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Title:
METHOD FOR REMOVING ETHANOL FROM ALCOHOLIC BEVERAGES WITH PRESERVATION OF TASTE AND. AROMA, DEVICE FOR APPLYING THIS METHOD AND AROMA CONCENTRATE OBTAINED FROM THIS METHOD
Document Type and Number:
WIPO Patent Application WO/2022/123420
Kind Code:
A1
Abstract:
The invention relates to a method for removing ethanol from an alcoholic beverage, consisting of the following steps: (i) distilling off a volatile fraction from the alcoholic beverage with formation of an ethanol distillate (2) in which the separated ethanol is found, but also higher alcohols and flavouring aromatics; (ii) rectifying the ethanol distillate (2) in a rectification column (7) in which an enriched pure ethanol fraction (22) is separated from an enriched pure aroma concentrate (30); and (iii) adding the separated pure aroma concentrate (30) back to the alcoholic beverage from which the aroma concentrate (30) was separated to restore the taste of the now non- alcoholic beverage.

Inventors:
VAN BEVEREN PETER CAROLUS
Application Number:
PCT/IB2021/061352
Publication Date:
June 16, 2022
Filing Date:
December 06, 2021
Export Citation:
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Assignee:
DUYNIE B V (NL)
International Classes:
C12H3/00; B01D3/00; C12H3/02
Foreign References:
US4626437A1986-12-02
CA2913095A12013-11-28
US4978547A1990-12-18
Other References:
YULISSA Y BELISARIO-SÃ NCHEZ ET AL: "Aroma Recovery in Wine Dealcoholization by SCC Distillation", FOOD AND BIOPROCESS TECHNOLOGY ; AN INTERNATIONAL JOURNAL, SPRINGER-VERLAG, NEW YORK, vol. 5, no. 6, 12 April 2011 (2011-04-12), pages 2529 - 2539, XP035089245, ISSN: 1935-5149, DOI: 10.1007/S11947-011-0574-Y
Attorney, Agent or Firm:
JACOBS, Tinneke et al. (BE)
Download PDF:
Claims:
Claims.

1.- Method for removing ethanol from an alcoholic beverage, consisting of the following steps: rectifying ethanol distillate (2) obtained from an alcoholic beverage in a rectification column (7) in which an ethanol fraction (22) is separated from an aroma concentrate (30), whereby the rectification column o on the underside is coupled to a circuit (23) which supplies vapour from a reboiler (25) to a vapour stripping section (10) in the rectification column (7), and discharges condensed liquid aroma concentrate at the bottom of the steam stripping zone (10) in liquid state from the bottom zone to a reboiler (25) where the liquid aroma concentrate is boiled again with formation of vapour which is fed back to the vapour stripping section; and o and on the upperside is coupled to a reflux circuit (11) which supplies the enriched pure ethanol fraction at the top of the rectification column (7) from the rectification section (9) to a condenser (14), which brings the enriched pure ethanol fraction into a liquid state and transports it to a separation tank (16) in which the liquid enriched pure ethanol fraction is separated from the aforementioned vapour phase which is returned to the rectification section

(9) at the top of the rectification column (7); and whereby the fluid level in the separation tank (16) is kept constant by a variable speed pump (33'), controlled by a level control unit (31) connected to a level sensor (32) in the separation tank (16), said pump (33') or control valve discharging a quantity of the liquid enriched pure ethanol fraction to a collecting tank ((2211)) for concentrated pure ethanol (22), and whereby the fluid level in the reboiler (25) is kept constant by a variable speed pump (33), controlled by a level control unit (32) connected to a level sensor (31) in the reboiler (25), said pump (33) discharging a quantity of liquid enriched pure arroomma concentrate (30) to a storage tank (29) for pure aroma concentrate (30).

2.- Method according to claim 1, characterised in that the reflux ratio in the reflux circuit (11) amounts to 1 to 3.

3.- Method according to claim 1, characterised in that the ethanol distillate (2) is heated in a heat exchanger (8) before being supplied to the rectification column (7), and the discharged aroma concentrate (30) is cooled in the same heat exchanger (8) before being added to the storage tank (29) for pure aroma concentrate.

4.- Method according to claim 1, characterised in that the separated pure ethanol concentrate (22) is reused as sustainable : fuel, a solvent or disinfectant, or is subjected to a ternary distillation process with separation of pure higher esters and alcohols, which can be used like ethanol itself as a raw material for the chemical industry.

