CZ88793A3 - Membrane method of removing alcohol from a natural fermented beverage, and apparatus for making the same - Google Patents

Abstract

Dealcoholization of a naturally fermented beverage comprising: A) optionally, contacting the beverage with a microfiltration membrane, to obtain a permeate and a retentate with, respectively, lower and higher concentrations of high molecular weight turbidity causing compounds; B) optionally, contacting beverage or the microfiltration permeate with a nanofiltration membrane, to obtain a permeate and a retentate with, respectively, lower and higher concentrations of aroma and flavor containing compounds, C) contacting the microfiltration permeate or the nanofiltration permeate with a reverse osmosis membrane, which selectively permeates ethanol and selectively retains aroma and flavor containing compounds, to obtain a permeate and a retentate with, respectively, higher and lower concentrations of ethanol, and lower and higher concentrations of aroma and flavor containing compounds.

Description

(57) A method of removing alcohol from natural fermented beverages, comprising (A) optionally contacting the beverage raw material with a microfiltration membrane to form a permeate and a retained fraction having a lower and lower fraction, respectively. (B) optionally contacting the beverage material or permeate from the microfiltration with the nanofiltration membrane to form a permeate and a retained fraction with a lower or lower fraction, respectively. higher concentration of flavorings and flavorings. (C) contacting the permeate from the microfiltration or the permeate from the nanofiltration with a reverse osmosis membrane which selectively permeates ethanol and selectively retains the aroma-forming and flavor-forming compounds to form a permeate and a retained fraction with a higher and higher resp. lower ethanol concentration and lower resp. higher concentration of flavorings and flavorings.

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A membrane process for removing alcohol from a natural fermented beverage and apparatus for carrying out the process.

Technical field

The invention relates to a two-stage and three-stage membrane process for removing alcohol from natural fermented beverage products. In addition, the present invention relates to a system suitable for carrying out these processes.

BACKGROUND OF THE INVENTION

Non-alcoholic beverages and low-alcoholic fermented beverages, such as different types of beer or wine, have recently become of great interest as these beverages provide the traditional taste and aroma of beer and wine without showing the unhealthy and socially adverse side effects of alcohol content. In addition, it should be noted that many people are increasingly interested in their caloric intake, which means that their interest is focused on low-calorie drinks and foods. It follows from the above that lower calorie alcoholic beverages have become increasingly popular in recent times. The main source of caloric content in beer and wine is the alcohol content of these beverages, so it is desirable and desirable to produce low alcohol and non-alcoholic beer and wine, while maintaining the taste and aroma of beer and wine.

Low-alcohol beer and wine and non-alcoholic types of beer and wine have been on the market for many years, but the methods applied in the production of these types of beer and wine cause undesirable taste and bouquet.

For example, the alcohol from these beverages may be oddesxilovax, but in xomxo posxup, the beer or wine is brewed or at least denatured, with most of the taste and aroma-generating substances being removed or converted. According to another mexico, alcohol reduction is achieved by dilution with water. These modifications, however, manifest themselves in weak chuxi, which can be assumed when diluting beer or wine with water.

According to the prior art, several methods of removing or lowering alcohol levels exist in natural fermented beverages in which a membrane separation step is used or included. U.S. Pat. No. 4,499,117 to Bonneau describes a three-step process consisting of a first step, a nanofiltration using a nanofiltration membrane separating a fraction of substances having a molecular weight of about 10,000, followed by a second step, a single-step process. reverse osmosis processing ultrafiltration permeate, using a Degremont-type reverse osmosis membrane made of aromatic polyamide hollow fibers, which exhibits a separation of the fraction of substances having a molecular weight of approximately 250. The next step is permeate from the reverse osmosis step is subjected to vacuum distillation using a pressure of about 0.015 MPa and a temperature of about 45 ° C. The product of this process is a retained fraction of the three steps, which is then recombined in the subsequent phase. With respect to this process, it should be noted that a significant proportion of the flavorings and flavorings pass through the membrane used to carry out the reverse osmosis, which is then subjected to distillation treatment in the next step. In the temperature range of approximately 45 ° C, these flavorings and flavorings are negatively altered, thereby deteriorating the taste and bouquet of the final beverage thus prepared.

U.S. Patent No. 4,612,916 to Goldstein discloses the use of a reverse osmosis membrane to remove alcohol from wine and malt beverages. Specifically, this patent describes a process whereby the beverages can be prepared by subjecting a traditionally prepared beverage ingredient to conventional reverse fermentation using a conventional thin-film composite membrane having a polyamide active layer on a microporous polysulfone carrier material. This membrane retains the volatile substances and other flavor components of the beer and allows 25% to 30% of the alcohol contained in the beverage to pass through the membrane. This Goldstein patent compares composite thin film membranes with cellulose acetate membranes, demonstrating that 99% of flavor and flavoring agents are retained when using a thin film of the composite membrane, while using an asymmetric membrane for only about 16% of these volatiles are retained by the cellulose acetate base.

U.S. Pat. No. 4,441,678 discloses the use of nanofiltration for both grape juice and fermented wine product prepared from the juice. According to this patent, grape juice and wine are passed through a membrane separating a fraction having a molecular weight ranging from 175 to 200 to separate the methyl anthranilate and other objectionable flavor components contained in the Labrusca grape.

In United Kingdom Patent No. 2,133,418. by Keufner, published July 25, 1984, discloses a process for concentrating beer and wine, wherein xyxo beverage ingredients are passed through a reverse osmoxic semipermeable membrane, and water is added to the product to form a reconsixed beverage. With this water used for reconixing, reverse osmosis water can be used to remove 99% of the mineral constituents. The membrane is a thin composite film on a polymeric carrier material. The reverse osmosis system operates at xeplox ranging from about -2 ° C to about 40 ° C and at a pressure ranging from about 689.5 kPa to about 758.5 kPa using non-oxidizing axmospheres produced by the use of carbon dioxide. The water used for reconixing is only added after the reverse osmosis process has been completed. In the xohoxo paxenx posxup, approximately 45% alcohol and 75% water from the processed beer can be removed. The resulting beer contains 2.3% of Hx-Oxx alcohol. Of the x5 samples produced, one had a slight after-burn flavor when flavored and the other sample was poor in taste, suggesting that upon dilution, the final product did not produce a sufficient amount of essential ingredients. Beverages prepared according to xohoxo paxenx can be characxerized as light beers with low alcohol content.

