Method for Dealcoholization of Beverages

Abstract

The present invention relates to a method and production system for dealcoholization of beverages such as beers and wines.

Claims

1. Method for dealcoholization of beverages comprising the steps (a) Providing a beverage containing from 1 to 40 vol.-% of ethanol in a container; (b) Conveying the beverage through at least one exchange column comprising filling material and a counter-currently flowing inert-gas stream; (c) Contacting the inert-gas stream with at least one adsorber column comprising a MFI zeolite and/or a silicalite with a molar SiO.sub.2/Al.sub.2O.sub.3 ratio of at least 200; (d) Recycling of the inert-gas stream to the at least one exchange column; (e) Desorbing the ethanol from at least one adsorber column; (f) Repeating steps (a) to (e) at least once; wherein steps (c) and (e) are at least partly carried out simultaneously.

2. Method according to claim 1, wherein the at least one exchange column is a packed column.

3. Method according to any of the foregoing claims, wherein the beverage is selected from beer, wine, spirit or mash.

4. Method according to any of the foregoing claims, wherein the adsorber of the at least one adsorber column is an MFI zeolite, a silicalite or a mixtures thereof with a molar SiO.sub.2/Al.sub.2O.sub.3 ratio of from 200 to 1500.

5. Method according to any of the foregoing claims, wherein steps (a) to (e) are repeated from 10 to 3500 times for a time period of from 2 minutes to 60 minutes.

6. Method according to any of claims 2 to 5, wherein the filling material of the at least one exchange column comprises from 100 to 5000 Raschig rings per liter exchange column capacity.

7. Method according to any of the foregoing claims further comprising the step (g) separating the dealcoholized beverage.

8. System for the dealcoholization of beverages, comprising (i) A container [6]; (ii) At least one exchange column [1] comprising a filling material [2]; (iii) At least two adsorber columns [4a] and [4b] comprising a MFI zeolite and/or a silicalite with a molar SiO.sub.2/Al.sub.2O.sub.3 ratio of at least 200;

9. System according to claim 8, wherein at least one desorption cycle is connected to at least one adsorber column [4].

10. System according to any of claim 8 or 9, wherein the system contains at least one heat exchanger [11].

11. System according to any of claims 8 to 10, wherein the system contains at least one ethanol trap [12].

12. System according to any of claims 8 to 11, wherein the system contains at least one inert-gas source [GS].

Description

EXAMPLES AND FIGURES

[0087] The present invention is explained in greater detail below by means of the examples. It is emphasized that the examples illustrate particular embodiments and do not limit the scope of the present application in any way.

[0088] FIG. 1: shows an exemplary system according to the invention comprising on exchange column and two adsorber columns

[0089] FIG. 2: shows an exemplary system according to the invention comprising one exchange column, two adsorber columns, a heat exchanger and an ethanol trap

[0090] FIG. 3: shows the results of example 1

[0091] FIG. 4: shows the results of example 3

[0092] FIG. 5: shows the results of example 4

[0093] FIG. 6: shows the results of example 5

[0094] FIG. 7 shows an exemplary set up of a continuous production line

DETAILED DESCRIPTION OF FIG. 1

[0095] FIG. 1 shows an exemplary system for conducting a method for dealcoholization of beverages comprising the steps [0096] (a) Providing a beverage containing from 1 to 40 vol.-% of ethanol in a container [6]; [0097] (b) Conveying the beverage [7] through one exchange column [1] comprising filling material [2] and a counter-currently flowing inert-gas stream [3]; [0098] (c) Contacting the inert-gas stream with at least one adsorber column [4a] or [4b] comprising a MFI zeolite and/or a silicalite with a molar SiO.sub.2/Al.sub.2O.sub.3 ratio of at least 200; [0099] (d) Recycling of the inert-gas stream [5] to the exchange column [1]; [0100] (e) Desorbing [8] the ethanol from at least one adsorber column [4a] or [4b]; [0101] (f) Repeating steps (a) to (e) at least once;
wherein steps (c) and (e) are at least partly carried out simultaneously.

DETAILED DESCRIPTION OF FIG. 2

[0102] FIG. 2 exemplarily shows another setup of an inventive system comprising one exchange column, two adsorber columns, a heat exchanger and an ethanol trap.

[0103] The system includes a container [6] providing the beverage. A feed line [7] is provided for conveying the beverage to the exchange column [1]. In this example the feed line is provided with a respective pumping unit [P6] for controlling respective feed line flows. The exchange column [1] is filled with filling material [2]. At the bottom of the exchange column the beverage containing reduced ethanol concentration is removed [14]. In this example the beverage is removed by using a pump [P14]. The beverage is either pumped back [15] into the container [6] or removed [16] depending on the desired final ethanol concentration of the beverage.

[0104] The system includes a gas feed line [3] to feed the inert-gas stream into the exchange column [1]. The gas feed line is provided with a pumping unit [P3] for pumping the inert-gas into the exchange column [1]. After leaving the exchange column the gas stream is contacted with the adsorber column [4a] or [4b] and recycled into the gas line [5] feeding exchange column. In the present example two columns are used [4a] and [4b]. The gas line includes a gas source [GS1] to balance gas losses during the switch from adsorption to desorption. For switch between adsorption and desorption valves [9a], [9b], [9c] and [9d] are used.