5.- Method according to any one of the previous claims, characterised in that the method before rectifying the ethanol distillate contains the step of distilling off a volatile fraction from the alcoholic beverages at a low temperature and low pressure with formation of an ethanol distillate (2) in which the separated ethanol is present, but also higher alcohols and flavouring aromatics such as polyphenols from wine oorr hop aromatics from beer or aromatics from spirits.

6.- Method according to any one of the previous claims, characterised in that after discharging the aroma concentrate (30) to the storage tank (29) the aroma concentrate (30) is added to the alcoholic beverage again from which the aroma concentrate wwass separated to restore the taste of the now non-alcoholic beverage.

7.- Ethanol fraction obtained from the method according to any one of the previous claims.

8.- Aroma concentrate obtained from the method according to any one of the previous 1 to 6.

9.- Aroma concentrate according to claim 8, characterised in that the ethanol distillate is obtained from beer.

10. Aroma concentrate for enriching a non-alcoholic beverage, characterised in that the aroma concentrate is from an ethanol distillate obtained from an alcoholic beverage, said aroma concentrate containing less than 0.4 wt% ethanol calculated on the total weight of the aroma concentrate.

11.- Aroma concentrate according to claim 10, characterised in that the ethanol distillate is obtained from beer.

12.- Aroma concentrate according to claim 10 or 11, characterised in that the aroma concentrate contains less than 0.3 wt% ethanol.

13.- (Non-alcoholic) beverage containing the aroma concentrate according to any one of the claims 8 to 12.

14.- Device (1) for applying the method, described in claim

1, characterised in that it at least consists of: ethanol distillate a rectification column (7) consisting of a rectification section (9) and a vapour stripping section (10); a reflux circuit (11) consisting of a pipe (12) which connects the discharge (13) at the top of the rectification section (9) with the supply of a condenser (14), from a

Pipe (15) which transports the enriched pure ethanol fraction in liquid state from the condenser (14) to a separation tank (16) in which the liquid enriched pure ethanol fraction (22) is separated from the aforementioned gaseous phase, and a Pipe (17) which returns the aforementioned vapour phase for reflux to the rectification section (9) at the top of the rectification column (7); - a pipe (18) which connects the discharge (19) of the separation tank (16) with the supply (20) of a collecting tank (21) for the enriched pure ethanol fraction (22);

- a vapour stripping circuit (23) consisting of a pipe (24) which supplies vapour from a reboiler (25) to the vapour stripping section (10) in the rectification column (7), and a pipe (26) which discharges condensed liquid aroma concentrate at the bottom of the vapour stripping section (10) in liquid state to the reboiler (25) where the liquid aroma concentrate is boiled again with formation of vapour that is fed back to the vapour stripping zone (10) via the pipe (24); a pipe (27) which connects the discharge (28) for enriched liquid aroma concentrate on the underside of the reboiler (25) with a storage tank (29) for enriched liquid aroma concentrate (30), said pipe (27) going through the heat exchanger (8);

- three variable speed pumps, controlled by a level control unit (31) which is connected to a level sensor (32), one pump (33) of which in the reboiler (25), said pump keeping the level of liquid enriched pure aroma concentrate in the reboiler (25) constant and discharging the excess liquid enriched pure aroma concentrate to the storage tank (29) for pure aroma concentrate (30); a second pump (33') in the separation tank (16), said pump keeping the level of the enriched pure ethanol fraction in the separation tank (16) constant and discharging the excess liquid enriched pure ethanol fraction to the collecting tank (21) for the enriched pure ethanol fraction (22); and a third pump (33") in the pipe (26) keeping the level of liquid enriched aroma concentrate on the underside of the vapour stripping section (10) constant. two variable speed pumps, controlled by a flow control unit (34) which is connected to a flow sensor (35), one pump (36) keeping the flow of ethanol distillate (2) through the Pipe (4) to the rectification column (3) constant, and a second pump (36') keeping the flow of the gaseous phase of the enriched pure ethanol fraction through the pipe (17) to the rectification section (9) of the rectification column (7) constant with the purpose of refluxing.

15.- Device according to claim 14, characterised in that the device contains a pipe (4) which connects the discharge

(5) of the storage tank (2) with the supply (6) of a rectification column (7), said pipe (4) going through a heat exchanger (8).

Description:
Method for removing ethanol from alcoholic beverages with preservation of taste and aroma , device for applying this method and aroma concentrate obtained from this method

The present invention relates to a method for removing ethanol from alcoholic beverages with preservation of taste and aroma and a device for applying this method.