According to Belgian Paxenx No. 717,847 (December 1968), owned by the Guinness Company, a reverse osmosis and non-oxidizing axmosphere method is used to produce a concentrate, which is then transported to a destination where the alcohol produced there is reconstituted. Preferably, the cellulose acetate membrane of U.S. Pat. No. 3,133,132 is used in the process. Also disclosed is the possibility of using a polyvinyl acetate and polyacrylate membrane. According to this patent, a process is carried out in which the beverage is reconstituted only after being transported with an equal volume of alcohol and water or with water alone, thereby obtaining a non-alcoholic or almost non-alcoholic beverage.

United Kingdom Patent 1,447,505 protects a process for producing beer with a reduced alcohol content, a low alcohol content or without alcohol. This patent describes a process for removing alcohol from beer using a membrane system that is used in a batch type concentration system in which the beer processed therein is diluted with water either before or immediately after the process. However, this process has drawbacks due to the very nature of the process, since it changes the concentration of other complex constituents present in beer, leading to the likely formation of precipitates as well as other constituents that could clog the membrane. used in this procedure. It can be seen from the above that precipitates and / or membrane contaminants not only adversely affect the taste of beer, but also reduce the productivity of the membrane system. In addition, it should be noted that this process is carried out at relatively high pressure in the system.

U.S. Patent 4,617,127 to Light discloses a process for preparing low alcohol beverages by passing a high alcohol beverage ingredient through a reverse osmosis system in which a membrane portion is obtained (permeate) and fraction retained on the membrane (retentate). The membrane passage contains mainly alcohol and water and is discharged from the system. A small fraction of the retained fraction is separated as product, the major fraction being recycled to the reverse osmosis system and mixed with the fresh beverage material and the added water. Reference is also made to paxenx of United States Patent No. 4,717,482.

U.S. Pat. No. 4,888,189 to Gnekow discloses a simulxane reverse osmosis dual-process process for the preparation of beverages, in particular various types of wine, having a reduced alcohol content, the starting materials of which are used. They are any type of commonly obtained fermented sxol wines. All of the xéxo portion of the starting wine stock is subjected to reverse osmosis treatment to dehydrate alcohol and water, the latter being removed as permeate, and recycling the concen- trated retentate (rexenxax) while simultaneously feeding the water feed from the feedstock tank simultaneously or alternately. reverse osmosis to balance the total volume and maintain the original level of the raw wine stock in the xéxo tank. The final wine beverage thus obtained has an acceptable taste, bouquet and concentration of coloring solids for normal commercial use. This process can be carried out by a batch process or a modified semi-continuous process, whereby non-alcoholic wines (i.e., wines with a residual alcohol content of less than

0.5% by volume) or wines with a reduced alcohol content (i.e., an alcohol content of less than about 11 to 13% by volume).

These prior art processes have some disadvantages. Firstly, when using a reverse osmotic membrane, such as a cellulose acetate membrane, in the open environment, the passage of the beverage raw material through the membrane results in a significant loss of aroma-forming compounds. In an alternative embodiment of these processes, using relatively high density membranes, such as a thin film composite type membrane, the process capacity achieved is low because large molecular weight compounds tend to clog the membrane and reduce its efficiency. These high molecular weight compounds include proteins, betaglycans, polysaccharides, and polyphenol complexes. This phenomenon essentially means a reduction in the liquid flow through the membrane and a lower alcohol permeability. As a result, higher amounts of deionized water are required. In other processes, the fermented beverage raw materials are exposed to high temperatures or high pressures, both of which may destroy compounds that produce a characteristic taste and aroma, thereby deteriorating significantly the final taste and acceptability of the final beverage obtained.

It is clear from the above that there is a need in the art for a process that economically removes ethanol from natural fermented beverage raw materials while maintaining the flavor and aroma-forming compounds of the beverages. Further, there is a need to develop a process that avoids damage and destruction of flavor and taste-generating compounds by heat or pressure. In addition, there is a need in the art to devise a process that does not reduce the efficiency of the membrane used, for example by clogging the membrane while reducing the flow rate, and thereby compromising the economic performance of the process.

Another problem in the preparation of various types of beer and wine is the presence of a lax substance causing cloudiness of the beverage. Usually, xemox compounds are high molecular weight compounds that settle in xyxo natural fermented beverages after being bottled. It has been found in the prior art that xemo compounds of high molecular weight that cause haze are proxeins and bexaglycans, and xyo compounds of high molecular weight may adversely affect the taste of the final beverage. It follows from the above that there is also a need in the xomxo art to develop a low alcohol beverage preparation process to obtain a final beverage containing no xyxo haze-causing compounds.

