BE1028859B9 - Method for removing ethanol from alcoholic beverages while preserving taste and aroma and apparatus for applying this method - Google Patents

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 the formation of a residual product (2) containing the separated ethanol, but also higher alcohols and flavoring aromatics; (ii) rectifying the residual product (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 isolated pure flavor concentrate (30) back to the alcoholic beverage from which the flavor concentrate (30) was isolated to restore the taste of the now non-alcoholic beverage.

Description

Method for removing ethanol from alcoholic beverages while preserving taste and arcma and apparatus for applying this method. 9 ; éme it id recent rene Eeen 9 The present invention relates to a method; for removing ethanol from alcoholic beverages | while retaining taste and aroma and on a device for applying this method,

More specifically, the invention is intended to remove ethanol from beer, wine or spirits without affecting the taste of the beer, wine or spirits,

It is known that non-alcoholic drinks are marketed, for example to prevent excessive use of ethanol, or to protect the health of the user | or to promote road safety. =0 Traditionally, ethanol is thereby distilled off from the alcoholic beverages to form a residual product containing the separated ethanol, but also higher alcohols and flavoring substances such as hoparomatics.

The separated residual product with alcohols and aromatics is not completely lost to the remaining non-alcoholic drink, as a result of which the taste of the non-alcoholic drink, such as beer, wine or spirits, loses a lot of quality.

Another problem that arises here is that the alcoholic drink must not be heated to the temperature at which ethanol begins to evaporate, in the form of the azeotropic mixture erchancl/water (96.4%/3.6%), which is already boiling. at a temperature of 78,2 °C, is a temperature lower than the boiling point of pure {5 ethanol (78.4 °C) and of pure water (100 °C), [ To prevent degradation of the taste of the alcoholic drink too | Therefore, manufacturers use a vacuum distillery or distillation at reduced pressure where the volatile components evaporate. The distilled residual product is thereby destroyed or at least denalured. In order to prevent further use as a food, another problem that arises here is that the alcoholic beverage may not be refluxed to enrich the residual product with ethanol to enhance the taste of the alcoholic beverage. drink, as there is an annoying | skewing in the alcoholic drink can occur.

The present invention aims to solve the foregoing and other drawbacks by providing a method for removing ethanol from an alcoholic beverage without losing the taste of the alcoholic beverage. removal of ethanol from an alcoholic drink, consisting of the following steps:

- distilling off a volatile fraction from the alcoholic beverage at a low temperature and low pressure with the formation of a residual product containing the separated ethanol, but also higher alcohols and flavoring

& aromatics such as polyphenols from wine, hop aromas from beer,

: or aromatics from spirits;

- rectifying the residual product in a rectification column containing enriched pure

12 Ethanol fraction is separated from an enriched pure aroma concentrate, the rectification column at the bottom is coupled to a circuit that feeds vapor from a reboiler to a vapor stripping zone in the rectification column, and condensed liquid sroma concentrate at the bottom of the vapor stripping zone discharges in liquid state from the bottom zone to a reboiler where the liquid arcma concentrate is re-seeded to form vapor which is fed back to the vapor stripping zone; and is connected at the top to a reflux circuit which feeds the enriched pure erhanol fraction at the top of the rectification column from the rectification zone to a condenser, which converts the enriched pure ethanol fraction into a liquid state and passes it through to a separation tank in which the liquid enriched pure ethanol fraction is separated from the above damo-shaped phase which is returned to the rectification zone at the top of the rectification column: and wherein the vice substance 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, which pump or control valve delivers a quantity of the liquid enriched pure ethanol fraction to a receiving tank for | = concentrated pure ethanol, and ; wherein the liquid level in the reboiler is kept constant by a variable speed pump controlled by a level controller connected to a level sensor in the reboiler, the 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 loop is 1 to 3. An advantage of this method is that the reflux of the volatile fraction can take place in the reflux loop without causing annoying foaming.

Preferably, the residual product 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 receiving trough for pure aroma concentrate.

