not even when heated could be made fluid, because finely divided, fibrous, herbal substances were present.

The object of the invention is to provide a method for the mechanical separation of aroma resins and essential oils To create hop flour, which can be used just as well for the processing of good and bad quality hop flour leaves.

The object of the invention is also to create a device for carrying out the method.

With the invention a substantially pure concentrate is obtained in each case. Mechanical pressure is used to Crushing the walls of the lupulin glands is applied to free the resins and essential oils. Instead of the released resins and essential oils and the lupulin wall material To grind together, the liquids are separated from the solids with the method according to the invention separated. The fluidizable resins and essential oils are mechanically pressed out of the hop flour solids, while they are released from the cells, while all solids remain in the form of a press cake. All fibrous, possibly present in the hop flour, Vegetable substances remain in the press cake together with the cell wall material of the lupulin glands.

The method according to the invention provides essentially to first heat a lot of hop flour so much that the The resins contained in the lupulin glands melt. Pressure is then applied to the heated hop flour in order to create the aromatic resins and essential oils in the form of a viscous syrup or liquid that is essentially is free of cellular material. The pressure applied causes both the glands to burst, causing the Resins are released as well as the released resins and essential oils are squeezed out of the solids, so that the solids remain in the form of a press cake.

The viscous concentrate is pressed according to the invention through a wall which consists of a material which but not permeable to the concentrate for the solids that make up the press cake. This wall can be a sieve wall, the mesh openings of which are smaller than the intact lupulin glands, or a tissue wall with openings of similar size. If a sieve wall is provided, the hop flour is directly on the Sieve wall given and pressed, if a fabric wall is used, on the other hand, the hop flour is filled into a bag, which consists of the fabric, and this bag is pressed.

An important finding of the invention is that the press cake is processed further using solvents in order to extract the alpha acids remaining in the press cake in this way. The ones with the products produced by both processes are not mixed. Instead, the product of the mechanical separation process, which is free from solvent residues is sold to those consumers who have a solvent residue need free product. That obtained by treating the press cake with a solvent The product is sold to consumers who have a small amount of residual solvent in the product 5 is acceptable.

The following is the invention with further advantageous Details are explained in more detail using a schematically illustrated embodiment. In the drawings shows:

Figure 1 is a flow sheet of the primary process according to the invention and an optionally performed secondary Procedure;

2 shows an exploded view of a press for carrying out the method according to the invention; Fig. 3 is an enlarged vertical section through the press according to FIG. 2, in which a quantity or

Batch of hop meal is shown between a piston and a small mesh sieve; Fig. 4 is a view similar to Fig. 3, but in which the hop flour in a bag and the bag between the piston and a large mesh supporting screen for the bag is shown;

5 is an enlarged view of a bottom closure member for the press cylinder with grooves forming grooves in the top and a discharge opening to which the Drain from the grooves runs.

According to Fig. 1, the hop flour is from hop cones to any, known manner separated, for example by threshing. After that, the hop flour is raised to such a high temperature heated so that the resins contained in the lupulin glands melt. The heated hop flour is then put into a Press filled, the parts of which have been heated in advance so that they do not cool the resins. According to an alternative the lupulin is in the press together with the press in any way, for example by means of a heating jacket warmed up. Inside the press, the heated hop flour is pressed against a permeable wall that consists of a There is material having openings whose openings are smaller than intact lupulin glands. Sufficient pressure is then applied to both the

Walls of lupulin to break apart as well as the released ones Forcing resins and essential oils through the permeable wall and away from the solids. A concentrate is created which has the consistency of a viscous syrup or liquid and a high alpha acid content and is essentially free of solids.

The solids are pressed together in the press to form a press cake, which may contain so much more alpha acid that further processing by solvent extraction is possible worthwhile (referred to as an optional secondary procedure). When the press cake processed by treatment with a solvent, the resulting extract is not mixed with the concentrate mixed, which was obtained in the mechanical separation process. The one obtained by the mechanical separation Concentrate is sold where there is a need for a concentrate that does not contain an extraction solvent residue. The one by solvent extraction Extract obtained from the press cake, however, is sold where an extract is acceptable that is a low one Contains amount of a residue of the extraction solvent.

The main features of the press are that it can be used to apply sufficiently high pressure, to press the resins and essential oils out of the hop flour and at the same time the solid structural material of the Retain lupulin glands and other existing fibers. The most varied of industrially applicable ones are likely to be Presses are available, as the pressing of fats and oils and other vegetable substances, z. B. cocoa beans and other oleaginous seeds is a well known technique.