SUMMARY OF THE INVENTION

All xyxo of the aforementioned aspecxy meets the posxup of the present invention. The present invention relates to a method for removing alcohol from natural fermented beverages, comprising the following steps:

(A) optionally conducting a microfilter, contacting a feedstock feedstock stream containing a natural fermented beverage with a microfiltration membrane having a pore size in the range of 0.1 to 1.0 gm under conditions where the feedstock stream is divided into the fraction released by the microfilxing membrane having a lower concentration of high molecular weight haze-inducing compounds and the fraction retained by the microfilxing membrane having a higher concentration of high molecular weight haze-inducing compounds compared to the feedstock feed stream introduced into the microfiltration, (B) optional carrying out a nanofiltration contacting a feedstock feed stream comprising a natural fermented beverage or a portion passed through a microfiltration membrane with a nanofiltration membrane that separates the molecular fraction from 100 to 10,000, under conditions where the nanofiltration feed stream is divided into a nanofiltration membrane pass having a lower concentration of flavor and flavor compounds and a nanofiltration membrane retained with a higher concentration of flavor and flavor compounds (C) contacting a feedstock feed stream comprising a microfiltration membrane passage or a nanofiltration membrane passage with a reverse osmosis membrane that selectively permeates ethanol and selectively retains stannic and aroma-providing compounds compared to the nanofiltration feedstock feed stream; under conditions where the feed stream introduced into the reverse osmosis phase is divided into a fraction passed through the reverse osmotic membrane having a higher ethanol concentration and a lower content of compounds forming aroma and stilts, and the fraction retained by the reverse osmosis membrane having a lower ethanol concentration and a higher proportion of flavor and stilt-providing compounds, as compared to the feed stream fed to the reverse osmosis phase, the principle of the present invention being it necessarily carries out both said steps (A) and (B) or one of these steps, and in the case of sxupene (B), the proportion retained in reverse osmosis and the proportion retained in nanofiltration are recombined in the subsequently performed sxupni (C) .

The invention also relates to an apparatus for carrying out the aforesaid procedure. The method claimed in the xohoxo invention and the apparatus for performing the xohoxo method allow the preparation of natural fermented beverages without deoxidizing or destroying flavor-providing flavors. Further, it is noted that in the practice of the present invention, compounds that cause turbidity and negaxly affect the chux of the resulting product are removed. In addition to this, it is also desirable that the posxup and the apparatus of the present invention anticipate economic means to achieve the above objectives.

In the following description, definitions of some xermins used in the xomho description will be given, which are appropriate for clarification of the xohoxo of the invention. Natural fermented beverages in xomxo xexx mean drinks prepared by fermentation of naturally occurring starting materials. Among the xyxo natural fermented beverages can be included various types of wine, beer, English top fermented top types of beer, types of beer with a higher alcohol content, types of pear cider and similar other beverages.

Separation of the fraction with a specific molecular weight is xermine, which is used to characterize the membrane when retaining molecules of known size. Capturing or separating a molecular moiety with a molecular moiety predisposes the xac separation of a specific molecular moiety fraction, with at least 90% of the spherically elecxroneuxal molecules of the given molecular moiety being retained by the porous membrane while less than about 50% of the molecular weight is retained. By feedstock is meant the starting material to be treated by the process of the invention, which is fed to the membrane, which material may optionally contain recycled concentrate or the feedstock may be a mixture of the two materials. The result of the membrane separation process is the production of two liquid fractions, i.e. a fraction which passes through the membrane (permeat) and a fraction which is retained by the membrane and does not pass through the membrane (retentate). A permeate or moiety that passes through a membrane is a liquid and substances that are dissolved, suspended or otherwise contained in the liquid that permeates through the membrane. A retentate or moiety that is retained by a membrane is a liquid, including substances dissolved, suspended and otherwise contained in a liquid that does not pass through the membrane. In this context, it should be noted that flavorings and flavorings as used herein are meant to mean certain organic compounds which are contained in natural fermented beverages and which create a characteristic flavor and taste in the natural fermented beverage, including, for example, such compounds as propanol, higher aldehydes, acetates and ethers. These compounds also include n-propanol, ethyl acetate and isoamyl alcohol.

By the above haze-forming compounds is meant very high molecular weight proteins and betaglycans which tend to precipitate in the natural fermented beverage during settling. In general, they are compounds having a molecular weight of more than 200,000.

There are several ways to carry out the process of the present invention. The reverse osmosis phase must be performed in all cases. Either a microfiltration step or a nanofiltration step must be performed prior to reverse osmosis.

In certain cases, there may be situations where both steps need to be performed. The choice of the method used depends in each particular case on the economic side of the process and on the nature of the natural fermented beverage raw material processed by the selected process. Any person skilled in the art will be able to determine which method is most economically and technically appropriate for a particular case and for a particular feedstock to be processed.

When a nanofiltration step is used, the retentate moiety is combined with the reverse osmosis retentate to provide a reconstituted beverage containing substantially all flavor and flavor compounds while reducing ethanol concentration.

In one embodiment of the process of the present invention, the first fermented beverage raw material is first fed to a microfiltration membrane having a pore size in the range of 0.1 to 1.0 micrometer, under conditions where the retentate in the membrane contains a high concentration of compounds causing haze, such as high molecular weight proteins and betaglycans. The fraction released through this membrane contains a natural fermented beverage with a significantly reduced concentration of haze-producing compounds as compared to the feedstock. In a further phase of the process, the microfiltration membrane (permeate) fraction is fed to a nanofiltration membrane which separates the fraction having a molecular weight ranging from 100 to 10,000 under conditions in which the permeate has a high concentration of water and ethanol and a retained fraction (retentate) has a high concentration of flavorings and flavorings.

In a further stage of the process, the nanofiltration membrane permeate is introduced onto the reverse osmosis membrane under conditions where ethanol is selectively permeated through the reverse osmosis membrane, the retention rate on the reverse osmosis membrane having a substantially lower ethanol concentration.

In the final stage of the process, the natural fermented beverage raw material, either without ethanol or with a significantly reduced concentration of ethanol, is then reconstituted by combining the retentate from the reverse osmosis stage with the retentate from the nanofiltration process and possibly also with water.