In pa rticular, the invention is intended for removing ethanol from beer, wine or spirits without affecting the taste of the beer, the wine or the spirits .

It is known that non-alcoholic beverages are sold, for example to prevent excessive use of ethanol, or to improve the health of the user, or to improve road safety.

Traditionally, this is done by distilling off ethanol from the alcoholic beverages, with formation of ann ethanol distillate containing the separated ethanol, but also higher alcohols and flavouring substances such ass hop aromatics . The separated ethanol distillate with alcohols and aromatics is completely lost for the remaining non- alcoholic beverage, such that the taste of the non- alcoholic beverage, such as beer, wine , or spirits loses a lot of quality.

Another problem that poses itself, is that the alcoholic beverage must not be heated to the temperature at which ethanol begins to evaporate, in the form of the azeotropic ethanol/water mixture ( 96.4%/3. 6%) which already boils at a temperature of 78.2 °C, a temperature which is lower than the boiling point of pure ethanol (78.4 °C) and pure water

(100 °C) .

To combat the degradation of the taste of the alcoholic beverage, producers use vacuum distillation or distillation at reduced pressure whereby the volatile components evaporate. The distilled off ethanol distillate is destroyed or at least denatured to prevent further use as a foodstuff .

Another problem that poses itself here is that the alcoholic beverage itself must not be refluxed to enrich ethanol in the ethanol distillate to preserve the taste of the alcoholic beverage, as this may cause bothersome foaming of the alcoholic beverage.

The purpose of the present invention is to provide a solution to the aforementioned and other disadvantages, by providing in a method for removing ethanol from an alcoholic. beverage without losing the taste of the alcoholic beverage.

To this end the invention relates to a method for removing ethanol from an alcoholic beverage, consisting of the following steps: rectifying the ethanol distillate in a rectification column in which an enriched pure ethanol fraction is separated from an enriched pure aroma concentrate, the rectification column being coupled on the underside to a circuit which supplies vapour from a reboiler to a vapour stripping section in the rectification column and discharges condensed liquid aroma concentrate at the bottom of the vapour stripping section in a liquid state from the bottom section to a reboiler where the liquid aroma concentrate is reboiled with formation of vapour which is fed back to the vapour stripping section; and being coupled on the upperside to a reflux circuit which supplies the enriched pure ethanol fraction at the top of the rectification column from the rectification section to a condenser, which brings the enriched pure ethanol fraction into a liquid state and passes it to a separation tank in which the liquid enriched pure ethanol fraction is separated from the aforementioned vapour phase which is returned to the rectification section at the top of the rectification column; and whereby the fluid level in the separation tank is kept constant by a variable speed pump, controlled by a level control unit connected to a level sensor in the separation tank, said pump or control valve discharging a quantity of the liquid enriched pure ethanol fraction to a collecting tank for concentrated pure ethanol, and whereby the fluid level in the reboiler is kept constant by a variable speed pump, controlled by a level control unit connected to a level sensor in the reboiler, said pump discharging a quantity of liquid enriched pure aroma concentrate to a collecting tank for pure aroma concentrate. Preferably the reflux ratio in the reflux circuit is 1 to 3. An advantage of this method is that refluxing the volatile fraction can be done in the reflux circuit without causing bothersome foaming.

Preferably, the ethanol distillate is heated in a heat exchanger before being added to the rectification column, and the discharged pure aroma concentrate is cooled in the same heat exchanger before being added to the collecting tank for pure aroma concentrate.

An advantage of said heat exchanger is that it results in energy savings for the whole separation process of pure ethanol fraction and pure aroma concentrate.

The separated pure aroma concentrate can now be added back to the alcoholic beverages from which aroma concentrate was separated to restore the taste of the now non-alcoholic beverages.

The separated pure ethanol concentrate can be reused as a sustainable fuel, a solvent or disinfectant, or subjected to a ternary distillation process with separation of pure higher esters and alcohols, which like ethanol itself can be used as a raw material for the chemical industry. Table

I lists a number of esters and alcohols that were still found in the separated pure ethanol,concentrate of beer for example.

Table I: esters and alcohols occurring, in addition to ethanol, in the pure ethanol concentrate of beer.

(*) concentrated in the top of the distillation.

Table II lists volatile hop derivatives found in the separated pure aroma concentrate of beer Table II: volatile hop derivatives occurring in the separated pure aroma concentrate of beer.

(*) concentrated in the top of the distillation.

The analyses of the volatile hop derivatives from the separated pure aroma concentrate of beer show that said pure aroma concentrate can be added to beer without significantly increasing its ethanol content.