2 to 4 show a simple form of a press on which the method according to the invention has proven itself

Has. This press could be the basis for an industrially applicable press.

As Fig. 2 shows, the press has a cylinder 10, which delimits a chamber 12 inside. At the lower end of the chamber 12 is an end closure in the form of a plug 14 which can be inserted into the lower end of the cylinder 10. Through the top of the cylinder 10 is in the chamber 12 a piston 16 which has a piston head 18 at its lower end. The stopper is a fixed closure for the lower end of the chamber 12, and the piston head 18 is a movable closure for the top of the chamber 12.

The piston head 18 has a circumferential groove into which a sealing ring 24 is used to prevent leakage between the piston head 18 and the side wall of the cylinder 10 seals.

By way of example only, there may be a pattern of concentric V-shaped grooves or grooves in the top of the plug 14 20 be formed. The ones that remained between these grooves 20 Edges are relatively wide compared to the width of the grooves 20. The concentric grooves 20 are of three radial grooves or channels 21 are cut, and along one of these channels 21 there are vertical holes or openings 22 drilled. These vertical openings 22 are located at those points where the concentric grooves 20 meet this radial groove. The openings, for example 1.587 mm (1/16 ") in diameter are down to an inner, horizontal plenum 23 drilled through, the z. B. has an inside diameter of about 4.762 mm (3/16 ") and immediately below the Main radial channel and leads to a drain opening 26.

In the side wall of the plug 14 are two circumferential grooves, one above and one below the collecting duct outlet elaborated, are inserted into the sealing rings 24, the against leakage between the plug 14 and the Seal the side wall of the cylinder 10.

On the remaining edges between the grooves 20, a sieve 28 is supported, which at its edges, for example by welding or by using an epoxy resin? or some other glue on the stopper is attached. In the side wall of the cylinder 10, an outlet port 3 2 is formed, which is connected to the outlet port is in alignment when the plug 14 is inserted into the lower end region of the cylinder 10.

The cylinder 10 and piston 16 are heated before start-up. Also a quantity or batch of the hop flour is made z. B. heated in an oven and then poured onto the sieve 28 in the preheated cylinder. The opening size of the Siebs 28 is smaller than the size of whole, intact lupulin glands, so that the hop meal does not fall through can but is retained on the sieve 28. The cross-sectional dimension of an average lupulin gland is approx. 0.15 to 0.2 mm.

Then the preheated piston 16 is inserted into the cylinder 10 and placed between the plates of a hydraulic press. The lower end of the array rests on the lower plate, and the upper plate makes contact with the upper end of the piston 16. Means hydraulic cylinder, the plates are moved against each other.

The liquefied resins and essential oils begin to drain through the outlet port 32 when the pressure on the ^{hop meal reaches approximately 35 kgf / cm 2} (500 psig). The pressure exerted on the hop flour is gradually increased to

raised to 352 kgf / cm ² (5000 psig) or above for maximum yield of liquid concentrate. Following the pressing, the piston 16 and the stopper 14 forming the lower closure member are removed from the cylinder 10, the press cake is removed from the sieve 28 and the device is cleaned.

An alternative method provides for the heated hop flour in a bag 30 made of tightly woven fabric, for example to fill a canvas, canvas or nylon bag and then this bag 3 0 in the chamber 12 im Place the cylinder on a coarse screen 28 '(Fig. 4). The use of a pouch 30 makes it easier to remove the Press cake and the preparation of the arrangement for the next batch. When using a tissue bag it is also possible to use a large-mesh sieve 28 'as a support, since the wall material of the bag 3 0 the task of Sifting and retention of the solids fulfilled.

No precisely defined temperature and pressure conditions are necessary for the process to work. However, temperatures below 60 ° C and pressures below 35 kgf / cm ² (500 psig) are unsatisfactory from the standpoint of yield and rate of production. The upper limit for printing is determined solely by the ability of the press. However, pressures in ^{excess of 352 kgf / cm 2} (5000 psig) on the hop meal resulted in only a slightly higher concentrate yield.

At temperatures above 65 ° C, the viscosity of the resin is reduced and consequently that required for pressing Shortened time. However, it is known that hop aromas are sensitive to heat, so that from this Reason extremely high temperatures should be avoided.