In a further embodiment of the process, the natural fermented beverage raw material is fed to the microfiltration membrane in the same manner as above to obtain a retained fraction with a high concentration of high molecular weight haze compounds and a leaked fraction of the natural fermented beverage raw material with a significantly reduced concentration. haze compounds as compared to the feedstock. The fraction released in this microfiltration step through the microfiltration membrane is fed to the reverse osmosis membrane under conditions where ethanol is selectively passed through the reverse osmosis membrane, the retentate on the reverse osmosis membrane comprising a natural fermented beverage with a lower ethanol concentration compared to the feedstock feed to the membrane to carry out this reverse osmosis. Optionally, water can be added to the retained portion of the reverse osmosis membrane to replace the volume of liquid that passes through the reverse osmosis membrane.

According to another embodiment of the process, the natural fermented beverage raw material is fed to the nanofiltration membrane under conditions where the fraction permeated by the membrane has a higher ethanol concentration than the retention fraction on the membrane, the fraction retained on the nanofiltration membrane having a higher concentration of aroma-forming compounds and flavorings compared to the feedstock feedstock. In a further stage of the process, the nanofiltration membrane permeate obtained in the nanofiltration stage is fed to the reverse osmosis stage under conditions where the membrane osmosis permeation stage has a higher ethanol concentration than the feedstock and the retention of the reverse osmosis stage. it has a considerably lower ethanol concentration compared to the feedstock.

In a further stage of the process, the retentate on the nanofiltration membrane and the retentate osmosis retentate are recombined or water recombined to produce a reconstituted natural fermented beverage containing substantially all flavorings and flavorings, while substantially lower ethanol concentration in this beverage.

In the process of the present invention, the microfiltration step is intended to remove high molecular weight haze-inducing compounds that do not contribute to the flavor or flavor, or which remove the flavor and flavor contributing substances in these natural fermented beverages. By microfiltration is meant a process in which high molecular weight compounds are removed by passing this natural fermented beverage through a membrane that acts as a filter for said high molecular weight compounds. The term microfiltration, which is used in the art of preparing different membranes, has different meanings for those skilled in the art. In general, this refers to the separation of high molecular weight species from a fluid stream by passing the stream through a membrane of a certain pore size, the pore size being relatively large. The differences in the definition of this microfiltration between the various persons skilled in the art result from the determination of the lower pore size threshold of the membrane to perform this microfiltration. As mentioned above, the term microfiltration in the present specification refers to an embodiment of the microfiltration process using a membrane having a pore size in the range of 0.1 to 1.0 micrometer. Membranes suitable for carrying out the microfiltration step of the present invention are well known in the art. These membranes are usually homogeneous membranes or asymmetric porous membranes prepared from a polymeric material inert to the processed fermented beverage raw material and having sufficient chemical resistance and morphological strength to withstand the conditions under which the process is carried out. These membranes may be prepared from polyolefins such as polyethylene or polypropylene, polycarbonates, halogenated polycarbonates, fluorinated polyolefins such as polyvinylidene fluoride, polysulfones and polyethersulfones. Preferred materials for the purposes of the present invention are polysulfones, polyethersulfones and fluorinated polyolefins.

Even more preferred materials for preparing the microfiltration membranes of the present invention are polyvinylidene fluoride and polysulfones. Typically, homogeneous membranes are used as microfiltration membranes having a pore size in the upper region of the above pore size range. On the other hand, asymmetric membranes are usually used as microfiltration membranes having a pore size in the lower region of the above pore range.

In carrying out this microfiltration step, the starting feedstock on the microfiltration membrane is a natural fermented beverage material such as wine, beer, a type of English fermented top beer, a beer with a higher alcohol content and the like. This feedstock is divided into two portions, i.e., a retentate containing a higher concentration of high molecular weight haze-causing compounds, such as proteins and betaglycans, compared to the feedstock. The fraction discharged through the microfiltration membrane comprises a natural fermented beverage with a lower concentration of these higher molecular weight compounds causing turbidity compared to the feedstock, the fraction further comprising water, ethanol, flavorings and flavorings. For the purposes of preparing a low-natural fermented beverage, this retained fraction is of no importance. The fraction released by the microfiltration membrane is used as feedstock for the next phase of the process.

The feedstock is contacted with the membrane at a pressure sufficient to release the perraeate through the membrane. At this stage, it is necessary to use a crayfish burst that is sufficient to provide sufficient driving force and to push the permeate through the membrane, as well as to retain on the membrane the desired volatile substances, such as carbon dioxide, contained in this natural fermented beverage. On the other hand, the applied pressure must not be so high as to cause undesirable clogging of the membrane. If too high a pressure is used at this stage, the high molecular weight compounds are pushed onto the membrane, which may mean that they remain on the membrane and this will result in reduced membrane flow and inefficiency of the process. Preferably, the pressure applied is in the range of about 0.2 MPa to about 0.35 MPa. More preferably, the applied pressure is in the range of about 0.3 MPa to about 0.35 MPa. In order for this membrane process to function effectively, there must be sufficient driving force to force the permeate to pass through the membrane, typically the driving force being the difference in pressure upstream and downstream of the membrane, commonly referred to as transmembrane pressure. Preferably, the transmembrane pressure is greater than 0.05 MPa.

When the natural fermented beverage material is a beverage containing carbon dioxide, such as beer, the minimum pressure required to retain the carbon dioxide in the beverage is 0.175 MPa. Preferably, the transmembrane pressure in this case is 0.3 MPa or less. The temperature used in this process can have a considerable effect on the final taste and aroma of the beverage thus obtained. In cases where too low a temperature is used, these flavorings and flavorings may freeze or the flavorants and flavorings may precipitate in the beverage. If too high temperatures are used again, these flavorings and flavorings may be damaged. Preferably, the temperature for the process is in the range of about 2 ° C to about 10 ° C, most preferably in the range of about 2 to about 8 ° C. The flow rate released through this membrane is a very important characteristic of this process as it affects the economic side of the process. Preferably, the flow rate is in the range of about 100 liters per m / hour to 3000 liters per m / hour. Usually, high permeate flow rates through the membrane are started in the process according to the invention and after a certain period of time this level decreases, for example after 1 to 2 hours. Preferably, the permeate flow rate through the membrane after 2 hours of operation is in the range of about 100 to about 500 liters per m / hour, and more preferably in the range of about 200 to 250 liters per m 2 / hour.