The analysis of the pure ethanol concentrate shows that this concentrate can still be further purified by a ternary distillation process into pure esters and alcohols with a low to very low ethanol content.

These products are applied as aromas or fragrance components in the food industry, in pharmaceutical products such as in ointments and lotions and the like.

With the intention of better showing the characteristics of the invention, a preferred application of the method to remove alcohol from alcoholic beverages according to the invention is described hereinafter, by way of an example without any limiting nature, with reference to the accompanying drawings wherein: figure 1 schematically shows a device for the application of the method according to the invention.

Figure 1 schematically shows a device 1 for rectifying the ethanol distillate 2 obtained by distilling off a volatile fraction from an alcoholic beverage, which comprises the following components:

- a rectification column 7 consisting of a rectification section 9 and a vapour stripping section 10; a reflux circuit 11 consisting of a pipe 12 which connects the discharge 13 at the top of the rectification section 9 with the supply of a condenser 14, from a pipe 15 which transports the enriched pure ethanol fraction in liquid state from the condenser 14 to a separation tank 16 in which the liquid enriched pure ethanol fraction is separated from the aforementioned vapour phase, and a pipe

17 which returns the aforementioned vapour phase for reflux to the rectification section 9 at the top of the rectification column 7; a pipe 18 which connects the discharge 19 of the separation tank 16 with the supply 20 of a collecting tank 21 for the enriched pure ethanol fraction 22;

- a vapour stripping circuit 23 consisting of a pipe 24 which supplies vapour from a reboiler 25 to the vapour stripping section 10 in the rectification column 7, and a pipe 26 which discharges condensed liquid aroma concentrate at the bottom of the vapour stripping section 10 in liquid state to the reboiler 25 where the liquid aroma concentrate is boiled again with formation of vapour that is fed back to the steam stripping zone 10 via a pipe 24; a pipe 27 which connects the discharge 28 for enriched liquid aroma concentrate on the underside of the reboiler

25 with a storage tank 29 for enriched liquid aroma concentrate 30, said pipe 27 going through the heat exchanger 8;

- three variable speed pumps, controlled by a level control unit 31 which is connected to a level sensor 32, one pump

33 of which in the reboiler 25, said pump keeping the level of liquid enriched pure aroma concentrate in the reboiler 25 constant,and discharging the excess liquid enriched pure aroma concentrate to the storage tank 29 for pure aroma concentrate 30; a second pump 33' or control valve in the separation tank 16, said pump or control valve keeping the level of the enriched pure ethanol fraction in the separation tank 16 constant and discharging the excess liquid enriched pure ethanol fraction to the collecting tank for the enriched pure ethanol fraction 22; and a third pump 33" in the pipe 26 which keeps the level of liquid enriched aroma concentrate on the underside of the vapour stripping section 10 constant.

- two variable speed pumps, controlled by a flow control unit 34 which is connected to a flow sensor 35, one pump 36 keeping the flow of ethanol distillate 2 constant through the pipe 4 to the rectification column 7, and a second pump

36' keeping the flow of the vapour phase of the enriched pure ethanol fraction constant through the pipe 17 to the rectification section 9 of the rectification column 7 with the purpose of refluxing. In a preferred embodiment the device 1 contains a collecting tank 3 for the ethanol distillate 2 in which, in addition to separated ethanol, there are also higher alcohols and flavouring aromatics such as polyphenols from wine or hop aromatics from beer or aromatics from spirits.

Preferably, the device 1 also contains a pipe 4 which connects the discharge 5 of the collecting tank 3 with the supply 6 of a rectification column 7, said pipe 4 going through a heat exchanger 8.

The operation of the device 1 for rectifying the ethanol distillate 2 from alcoholic beverages in a rectification column according to the invention can be described as follows.

An ethanol distillate 2 is added to the upper rectification section 9.

Here the volatile ingredients meet the rising vapours from the underlying vapour stripping section 10 which carry the most volatile ingredients to the top 13 of the rectification column where the temperature is around 78.4 °C, the boiling point of the azeotropic ethanol/water mixture.

From here the enriched pure ethanol fraction is guided through a reflux circuit 11 via the pipe 12 to a condenser 14, where the pure ethanol fraction is cooled down until it is liquid, and continues via the pipe 15 to a separation tank 16, in which the liquid enriched pure ethanol,fraction is separated from the aforementioned gaseous phase after which the vapour phase is returned via the pipe 17 to the rectification section 9 at the top of the rectification column, after going through the reflux circuit 11, and is again refluxed in the rectification section 9 whereby a reflux ratio of 1 to 3 is maintained.