The process according to the invention will be explained in more detail with the aid of the following examples.

Example I.

A press cylinder was used, the inner chamber of which had a diameter of 85 mm and a height of 193 mm. That Sieve 28 had openings that were approximately 0.125 mm across the Measure opening. A batch of 140 g of hop flour with an alpha acid content of approx. 45.5% was weighed out and put into heated in an oven to approx. 65 ° C. The press arrangement was also heated to approx. 65 ° C.

The heated hop meal was then poured into the cylinder 10 onto the sieve 28. The piston 16 was then inserted and the assembly was placed between the plates of a conventional hydraulic press. By operating the press, the piston 16 was pressed against the hop meal. Liquid concentrate began to flow out of the outlet port 32 when the pressure applied to the hop meal reached about 35 kgf / cm ² . The pressure was then gradually increased over a period of 15 minutes to the maximum capacity of the press, which was about 352 kgf / cm ² .

95 g of liquid concentrate were collected which had an alpha acid content of 55.2%. This resulted in a Yield of 82% of the total alpha acid contained in the hop flour.

The liquid concentrate was light brown in color and had a pleasant aroma of natural hops. It was made at room temperature (20 to 25 ° C) very viscous, but could easily be liquefied when heated to approx. 60 ° C.

The press cake obtained weighed 45 g and had an alpha acid content of 23.8%.

Example II

A batch of 140 g of hop flour was placed in a nylon bag and the nylon bag was placed in the top of the cylinder placed on a coarse-meshed sieve 28 ', the sieve openings of which measured about 0.3 4 mm across the opening. The nylon fabric had sieve openings that measured approx. 0.07 mm across the opening.

The hop meal batch and the components of the press were all heated in advance to approx. 65 ° C. The piston 16 was against moving the bag and gradually applying pressure to maximum capacity over a period of 15 minutes the press increased as described in connection with Example I. The 140 g of hop flour, which has an alpha acid content 45%, 9 gave 2.8 g of a liquid concentrate with an alpha acid content of 53.6%. this represented a yield of 79% of the available alpha acid.

Example III

In this example, a lower quality hop flour was used, the alpha acid content of which was approx. 35%. The lower alpha acid content was due to the presence of finely divided green, fibrous, vegetable matter from the crushed scale leaves of the hop cones.

100 g of this lower quality hop flour was heated to approx. 65 ° C. and placed in a canvas bag. The bag was placed in the heated cylinder 10 on a bottom screen 28 having a mesh size of 0.34 mm square. A heated piston 16 was then inserted into cylinder 10 and the assembly placed in a hydraulic press. The pressure applied was gradually increased so that a pressure of about 211 kgf / cm ² (3000 psig) was applied to the hops meal, creating a liquid

Concentrate squeezed through the wall of the canvas bag became. The size of the mesh openings of the canvas was not determined; however, the bag held the solids back, which is a sign that the mesh size was small enough.

The weight of the press cake obtained was approx. 36.4 g, indicating that approx. 63.6 g of the resin had been pressed out was. The press cake contained approx. 14.4% alpha acid, which is approx. 5.24 g of alpha acid in the press cake of the original 35 g of alpha acid corresponded. The calculated alpha acid recovery in the liquid concentrate was approx. 85%.

Example IV

A rather poor quality hop flour was used for this experiment, as it only contained approx. 3 0.2% Alpha acid.

A batch of 100 g of hop meal was weighed out and placed in a nylon bag of the type already used in Example II. The alpha acid content of this batch was approx. 30.2 g. The bag and its contents, as well as the cylinder and piston of the press, were heated to approx. 65 ° C. The bag was then placed in the cylinder 10, the piston 16, preheated to 65 ° C., inserted and the assembly placed between the plates of a hydraulic press. The press was operated so that the pressure on the ^{hop meal batch was gradually increased to about 176 kg / cm 2} (2500 psig).

The press cake weighed approx. 56 g and had an alpha acid content of about 8.5%. This resulted in a remaining content of approx. 4.8 g of alpha acid in the press cake. the 0 amount of alpha acid in the squeezed liquid concentrate was calculated to be approx. 25.4 g, which is 84% of the alpha acid in the original batch represented.

The liquid concentrate was light brown in color and had the pleasant aroma of natural hops.