Typically, these membranes are preferably arranged in membrane modules. The arrangement of these modules is well known in the art. In a preferred embodiment, it is a spiral wound membrane device or a plate membrane device in a frame configuration.

The second step of the process of the invention is a nanofiltration step. The purpose of this nanofiltration step is to trap the average molecular weight substances that correspond to the flavor and flavor compounds, and to separate them from the process stream in such a way that the average molecular weight flavor and flavor compounds do not clog the reverse osmosis membrane in the and a reverse osmosis step. By avoiding clogging of the membrane used for reverse osmosis, a higher flow through the reverse osmosis membrane and thus more economical implementation of this reverse osmosis is achieved. The decision whether or not to carry out this nanofiltration step depends on the evaluation, on the one hand, of the operating costs additionally incurred as a result of the membrane fouling used to carry out reverse osmosis when this nanofiltration is not used, and use of this nanofiltration step. A further advantage of using this nanofiltration step is that it reduces the osmotic pressure to be overcome when performing the reverse osmosis step, thereby reducing the pressure to be applied to the feedstock in this step.

By said nanofiltration membranes is meant in this step membranes separating a fraction having a molecular weight in the range from 100 to 10,000, most preferably membranes separating a fraction having a molecular weight in the range from 100 to 1000. In a typical embodiment, the nanofiltration membrane is an asymmetric membrane with a pore size. adequate separation of the molecular weight substances listed above.

These membranes are well known in the art and can be prepared from cellulose acetates, regenerated cellulose acetate, aliphatic polyamides, aromatic polyamides and polyvinyl alcohol. Preferably, the membranes are prepared from cellulose acetate, aliphatic polyamides, regenerated cellulose acetate or polyvinyl alcohol.

In an even more preferred embodiment, the xyxo membranes are prepared from cellulose acexax or aliphaxic polyamides. The tyso membranes may also be in the form of a thin composite film descending from a thin film by a selective layer on a porous asymexric carrier maxerial. The taxo-porous asymexric carrier layer may be prepared from a polyolefin, a halogenated polyolefin, such as fluorinated polyolefins, polycarbonates, polysulfones or polyexhersulfones. In a preferred embodiment of the present invention, the carrier maxerial is polysulfone, polyexhersulfone, and fluorinated polyolefins such as polyvinylidene fluoride. Said selective layer may be a xixix thin film of polyurexane, hydroxyalkylcellulose, polyvinyl alcohol or polyamide deposited on a carrier maxerial. According to a preferred embodiment, the xenox film is formed by the interfacial reaction product of a difunctional or xrifugal aromax acid halide or a mixture of xenox compounds with a difunctional or xifunctional polyamine, such as piperazine or subsxixed piperazine. An example of many membranes is found in paxenxes of the United States of America No. 4,259,183, whose auxor is Cadoxxe, No. 4,769,148, whose auxor is Fibinger, No. 4,619,767, whose auxor is Kamiyama, and No. 4,769,148.

595 139, whose auxor is Uemura, and all xyxo paxenxy pre-xxs only reference maxerials. These nanofiltration membranes are usually arranged in membrane modules. Several x and y membrane assemblies are known from the prior art, such as, for example, plate membrane devices in a frame configuration, spiral vinux membranes, duxé membrane xrubs and duxá fibers. The selection of the xyxo membrane modules for concrex use depends on the process being performed. It will be easy for those skilled in the art to determine which membrane arrangement will best suit the requirements of the process being performed. In a preferred embodiment of the invention, spiral wound diaphragm modules or plate diaphragm modules are used in a frame configuration.

The feedstock feedstock for the nanofiltration stage is either a natural fermented beverage or a fraction released in the microfilter stage. The initial feed stream is divided into a retained portion having a high concentration of flavor-forming and flavor compounds as compared to the feed stream as well as a lower ethanol concentration compared to the feed stream. The fraction passed through the nanofiltration membrane represents a stream with a higher concentration of ethanol and a lower concentration of flavorings and flavorings compared to the feed stream.

In the membrane process, complete separation is seldom achieved, so it is advisable to recycle the retained portion back to the feedstock fed to the nanofiltration membrane or further treat the retained portion by feeding this portion to further nanofiltration membranes to further reduce the ethanol content of the stream. In this context, it should be noted that the feedstock onto the nanofiltration membrane may contain, in addition to the discharged fraction from the microfiltration stage or the natural fermented beverage raw material, a retained fraction that has been recycled from the previous nanofiltration stage or possibly water treatment.

In a preferred embodiment of the present invention, sufficient feedstock pressure applied to the nanofiltration membrane is used to provide sufficient driving force to effect the permeate extrusion through the membrane.

If the feedstock pressure is too low, the generation of sufficient driving force to push the permeate through the membrane will not be achieved, and if the feedstock pressure is too high, the membrane may become clogged, thereby reducing the flow through the membrane and thereby reducing the economic benefits of the process. In a preferred embodiment of the invention, the lower pressure used is about 3 MPa. In a preferred embodiment, the upper pressure is about 6 MPa. Even more preferably, the upper pressure value is about 4 MPa. Typically, the transmembrane pressure value must be sufficient to provide sufficient process driving force. Since this transmembrane pressure is a function of the feedstock pressure used, the membrane becomes clogged if the transmembrane pressure is too high. Preferably, the lower limit of the transmembrane pressure is 2.8 MPa. Preferably, the upper limit of the transmembrane pressure is 5.8 MPa, most preferably 3.8 MPa. The flow rate of the liquid passing through the membrane must necessarily be sufficient to make the process economical.