An advantage of this heat exchanger is that it provides energy savings for the entire separation process of pure ethanol fraction and pure aroma concentrate.

The separated pure aroma concentrate can now be added back to the alcoholic drink from which the aroma concentrate was separated in order to restore the taste of the now non-alcoholic drink. 5 { The isolated pure ethanol concentrate can be reused ; can be used as a sustainable fuel, as a solvent or disinfectant, or can be tertiary distilled with separation of pure higher esters and alcohols, which, like ethanol itself, can be used as raw material for the chemical industry.

Table I lists a number of esters and alcohol: which were still found in the isolated pure ethanol concentrate of beer, for example,

& BE2020/5886 n-propañol PR 40.3 { <i.0 | | Isoburanol — 40.5 { <0.5 | |2+3-methylbutanol 226 | <0.5 } Ethyihezancate OÙ 0.18 160208 2 2rphenylethanol | | 3.20 «0.05 Phthyloctanoate A 0.02 <0.01 | Phenylethyl acetate 3.23 | <0.03 |

EE Ethyvl decancate n.C, { n.d, | Table I: Esters and alcohols occurring in addition to ethanol in the pure ethanol concentrate of beer, {*) concentrated at the top of the distillation, Table II lists the liquid hop derivatives found in the isolated pure beer aroma concentrate.

Gien — kenn ; SD | UG /L* | uG/L* | | Monote rpen already € cholen | | | : egg ; oh linalol | 48.2 | <0.05 { : ee L eee 9 | 1-terpinene-é-ol 0.83 | <0.05 | : | SE | | alpha-terpinol 21.9 ; <0.05 3 | nerol + b-citronellol 23.5 | 20.05 | geraniol 17.2 PU <0.05 | Geranicide derivative nn PE geranial 7 7 1,06 | <0.05 aa neryl acetate <0.05 | <0.05 nen one] | geranyl acetate 0.41 | <0.05 | Monoterpene Sa | brmyrcene | <0.05 | <0.05 | ‘ Ketones | Oxzy-trans-nerolidol <0.05 | caryophyllene alcohol 11.0 | <0.05 ' 4 ee humulene epoxide I ' 0.70 | <0. 05 | humuiol 10 18.3 | <0.05 | humuiene epoxide II 0.63 { <0.05 | OO ra-cadinol 6.91 | <0.05 t-cadinol | 22.3 | <0.05 b-eudesmol I 16.7 <0.05 | g BE2020/5886 Table II: volatile hop derivatives present in the isolated pure beer flavor concentrate, {*) concentrated at the top of the distillation, | > The analyzes of the volatile hop derivatives from the isolated pure beer aroma concentrate show that this pure aroma concentrate can be added to beer without appreciably increasing its ethanol content.

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

{ 15 These products find application as aromas or fragrance components in the food industry, in pharmaceutical products such as in ointments and lotions and so on.

| In order to better demonstrate the features of the invention, a preferred application of the method for removing ethanol from alcoholic beverages according to the invention is described below, by way of example without any limiting character, with reference to the accompanying drawings, in which : figure 1 schematically represents a device for applying the method according to the invention. Figure 1 schematically represents a device 1 for rectifying the residual product 2 obtained by distilling off a volatile fraction from an alcoholic beverage, comprising the following parts includes:

- a storage tank 3 for the residual product 2 in which, in addition to separated erhanol, there are also higher alcohols and 9 flavoring aromatics such as polyphenols from wine or hop aromas from beer or aromatics from spirits; - a conduit 4 connecting the outlet 5 of the storage tank 2 with the inlet 6 of a rectification column 7, which conduit 4 passes through a heat exchanger 8; - a rectification column 7 consisting of a rectification zone 3 and a vapor stripping zone 10; : 15 - a reflux circuit 11 consisting of a pipe 12 connecting the outlet 13 at the top of the rectification zone 9 to the inlet of a condenser 14, of a pipe 15 connecting the | liquid enriched pure ethanol fraction passes from the condenser 14 to a separation tank 16 in which the liquid enriched pure ethanol fraction is separated from the above vaporous phase, and from a line 17 which returns the above vaporous phase for reflux to the rectification zone 9 at the top in the rectification column 7; - a line 18 connecting the outlet 19 of the separation tank 16 with the inlet 20 of a storage tank 21 for the enriched pure ethanol fraction 22:

= a vapor stripping loop 23 consisting of a pipe

24 feeding vapor from a reboiler 25 to the vapor stripping zone 10 in the rectification column 7, and a conduit 26 which discharges condensed wineable flavor concentrate at the bottom of the vapor stripping zone 10 into liquid | > state to the reboiler 25 where the liquid | aroma concentrate is reboiled with formation of vapour; which is returned to the steam stripping zone 10 via line 24 | fed; 10 - a conduit 27 connecting the discharge 28 for fortified liquid aroma concentrate at the bottom of the reboiler 25 to a storage tank 25 for fortified liquid aroma concentrate 38, which conduit 27 passes through the heat exchanger 8;

- three variable-speed pumps controlled by a level control unit 31 connected to a level sensor 32, one of which is pump 33 in the reboiler 25, which pump keeps the level of liquid pure aroma concentrate in the reboiler 25 constant and makes the mixture liquid discharges pure aroma concentrate to the pure aroma concentrate collecting tank 29; a second pump 337 Qt control valve in the separator vessel 16 which pump or pilot valve maintains the level of the enriched pure ethanol fraction in the separator vessel 16 constant and discharges the excess liquid san-rich pure ethanol fraction to the enriched pure ethanol fraction collecting tank 21; and a third pump 33" in line 26 that maintains the level of liquid-enriched arcma concentrate at the bottom of the vapor stripping zone 19 constant.

- two variable speed pumps controlled by a flow control unit 34 connected to a flow rate sensor 35, one pump 36 of which keeps the flow rate constant # of residual product 2 through line 4 to the | 5 rectification column 3, and a Lweede pump 36° the flow rate | keeps constant the vaporous phase of the enriched pure ethanol fraction through the line 17 to the rectification zone 9 of the rectification column 7 for reflux. | The operation of the device 1 for rectifying the residual product 2 from alcoholic beverages in a rectification column according to the invention can be described as follows,

The residual product 2, formed by distilling off a volatile fraction from an alcoholic beverage, contains separated erhanol, higher alcohols and flavoring aromatics such as polyphenols from wine or hop aromas from beer.

This residual product 2 is collected in a storage tank 3, from which the residual product 2 is pumped via a line 4: is sent by a flow-controlled pump 36 to a heat exchanger 8 in which the residual product 2 is observed before flowing to a rectification chamber 7, where it is residual product is fed to the upper rectification zone 5. Here the volatile components meet the rising vapors from the underlying vapor stripping zone 10 which carry the most volatile components to the top 13 of the rectification column where the temperature is at and around 78.4 °C. the azectropic mixture ethanol/water.

From here, the enriched pure ethanol fraction ; 3 through a reËfluzkringionp 11 vis conduit 12 to a | condenser 14, where the pure ethanol fraction is cooled until it is liquid, and via line 15 on to a separation tank 16, where the liquid pure ethanol fraction used is separated from the above gaseous phase after which the vapor phase is recycled via line 17 to the rectification zone 9 at the top of the rectification column, after going through the reflux cycle il, and refluxed again in the rectification zone 9 maintaining a reflux ratio of 1 to 3. In the separation tank 16 the level of liquid enriched pure ethanol fraction is kept constant by a pump 33 variable speed in line 18, controlled by a level controller 32 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 receiving tank 21 for the concentrated pure ethanol fraction.

At the bottom of the vapor stripping zone 10 of the rectification column 7 there is a temperature of 100°C fed by a vapor stripping loop 23 which supplies vapor from a reboiler 25 via line 24 to the vapor stripping zone 10. The supplied vapor strips volatile components from their vapor mantle leaving pure volatile components such as alcohols rise upwards to the rectification zone 9, and liquid water moves downwards forming condensed liquid aroma concentrate at the bottom of the vapor stripping zone 10.