In accordance with the invention, the press cakes removed from cylinder 10 of the press can be removed using the well known solvent extraction process be treated further. If, as already mentioned, solvent extraction is used to recover more alpha acid from the press cake becomes the product of this secondary process kept separated from the product obtained by mechanical separation in the press and sold to consumers, for which is acceptable as a liquid concentrate containing minor amounts of a residual solvent.

Claims (32)

LIEGK BETTER * Patent Attorneys: - "" 'Dipl.-lng. H.-PeterLiec European Patent'Ättomeys Dipl.-lng. Jürgen Bette Maximiliansplatz D-8000 Munich © 089-220821 Telex 5 216 741 list d Technolaw® Telegram Electropat Process and device ο / O C / g y for the extraction of aromatic resins and oils from hop flour Patent claims 1. Process for separating aromatic resins and oils from hop flour, characterized in that an amount of hop flour is heated to a degree at which the therein Resins contained melt that a pressure of an order of magnitude is exerted on the heated hop flour which breaks down the lupulin and squeezes a viscous, liquid concentrate of aromatic resins and essential oils which is essentially free of cell material, at the same time a press cake is produced as residue, which has the cell material, and that the viscous, liquid concentrate is separated from the press cake. 2. The method according to claim 1, characterized in that the viscous, liquid concentrate through a wall made of a material is pressed out, which is permeable for the viscous, liquid concentrate but not for the press cake. 3. The method according to claim 2, characterized in that the viscous, liquid concentrate is pressed out through openings in a sieve whose size is smaller than intact lupulin glands, whereby the cell material is retained on the sieve is and in this way the press cake is formed and the viscous liquid is separated from the press cake, 4. The method according to claim 3, characterized in that the sieve is on a surface is supported which contains channels into which the separated, viscous, liquid concentrate when pressed flows from the heated lupulin glands through the sieve openings. 5. The method according to claim 1, characterized in that the heated hop flour is filled into a bag consisting of a for the viscous, liquid concentrate, however, is not permeable to the press cake tissue material that this Bag is supported on a coarse sieve, and that pressure is applied to the bag, whereby viscous, liquid concentrate is squeezed out of the heated hop meal through the wall of the bag, while the press cake is retained in the bag. 6. The method according to claim 5, characterized in that the coarse screen is supported on a surface which has grooves, into which the separated, viscous, liquid concentrate when pressed out of the heated hop flour through the wall of the bag and the sieve openings flows. 7. The method according to claim 1, 5 characterized in that additional aroma components of the hops by using a solvent extracted from the press cake. 8. The method according to claim 1, characterized in that pressure is exerted by means of a press comprising a "cylinder and a An end closure member for the cylinder having an interior surface in which a pattern of grooves is formed is that lead to a collection opening that the sieve on this inner surface is arranged so that the heated amount of hop flour is arranged on the sieve side opposite the channels and that a piston is inserted into the cylinder and used to apply pressure to the heated hop meal is used. 9. The method according to claim 8, characterized in that a sieve is used, the openings of which are smaller than the whole, intact Hop flour, and that a sieve is used to collect the press cake, and that the viscous, liquid one Concentrate is separated from the press cake. 10. Method according to claim 8, characterized in that the heated hop flour is filled into a bag, the wall material of which for the viscous, liquid concentrate but not for the press cake that a coarse sieve is permeable the gutters and that a piston is inserted into the cylinder and used to apply pressure to that in the bag Contained, heated hop flour is used, whereby the viscous, liquid concentrate of aromatic resins and oils is squeezed out of the heated hop flour through the wall of the bag and into the gutters. 11. The method according to claim 8, characterized in that the cylinder and the piston are heated to keep the hop meal warm. 12. The method according to claim 11, characterized in that further aroma constituents of the hops are obtained by using a solvent extracted from the press cake. 13. The method according to claim 8, characterized in that by use a solvent further aroma components of the hops are extracted from the press cake. 14. The method according to claim 1, characterized in that a hop flour is used, which with finely divided, green, fibrous, plant matter is mixed with crushed scale leaves of hop cones, and that the fibrous, Vegetable substances are collected in the press cake. 15. The method according to claim 3, characterized in that a hop flour is used, which with finely divided, green, fibrous, plant matter is mixed with crushed scale leaves of hop cones, and that the fibrous, Vegetable substances are collected in the press cake. 16. The method according to claim 4, characterized in that a hop flour is used, which with finely divided, green, fibrous, plant matter is mixed with crushed scale leaves of hop cones, and that the fibrous, Vegetable substances are collected in the press cake. 