If the flow rate is too small, the process is difficult to carry out, there is insufficient separation and the membrane may become clogged. If the flow rate is too high, then the energy consumption is too high and the process becomes uneconomical. In a preferred embodiment of the invention, the lower limit of the flow rate is about 50 liters per m < 3 > / hour, more preferably 200 liters per m < 2 > / hour. Preferably, the upper limit of the flow rate is about 300 liters per m < 2 > / hour, and more preferably the flow rate is 300 liters per m < 2 > / hour. The temperature used in the process is the same as mentioned above for the microfiltration step.

Since membrane separation rarely results in precise separation of the components, it is desirable to further concentrate the retained portion either by recycling the retained portion as feedstock into the nanofiltration process or by guiding this portion through one or more further nanofiltration membranes arranged in series. In the case where a series of nanofiltration membranes is used, the retentate can be introduced onto one or more other nanofiltration membranes, the number of which is selected to achieve the desired level of ethanol in the retentate. If the retained portion is recycled, it can be recycled directly into the feed line or recycled to the storage tank. Preferably, the nanofiltration process is carried out in such a way that the feed onto the nanofiltration membrane is collected in a storage tank, whereupon the feedstock is fed directly from the storage tank onto the nanofiltration membrane. When recycled, the retained fraction from the nanofiltration stage is returned to the storage tank. The feedstock collected in the storage tank may be passed through the nanofiltration membrane several times to achieve sufficient concentration of the feedstock on the nanofiltration membrane and to sufficiently reduce the ethanol content of the feedstock. In a preferred embodiment, the concentration is in the range of about 1.5 to about 10, more preferably in the range of about 2 to 3. During the concentration of the feedstock, water may optionally be supplied to the storage tank for those skilled in the art. the amount of water possibly added is readily determined in the art. In a preferred embodiment of the invention, the amount of water added is such that it corresponds to the volume passed through the nanofiltration membrane.

The third step in the process of the invention is reverse osmosis, at which point ethanol is removed from the remainder of the natural fermented beverage raw material. In carrying out this step, the particular membrane chosen is selected in such a way as to allow the passage of ethanol in the permeate stream and to prevent the passage of the flavor-forming compounds and flavorings through the membrane. Preferably, the membrane separates a fraction having a molecular weight in the range of about 40 to 100. More preferably, the membrane separates a fraction having a molecular weight in the range of about 40 to 50. In the region above the molecular weight 100, there is usually a significant permeation of flavorings and flavorings through the membrane. Below about 40, there is no significant release of ethanol through the membrane.

Any of the reverse osmosis membranes known in the art and described above with the above permeability characteristics may be used to effect this reverse osmosis. These membranes used for reverse osmosis are well known in the art. In a preferred embodiment of the present invention, thin film composite membranes are formed to provide reverse osmosis and are formed by an asymmetric carrier membrane on which a polymer film is deposited, the polymer film controlling the permeation characteristics of the membrane.

More preferably, the thin film composite membranes comprise a polyamide selective layer made by reacting piperazine or substituted piperazine with a polyhydric acyl halide, and more preferably the thin film selective layer is made of piperazine or substituted piperazine and trimesoyl chloride and optionally difunctional acyl chloride.

These membranes are described in more detail in U.S. Patent 4,259,183, which is incorporated herein by reference.

The feedstock fed to this reverse osmotic membrane depends on what previous membrane separation steps have been performed. In general, this feed forms a permeate either from a microfiltration membrane or from a nanofiltration membrane.

When using both of these embodiments, the reverse osmosis membrane injection forms a microfiltration permeate that has passed through the nanofiltration membrane in the next step. In addition, it should be noted that the feedstock may comprise a recycled retained fraction from the reverse osmotic membrane and further a treatment water which is necessary to maintain the proper course of the process. In general, this separation yields a retained portion with a higher concentration of flavorings and flavorings that have been released in the previous processing steps, as compared to the feedstock. This retained portion has a lower ethanol concentration than the feedstock. The expired fraction consists mainly of water and ethanol, the concentration of this ethanol being higher than that of the feedstock, and a small proportion of flavorings and flavorings, if any.

The required feedstock pressure is considerably lower in cases where there is little risk of fouling of the membrane due to the presence of high molecular weight compounds. In cases where the feedstock pressure is too low, the driving force of the process is not high enough to overcome the permeate side osmotic pressure, causing the amount of permeate produced to be insufficient. In cases where the feed pressure is too high, the membrane becomes too clogged or there is a risk of membrane damage. In a preferred embodiment of the invention, the lower injection pressure limit is about 2.0 MPa or greater, and even more preferably the lower injection pressure limit is about 2.5 MPa or greater. In a preferred embodiment of the process of the invention, the feedstock pressure is 6.0 MPa or less, and even more preferably the pressure is 3.0 MPa or less. The temperature of the xenxo process is about 2 ° C to about 30 ° C, preferably about 2 ° C to about 10 ° C.