[0105] For desorption a gas line [8] is used provided by a gas source [GS2]. The gas desorbs the ethanol from the adsorber columns and leaves the adsorber columns in a gas line [10]. In this example a vacuum pump [P10] is used to reduce the pressure during desorption. The inert-gas stream is cooled by a heat exchanger [11] to condensate the ethanol and removed in an ethanol trap [12] from the gas stream. The inert-gas stream is either recycled into the desorption gas line [8] or removed [13].

DETAILED DESCRIPTION OF FIG. 7

[0106] FIG. 7 exemplarily shows another setup of an inventive system for a continuous dealcoholization of the beverage resulting in a decreased process time compared to the batch process and a lower influence on the product behavior.

[0107] The system includes the container system [A] providing the beverage. The beverage is fed into the dealcoholization system [B1] as described in FIG. 2. The beverage is not recycled into the container and fed into a second dealcoholization system [B1], leaving as dealcoholized product [P].

Example 1

[0108] Comparison batch and inventive continuous dealcoholization process 15 L beer (Oettinger export, 5.4 vol.-%) were provided in a container.

[0109] Within the batch process a CO.sub.2 stream (20 L/min) was sparged at the bottom of the container. After leaving the container at the top the CO.sub.2 gas stream was contacted with the adsorber columns and recycled into the container continuously.

[0110] Within the continuous process the beer was conveyed by using a peristaltic pump (Watson Marlow, 520DU) into an exchange column (height 1400 mm, diameter 60 mm) at the top of the column with a volume flow of 1.5 L/h. The exchange column (diameter 60 mm, height 1400 mm) was filled with filling material (Glas Raschig rings, diameter 4 mm, height 4 mm, Lenz Laborglas Instrumente). The dealcoholized beer was removed at the bottom by a second peristaltic pump (Watson marlow, 520DU) and fed back into the container. A counter-currently flowing CO.sub.2 stream (20 L/min) was conveyed from the bottom to the top of the exchange column. The exchange column was used at a pressure of 1.013 bar and a temperature of 22° C. The CO.sub.2 gas stream was contacted with the adsorber columns and recycled into the exchange column.

[0111] For adsorption three adsorber columns were used, filled with adsorber material (Clariant, TZP9028; MFI Zeolith, molar SiO.sub.2/Al.sub.2O.sub.3 ratio 1000). Simultaneously two columns were used for adsorption, one column for desorption. After 10 min the columns were switched. For desorption of the ethanol from the adsorber columns a CO.sub.2 gas flow (0.5 L/min) was used. By a vacuum pump the pressure in the adsorber columns was reduced to 120 mbar.

[0112] FIG. 3 shows the mass of ethanol which was removed after 100 h and 200 h from the beer per L of used adsorber material. It is apparent from the results of example 1 that the inventive continuous process leads to a significant higher removal of ethanol.

Example 2: Comparison of Operating Costs and Environmental Impact for Reverse Osmosis and Inventive Continuous Dealcoholization Process

[0113] The operating costs of the state of the art dealcoholisation by reverse osmosis were compared with the inventive process. For the reverse osmosis the data were used, provided by a manufacturer of a reverse osmosis plant for dealcoholization of beer (Alfa Laval beer dealcoholization system, Beer DeAL 300):

Energy price of 0.095€/kWh
Waste water costs of 1.50 €/m

[0114] The diafiltration water for the reverse osmosis unit was produced by a second reverse osmosis with an energy demand of 0.75 kWh/m.sup.3 for produced diafiltration water and a recovery of 80%.

[0115] The tables 1 and 2 show the costs of both processes. The costs of the inventive continuous process are caused by the energy demand for the adsorption and desorption gas flows and the cooling and heating of these flows. The reverse osmosis needs less electrical energy but the costs are dominated by the disposal of the waste water. For the production of dealcoholized beer the threefold amount of diafiltrated water is needed.

[0116] It is apparent from the results as shown in tables 1 and 2 that the inventive process is more cost effective compared to the state of the art process of reverse osmosis. Another advantage is the minimization of wastes by the inventive process. Only a gas as CO.sub.2 is needed for the process which is available from the fermentation and/or brewing process. For the reverse osmosis water and additional cleaning agents are needed which must be disposed.