The level of liquid flavor concentrate at the bottom of the vapor stripping zone 10 is kept constant by a variable rate comp 33% in line 26, controlled by a level controller 32 connected to a level sensor 31 at the bottom of rectification column 7, which measures the amount of the liquid aroma concentrate is returned to the reboiler 25 where it is converted back to vapor and the vapor stripping loop 23 is closed.

In the reboiler 25, the level of liquid aroma concentrate is kept constant by a variable speed pump 33 in line 27, controlled by a level control unit 32 connected to a level sensor 31 in the reboiler 25, which discharges an excess of the liquid aroma concentrate. via a conduit 27 through the heat exchanger 3 in which the aroma concentrate is cooled and is further passed to a collecting tank 29 for liquid arcma concentrate.

The alcoholic beverage from which ethanol has been removed can be re-smasked by adding an appropriate amount of aroma concentrate, and the remaining pure ethanol concentrate can be further purified to pure esters and alcohols which can be used for the chemical industry or as a sustainable fuel or as raw material.

A pipe 27 which connects the discharge 28 for enriched liquid aroma concentrate at the bottom of the reboiler 25 to a storage tank 28 FOR liquid aroma concentrate 30, is a pipe 27 which flows through the heat exchanger 8 where the aroma concentrate is cooled by the newly supplied residual product in pipe ; to heat à co, which saves thermal energy.

An advantage of the device 1 for applying the method according to the invention is that it allows to maintain a continuous process with a constant supply of residual product 2 and a constant discharge of aroma concentrate 30 for addition to the now non-alcoholic alcoholic drink, whereby this drink retains its taste and aroma.

The present invention is by no means limited to the embodiment described by way of example and shown in the figures, but such a method for removing ethanol from alcoholic beverages and such a device for applying this method can be realized according to different variants without going beyond the scope of the invention as defined in the following claims,

Claims (1)