If the penetration rate of the membrane is too low, the overall performance of the posxup is uneconomical, and if the xoxo penetration rate is too high, the poxom is compromised by the quality of the distribution of the single moieties. In a preferred embodiment of the present invention, the value of the void amount is in the range of 10 lixers per m / hour to more times, and in a more preferred embodiment the value of the void quantity is 20 lixers per m / hour or greater. Preferably, the xoxo is an amount of about 50 lixers per m @ 2 / hour or less, and even more preferably the xoxo is an amount of liters per m @ 2 / hour or less. In general, when the feedstock is contacted with the reverse osmosis membrane module, one module may sometimes not be sufficient to remove the required amount of ethanol, so that the retention portion may in some cases have a higher ethanol concentration than necessary. To achieve the desired level of ethanol concentration in the retentate, the retentate can be passed through a series of reverse osmotic membranes, or the retentate can be recycled and introduced onto the same reverse osmotic membrane. According to an alternative embodiment, the retentate can be recycled to the feed line and recycled directly to the process, whereby the retentate from the microfiltration or nanofiltration process can be discharged to the storage tank and the retentate from the reverse osmosis process can be added thereto. and bring it to the same storage tank. Optionally, the treatment water can also be fed to this storage tank. The reverse feed osmosis feedstock is then removed from the storage tank. Preferably, the retentate in the reverse osmosis membrane is continuously recycled to said storage tank until the desired level of ethanol in the mixture contained in the storage tank is reached. Preferably, water is added to the storage tank in an amount substantially equivalent to the permeate volume permeated by the membrane to effect reverse osmosis. In general, the extent to which alcohol is reduced depends on the desired product. For example, in Germany, low alcohol beer is defined as containing 2% or less by volume of alcohol, while non-alcoholic beer is defined as containing 0.5% by volume of alcohol. On the other hand, in the UK, low-alcohol beer is defined as beer containing 1.2% by volume of alcohol, while non-alcoholic beer is defined as beer containing 0.5% by volume of alcohol. It can be seen from the above that the required level of ethanol in the final product is different and depends on the classification of the fermented beverage and the country into which the product is imported and sold. In a preferred embodiment, the concentration reduction is in the range of about 2 to 15, more preferably in the range of about 2 to 8.

In one embodiment, it is desirable to concentrate the retained portion of the reverse osmosis that is discharged into the storage tank to some extent before adding the water treatment. According to this embodiment, the amount of water added to the storage tank is less than the amount of permeate that has passed through the reverse osmosis membrane during this concentration. In carrying out the process according to this variant, the amount of treatment water required is less. Preferably, the treatment water is deionized water. This water can be deionized by conventional techniques known in the art, such as diafiltration. Since the production of deionized water is costly, it is necessary to minimize water consumption when carrying out the process of the invention. If a treatment water addition is used in this step, it can be added continuously. In this case, two methods of adding water treatment can be used. According to one embodiment, the water is added to the process in such a way that the flow rate of the membrane-permeable liquid remains constant. According to a second embodiment, the amount of water added is such that a constant volume of liquid in the storage tank is maintained.

When reconstituting the beverage composition, the retained fraction of the nanofiltration process and the reverse osmosis process are recombined. The recombination can be carried out in a batch tank or the recombination can be carried out in a mixer with a cylindrical liquid flow. The purpose of this process is to restore the natural flavor and taste of this processed natural fermented beverage.

Preferably, the feedstock to be treated in the process of the present invention and in the apparatus of the present invention is beer.

The invention also includes apparatus for carrying out the above process. This equipment consists of the following parts:

(A) optionally comprising one or more microfiltration membrane modules in which the membrane has a pore size in the range of 0.1 to 1.0 gm, (B) optionally comprising means for supplying a natural fermented beverage to said microfiltration membrane module, (C) optionally comprising means for removing the fraction retained in the microfiltration from the area of the microfiltration membrane module, (D) optionally comprising means for discharging microfiltration permeate from the area of the microfiltration membrane module, (E) optionally comprising one or more nanofiltration membrane modules in which the membrane separates the fraction; a molecular weight in the range of from 100 to 10,000, (F) optionally comprising means for feeding the natural fermented beverage ingredient or permeate from microfiltration to the nanofiltration membrane module; optionally, nanofiltration from the nanofiltration membrane module region, (H) optionally comprising means for removing nanofiltration permeate from the nanofiltration membrane module region, (I) one or more membrane modules to effect a reverse osmosis containing membrane that is capable of selectively permeate ethanol and selectively retain compounds forming compounds flavors and flavorings contained in natural fermented beverages, (J) means for introducing microfiltration permeate or nanofiltration permeate into the reverse osmosis membrane module, (K) means for removing the portion retained in reverse osmosis from the reverse osmosis membrane module region, ( L) means for removing permeate from reverse osmosis

- -31 from the region of the membrane module for reverse osmosis, the principle being that if parts (A), (B), (C) and (D) are used, then all are used simultaneously, if parts ( E), (F), (G) and (H), then all are used simultaneously and either the set of parts (A), (B), (C) and (D), or the set of parts (E), (F) , (G) and (H), or both, must be present, wherein the apparatus of the present invention is further characterized in that when an assembly of parts (E), (F), (G) and (H) is used, the portion (M) that represents;

(M) means for combining the fraction retained in the nanofiltration and the fraction retained in the reverse osmosis.

In this context, it should be noted that said parts (A), (B), (C) and (D) as defined above constitute an integral unit. Specifically, the portion (B), representing the means for feeding the natural fermented beverage material to the microfiltration module, is only necessary when the microfiltration membrane module is used, in the same way for portions (C) and (D), which are means for discharging the released portion and the retained portion from the microfiltration membrane module. In addition, parts (E), (F), (G) and (H) are also integrally associated. Part (F) relates to means for feeding the feed material to the nanofiltration membrane module, and parts (G) and (H) relate to means for removing the fraction released in the nanofiltration and respiration. retained in the nanofiltration, from said nanofiltration membrane module. As mentioned above in connection with the description of the process of the present invention, the use of either a microfiltration or a nanofiltration membrane module is necessary, i.e. one or both of these modules constituting a set of the above-mentioned parts must always be present. In addition, if a nanofiltration membrane module and its integrated supply and removal means are used, then means to recombine the nanofiltration retentate with the reverse osmosis retentive, i.e., part (M), must be incorporated into the apparatus.

A membrane having a pore size ranging from 0.1 to 1.0 micrometer is included in the microfiltration module. The membrane module can be any prior art microfiltration membrane module. The membrane module may have a configuration of membrane plates in a frame configuration, spiral wound membranes or hollow tubes. In a preferred embodiment of the invention, a spiral wound membrane module or a plate membrane module in a frame assembly is used. These modules are well known in the art and are also readily available on the market. Said means for supplying the natural fermented beverage ingredient to the microfiltration module is typically a conduit in which the necessary valves are further included and preferably a pump of the type generating the necessary feed material pressure to pass the permeate through the microfiltration membrane. . Typically, said means for discharging the fraction retained in the microfiltration from the region of the microfiltration module is an opening in the membrane module and further downstream a conduit for evacuating the fraction retained therein from the module. Typically, said means for draining permeate from the microfiltration module is one or more openings in the membrane module that are connected to a conduit for draining the permeate from the region of the microfiltration membrane module.