In the separation tank 16 the level of liquid enriched pure ethanol fraction is kept constant by a variable speed pump 33' in the pipe 18, controlled by a level control unit 32 which is connected to a level, sensor 31 in the separation tank 16, which discharges an excess of the liquid enriched pure ethanol fraction 22 to a collecting tank 21 for the concentrated pure ethanol fraction.

The underside of the vapour stripping section 10 of the rectification column 7 has a temperature of 100°C fed by a vapour stripping circuit 23 which supplies vapour from a reboiler 25 via pipe 24 to the vapour stripping section 10. The supplied vapour strips volatile components of their water jacket whereby pure volatile components such as alcohols rise upward to the rectification section 9, and liquid water moves downward with formation of condensed liquid aroma concentrate at the bottom of the vapour stripping section 10.

The level of liquid aroma concentrate at the bottom of the vapour stripping section 10 is kept constant by a variable speed pump 33" in the pipe 26, controlled by a level control unit 32 which is connected to a level sensor 31 on the underside of the rectification column 7, which returns an excess of the liquid aroma concentrate to the reboiler 25 where it is converted again into vapour and the vapour stripping circuit 23 is closed.

The level of liquid aroma concentrate is kept constant in the reboiler 25 by a variable speed pump 33 in the pipe 27, controlled by a level control unit 32 which is connected to a level sensor 31 in the reboiler 25, which discharges an excess of the liquid aroma concentrate via a pipe 27 through the heat exchanger 8 in which the aroma concentrate is cooled and further guided to a storage tank 29 for liquid aroma concentrate.

The alcoholic beverage from which ethanol was removed, can be flavoured again by adding a suitable quantity of aroma concentrate, and the residual pure ethanol concentrate can be further purified into pure esters and alcohols for use in the chemical industry or as a sustainable fuel or as a raw material.

A pipe 27 which connects the discharge 28 for enriched liquid aroma on the underside of the reboiler 25 with a storage tank 29 for enriched liquid aroma concentrate 30, is a pipe 27 which goes through the heat exchanger 8 whereby the aroma concentrate is cooled by heating the newly supplied ethanol distillate in the pipe 4 such that thermal energy is saved.

An advantage of the device 1 for the application of the method according to the invention is that it allows a continuous process to be maintained with a constant supply of ethanol distillate 2 and a constant discharge of aroma concentrate 30 for addition to the now non-alcoholic alcoholic beverage, such that said beverage retains its taste and aroma.

Preferably, the aforementioned ethanol distillate 2, formed by distilling off a volatile fraction from an alcoholic beverage, contains separated ethanol, higher alcohols and flavouring aromatics such as polyphenols from wine or hop aromatics from beer.

This ethanol distillate 2 can then be collected in a storage tank 3, from where the ethanol distillate 2 can be pumped via a pipe 4 by a flow controlled pump 36 to a heat exchanger 8 in which the ethanol distillate 2 is preferably heated before flowing to a rectification column 7.

The present invention also relates to an ethanol fraction and an aroma concentrate 30.

The aforementioned ethanol fraction is obtained from the method as described above.

The aroma concentrate 30 is also obtained from the method as described above.

The aroma concentrate 30 is intended for enriching a non- alcoholic beverage, said aroma concentrate 30 coming from an ethanol distillate 2 obtained from an alcoholic beverage. An advantage of this is that the non-alcoholic beverages enriched with the aroma concentrate 30 are closer to the alcoholic variant at least in terms of taste compared to the non-enriched non-alcoholic beverages.

Consequently, lovers of the alcoholic variant will be.more inclined to consume the enriched non-alcoholic beverage.

This aroma concentrate 30 contains less than 0.4 wt% ethanol relative to the total weight of the aroma concentrate 30.

Preferably, the ethanol distillate 2, from which the aroma concentrate 30 is obtained, is from beer.

Preferably, the aforementioned aroma concentrate 30 contains less than 0.3 wt% ethanol, more preferably even less than 0.2 wt% ethanol and most preferably less than 0.1 wt% ethanol and preferably more than 0.001 wt% ethanol and even more preferable more than 0.01 wt% ethanol.

The present invention is by no means limited to the embodiment described as an example and shown in the drawings, but such a method for removing ethanol from alcoholic beverages and a device for applying this method can be realised according to different variants without departing from the scope of the invention, as described in the following claims.