Conclusions, Li.” Process for removing ethanol from an alcoholic drink, consisting of the following steps: - distilling off a liquid reaction from the alcoholic drink at low temperature and low pressure with the formation of a residual product (2) containing the separated ethanci, but also higher alcohols and flavoring aromatics such as polyphenols from wine or hop aromas from beer or aromatics from spirits; - the rectification of the residual product {23 in a rectification column {#3 in which an added pure ethanol fraction {22} is separated from an enriched: pure aroma concentrate (30), wherein the rectification column Do is connected at the bottom to a circuit (23) which Steam from a reboiler (25) feeds to a vapor stripping zone {10} in the rectification column (73, and condensed liquid aroma concentrate at the bottom of the steam stripping zone {10}; discharges in liquid state from the bottom zone to a reboiler (25) where the liquid arcma concentrate is reboiled producing vapor which is fed back to the vapor stripping zone; and Oo is coupled at the top to a reflux loop {11} which feeds the enriched pure ethanol fraction at the top of the rectification column (7) from the rectification zone (8 to a condenser (14), which converts the enriched pure ethanol fraction into a viable state: and passes through : to a separation tank {16) in which the liquid | enriched pure ethanol fraction is separated from | 5 the above gaseous phase which is recycled to the rectification zone (3) at the top of the ; rectification column (71; and | wherein the liquid substance level in the separation tank {16} | 18 is kept constant by a variable-speed pump (33°) controlled by a level control unit (313 | connected to a level sensor 132) in the | separation tank {16}, which pump {337} or control valve discharges a quantity of the liquid enriched pure : 15 ethanol fraction to a collecting tank {21} for concentrated pure ethanol (22), and whereby the liquid level in the reboiler {25) is constant is maintained by a variable speed pump (33) controlled by a level control unit {32} which is connected to a level sensor (31) in the reboiler {25}, which pump {33} and quantity of liquid enriched pure aroma concentrate ( 30) to a collecting tank (29) for pure aroma concentrate (30), and = adding the separated pure aroma concentrate (30) back to the alcoholic drink from which the aroma concentrate was separated in order to restore the taste of the now non-alcoholic drink, Method according to claim 1, characterized in that the reflux ratio in the refluxing cycle lye {11} is 1 to 3. Method according to claim 1, characterized in that : the residual product {2} is heated in a heat exchanger 9 {8}; before being fed to the rectification column (73:), and the discharged pure aroma concentrate {30} | is cooled in the same heat exchanger {8} before being added to the collecting tank (29) for pure aroma concentrate. Method according to claim 1, characterized in that | the isolated pure ethanol concentrate {22} | 15 is reused as a sustainable fuel, as a solvent or disinfectant, or is tertiary distilled with separation of pure higher esters and alcohols, which, like ethanol, can be used as raw material for the chemical industry. 5.- Device for applying the method described in claim 1, characterized in that it consists at least of: —- a storage tank {3} for the residual product {2} in which, in addition to separated ethanol, also higher alcohols and flavoring aromatics such as polyphenols from wine or noparcomates from beer; - a conduit {4} connecting the outlet (5) of the storage tank (2) with the inlet (6) of a rectification column (7), which conduit (4) passes through a heat exchanger {8}; ; 5 - a rectification koion {7} consisting of a | rectification zone {5) and a vapor stripping zone {10}; - a reflux circuit {11} consisting of a pipe {12) | connecting the drain (123) at the top of the rectification zone (92) TG connects to the feed of a condenser (143, from a line (15) which carries the enriched pure ethanol fraction in liquid state from the condenser (14! to a separation tank {L6) in which the liquid enriched pure ethanol fraction (22) is separated from the above gaseous phase, and from a conduit (17) which returns the above vapor phase for reflux to the rectification zone {9} at the top of the rectification chamber {7); - a line {18} connecting the outlet {19} of the separation tank {16} with the inlet (20) of a storage tank (21) for the enriched pure ethanol fraction {22}; 23 - a vapor stripping loop (23) consisting of a conduit {24) feeding vapor from a recoke circuit (25) to the vapor stripping zone (10) in the rectification column {7}, and a conduit {26) carrying condensed liquid aroma concentrate at the bottom of the vapor stripping zone (10) passes in liquid state to the reboiler (25) where the liquid aroma concentrate is reboiled to form vapor which is fed back to the vapor stripping zone {10} via line (24); - a pipe (27) connecting the discharge {28} for enriched liquid aroma concentrate at the bottom of the reboiler (25) to a storage tank (29) for enriched liquid aroma concentrate {30}, which pipe (27) through the heat exchanger {58} Icopt: id - three variable speed pumps controlled by a level control unit {31} which is connected to a level sensor (32), one of which is pump (33) in the counter-boiler (25) which pumps the level of liquid enriched pure aroma concentrate in the recoke kettle (25) constant and transfer the excess liquid fortified pure flavor concentrate to the covan tank 29 for pure flavor concentrate 30; a second pump {33} in the separation vessel (16), which pump keeps the level of the enriched pure ethanol fraction in the separation vessel (16) constant and discharges the excess liquid enriched pure ethanol fraction to the receiving tank {21} for the enriched pure ethanol fraction (22 ); and a third pump {33%} in the line {26} which keeps the level of liquid fortified aroma concentrate constant at the bottom of the vapor stripping zone {10}. - Two pumps with variable speed, controlled by a flow control unit {34} connected to a flow sensor (35), of which one pump (36) keeps the flow rate constant of residual product {2} through pipe (4} to the rectification column { 3}, and a second pomo (36°) keeps constant the flow rate of the gaseous phase of the enriched pure ethanol fraction through the line {17} to the rectification zone (9) of the rectification column {7} for the purpose of refluxing. Device according to claim 5, characterized in that | this tocelate to maintain a continuous process with sen ; constant Loevoer of residual product (2) and a constant | discharge of aroma concentrate {30} for addition to the now non-alcoholic alcoholic drink, so that this drink retains its taste and aroma,