TABLE-US-00001 TABLE 1 Costs for dealcoholisation by inventive continuous process Process Costs [€ Cent/L beer] Adsorption 0.3557 Desorption 0.0587 Beer conveying 0.0029 Total cost 0.4173

TABLE-US-00002 TABLE 2 Cost for state of the art dealcoholisation by reverse osmosis Process Costs [€ Cent/L beer] Reverse osmosis 0.2533 Cleaning reverse osmosis 0.1057 Providing diafiltration water 0.0214 Waste water 0.5875 Total cost 0.9679

Example 3: Dealcoholization of Beer (5.4 Vol.-%) to 0.8 Vol.-%

[0117] 2 L beer (Oettinger export, 5.4 vol.-%) were provided in a container and conveyed by using a peristaltic pump (Watson Marlow, 520DU) into the exchange column (diameter 60 mm, height 1400 mm) at the top of the column with a volume flow of 1.5 L/h. The exchange column (diameter 60 mm, height 1400 mm) was filled with filling material (Glas Raschig rings, diameter 4 mm, height 4 mm, Lenz Laborglas Instrumente). The dealcoholized beer was removed at the bottom by a second peristaltic pump (Watson marlow, 520DU) and fed back into the container. A counter-currently flowing CO.sub.2 stream (20 L/min) was conveyed from the bottom to the top of the exchange column. The exchange column was used at a pressure of 1.013 bar and a temperature of 22° C. The CO.sub.2 gas stream was contacted with the adsorber columns and recycled into the exchange column. For adsorption three adsorber columns were used, filled with adsorber material (Clariant, TZP9028; MFI Zeolith, molar SiO.sub.2/Al.sub.2O.sub.3 ratio 1000). Simultaneously two columns were used for adsorption, one column for desorption. After 10 min the columns were switched. For desorption of the ethanol from the adsorber columns a CO.sub.2 gas flow (0.5 L/min) was used. By a vacuum pump the pressure in the adsorber columns was reduced to 120 mbar.

[0118] FIG. 4 shows the ethanol concentration of the beer sample during the dealcoholisation process. It can be seen from the results of example 3 that the ethanol was removed from the beer continuously.

Example 4: Dealcoholization of White Wine (10.2 Vol.-%) to 3.2 Vol.-%

[0119] 1.5 L white wine (Caveneta, Niederrhein-Gold Tersteegen GmbH & Co. KG, 10.0 vol.-%) were provided in a container and conveyed by using a peristaltic pump (Watson Marlow, 520DU) into the exchange column (1400 mm height, 60 mm diameter) at the top of the column with a volume flow of 1.5 L/h. The exchange column (diameter 60 mm, height 1400 mm) was filled with filling material (Glas Raschig rings, diameter 4 mm, height 4 mm, Lenz Laborglas Instrumente). The dealcoholized white wine was removed at the bottom by a second peristaltic pump (Watson marlow, 520DU) and fed back into the container. A counter-currently flowing CO.sub.2 stream (20 L/min) was conveyed from the bottom to the top of the exchange column. The exchange column was used at a pressure of 1.013 bar and a temperature of 21° C. The CO.sub.2 gas stream was contacted with the adsorber columns and recycled into the exchange column. For adsorption three adsorber columns were used, filled with adsorber material (Clariant, TZP9028; MFI Zeolith, molar SiO.sub.2/Al.sub.2O.sub.3 ratio 1000). Simultaneously two columns were used for adsorption, one column for desorption. After 10 min the columns were switched. For desorption of the ethanol from the adsorber columns a CO.sub.2 gas flow (0.5 L/min) was used. By a vacuum pump the pressure in the adsorber columns was reduced to 120 mbar.

[0120] FIG. 5 shows the ethanol concentration of the white wine sample during inventive dealcoholisation process. It can be seen from the results of example 4 that the ethanol was removed from the white wine continuously.

Example 5: Dealcoholization of Sparkling Wine (10.2 Vol.-%) to 4.0 Vol.-%

[0121] 1.5 L sparkling wine (Burg Schoeneck, St. Ambrosius Sektkellerei GmbH, 11.0 vol.-%) were provided in a container and conveyed by using a peristaltic pump (Watson Marlow, 520DU) into the exchange column (1400 height, 60 diameter) at the top of the column with a volume flow of 1.5 L/h. The exchange column (diameter 60 mm, height 1400 mm) was filled with filling material (Glas Raschig rings, diameter 4 mm, height 4 mm, Lenz Laborglas Instrumente). The dealcoholized sparkling wine was removed at the bottom by a second peristaltic pump (Watson marlow, 520DU) and fed back into the container. A counter-currently flowing CO.sub.2 stream (20 L/min) was conveyed from the bottom to the top of the exchange column. The exchange column was used at a pressure of 1.013 bar and a temperature of 21° C. The CO.sub.2 gas stream was contacted with the adsorber columns and recycled into the exchange column. For adsorption three adsorber columns were used, filled with adsorber material (Clariant, TZP9028; MFI Zeolith, molar SiO.sub.2/Al.sub.2O.sub.3 ratio 1000). Simultaneously two columns were used for adsorption, one column for desorption. After 10 min the columns were switched. For desorption of the ethanol from the adsorber columns a CO.sub.2 gas flow (0.5 L/min) was used. By a vacuum pump the pressure in the adsorber columns was reduced to 120 mbar.

[0122] FIG. 6 shows the ethanol concentration of the sparkling wine sample during the dealcoholisation process. It can be seen from the results of example 5 that the ethanol was removed from the sparkling wine continuously.