17. The method according to claim 8, characterized in that a hop flour is used, which with finely divided, green, fibrous, plant matter is mixed with crushed scale leaves of hop cones, and that the fibrous, Vegetable substances are collected in the press cake. 18. The method according to claim 17, characterized in that the cylinder and the piston are heated, wherein the lupulin-containing material is kept warm. 19. Process for separating aromatic resins and oils from hop flour, characterized in that a quantity of hop flour is applied to one for melting the resins contained therein a sufficient degree of preheating is applied to the heated hop meal using a heated press so much pressure is exerted that a viscous, liquid concentrate of aromatic resins and oils from the hops is pressed out, which is essentially free of cell material, at the same time a press cake is produced as a residue, which has the cell material, and that the viscous, liquid concentrate is thereby separated from the press cake that the viscous, liquid concentrate when applied is washed away from the press cake by pressure. 20. The method according to claim 19, characterized in that the viscous, liquid concentrate is pressed through a wall material, which for the viscous, liquid concentrate but not for the press cake is permeable. 21. The method according to claim 19, characterized in that the viscous, liquid concentrate is pressed through openings in a sieve that are smaller than intact, whole lupulin glands, with the cell material being retained on the sieve is and forms the press cake, and that the viscous liquid is separated from the press cake. 22. The method according to claim 21, characterized in that the screen is supported on a surface which has grooves into which the separated, viscous, liquid concentrate after pressing out of the heated hop flour through the sieve openings flows. 23. The method according to claim 22, characterized in that the heated Hop flour is filled into a bag made of a fabric material that is used for the viscous, but liquid concentrate is not permeable to the material of the press cake that the bag on a coarse Sieve is supported, and that pressure is exerted on the bag, the viscous, liquid concentrate from the heated hop flour is pressed through the bag wall and the press cake is retained in the bag. 24. The method according to claim 20, characterized in that the heated Hop flour is filled into a bag, which consists of a fabric material, which for the viscous, liquid But concentrate is not permeable to the material of the press cake that the bag is supported on a coarse sieve is, and that pressure is exerted on the bag, whereby the viscous, liquid concentrate from the heated Hop flour squeezed through the wall of the bag and the press cake is retained in the bag. 25. The method according to claim 24, characterized in that by using a solvent further aroma components of the hops are extracted from the press cake. 26. The method according to claim 20, characterized in that by using a solvent further aroma components of the hops are extracted from the press cake. 27. Product manufactured according to one of processes 1 to 26. 28. Device for pressing out aromatic resins and oils from hops flour, which is used to melt the Resins contained therein preheated to a sufficient degree became, characterized in that an open ended cylinder (10) and an end closure member on the opposite end is provided that the end closure member has an inner surface in which a pattern of is formed leading to a collecting opening grooves that the grooves a sieve (28; 28 ') is superimposed that the The cylinder has a discharge opening communicating with the grooves, and that a piston (16) can be inserted into the cylinder, which, like the cylinder, can be preheated, and that preheated hop meal can be placed between the sieve and the piston, and that the piston is pressed out a viscous, liquid concentrate of aromatic resins and oils from the hop meal is movable to the sieve, wherein the concentrate is essentially free of cell material and at the same time a press cake can be produced as residue, which has the cell material. 29. The device according to claim 28, characterized in that the sieve (28) Has openings that are smaller than intact Lujiulin glands, that the hop flour can be placed on the sieve, and that the sieve collects the press cake and the viscous, separates liquid concentrate from the press cake. 30. Apparatus according to claim 28, characterized in that a bag (3 0), into which the heated hop flour can be filled, consists of a wall material which is suitable for the viscous, liquid But concentrate is not permeable to the material of the press cake so that the bag can be attached to the sieve is, and that the piston is movable against the bag, wherein the hop flour is pressed and the aroma resins and Oils from the heated hop flour through the wall material of the bag, the sieve openings and into the gutters and out the channels are pressed into the dispensing opening. 31. Apparatus according to claim 28, characterized in that the end closure member for the cylinder (10) is removable in the cylinder can be used, and that a sealing device is provided between the end closure member and the cylinder (10) is. 32. Apparatus according to claim 31, characterized in that the end closure member has a side wall opening which corresponds to the grooves in Is connected, and that the cylinder (10) has a side wall opening which corresponds to the side wall opening in the end closure member can be aligned when the end closure member assumes its position in the cylinder.