The nanofiltration membrane module comprises a nanofiltration membrane which has been described in detail above. The module may have any of the prior art membrane configurations, including hollow fiber, hollow tube, spiral wound and plate membranes in the frame assembly. In a preferred embodiment of the invention, a module with spiral wound membranes or plate membranes in a frame assembly is used. These membrane modules are well known in the art and are also readily available on the market. Typically, said means for supplying the natural fermented beverage material or microfiltration permeate to the nanofiltration module is a feed line or line in which a pump is connected or connected to, which works to compress the feed material to the necessary level to operate the nanofiltration membrane module. this pressure must allow economical permeability of the permeate through said nanofiltration membrane.

Typically, said means for removing the nanofiltration retentate from the nanofiltration membrane region is one or more apertures in the nanofiltration module that are connected to a conduit to drain the retentate from the nanofiltration module region. Typically, the nanofiltration permeate removal means is one or more apertures in the module that are connected to a duct to drain the nanofiltration permeate from the region of the nanofiltration membrane module.

The reverse osmosis membrane has already been described in detail above, wherein said reverse osmosis membrane module is a module comprising engraved membranes. These modules are well known to those skilled in the art, and engraved membranes may be in the form of hollow fibers, hollow tubes, spiral wound membranes, or may be plate membranes in a frame configuration. In a preferred embodiment of the invention, a spiral wound diaphragm and plate diaphragm arrangement is used in the frame assembly. These membrane modules are well known to those skilled in the art and are readily obtainable on the market. Typically, said means for supplying feedstock to the reverse osmosis membrane module is a pipe or conduit, preferably comprising a pump, which compresses the feedstock to a level sufficient to pass the permeate through the reverse osmosis membrane. Typically, said means for discharging the portion retained in reverse osmosis from the region of the reverse osmosis membrane is one or more openings in the reverse osmosis membrane module connected to the duct to drain the retained portion. Typically, the means for draining permeate from the reverse osmosis membrane module is a plurality of apertures in the membrane module connected to a conduit for draining the permeate.

Typically, said means for combining the nanofiltration retentate and the reverse osmosis retentate is either a storage tank, a mixing tank or one of the types of cylindrical flow mixers in which the retentate on the nanofiltration membrane is contacted with the retention osmosis retentate and these proportions are mixed.

Preferably, the apparatus further comprises a storage tank that is adapted to supply permeate from the nanofiltration fed by means of withdrawing nanofiltration permeate from the membrane module area to conduct nanofiltration or microfiltration permeate fed by means of withdrawing microfiltration permeate from the microfiltration membrane area. module. According to this embodiment, the apparatus of the invention further comprises means for transporting the contents from the storage tank to the reverse osmosis membrane module, means for recycling the portion retained in reverse osmosis to the storage tank, and means for adding water to the storage tank to adjust some or all of the volume permeate from reverse osmosis.

In this embodiment, where a storage tank is used to prepare feedstock into the reverse osmosis membrane module, permeate from the microfiltration membrane module or nanofiltration membrane module is fed to the storage tank by means of permeate withdrawal from the microfiltration membrane. membrane module or nanofiltration membrane module. The storage tank is connected to the reverse osmosis membrane module by means for transporting the contents of the storage container to the reverse osmosis membrane module. These means are connected to means for introducing the feedstock into the reverse osmosis membrane module. In fact, the means for transporting the contents from the storage tank to the reverse osmosis membrane module are closely related to the means for feeding the feedstock to the reverse osmosis membrane module, the two means usually forming a connecting pipe in which it is preferably included suitable pump. Said means for recycling the retained fraction from the reverse osmosis to the storage tank are connected to the means for discharging the retained fraction from the membrane module to effect the reverse osmosis. The system may be a plurality of interconnected conduits, which conduits are connected to openings in the reverse osmosis membrane module to drain the retained fraction from the module. The means for supplying the treatment water to said storage tank consist of a source of the treatment water and a conduit for transporting the treatment water to said storage tank. The conveyor for conveying the treatment water may be connected to the means for recycling the retained fraction from the reverse osmosis, or the treatment water may be discharged directly to said storage tank.

According to another embodiment, the apparatus of the present invention further comprises a storage tank adapted to collect the feed to the nanofiltration membrane, which comprises a natural fermented beverage material or a permeate from the microfiltration membrane module. The apparatus may further comprise means for recycling the fraction retained on the nanofiltration membrane to said storage tank. In addition, the device may optionally further comprise means for transporting the contents from said storage tank to the nanofiltration membrane module as well as means for transporting the concentrated containment contained in the storage tank to the means for combining the nanofiltration retained and reverse osmosis retained. According to this embodiment, the feedstock into the nanofiltration membrane module is introduced into a storage tank. In an embodiment where a microfiltration membrane module is used, the permeate removal means from the microfiltration module can be connected directly to said storage tank, whereby the permeate from the microfiltration membrane module is discharged directly into said storage tank. Said means for recycling the nanofiltration retentate to the storage tank are closely related to the nanofiltration retentate removal means from the nanofiltration membrane module. These means represent an interconnected piping system for guiding the fraction retained during nanofiltration from the nanofiltration membrane module to the storage tank. In addition, it should be noted that the means for transporting the contents of the storage tank to the nanofiltration membrane module are in close association with the means for feeding the feedstock to the nanofiltration membrane module, and these means usually represent a piping system in which a pump for compressing the feed raw materials fed to this nanofiltration membrane module. In this embodiment, the device of the invention further comprises means for transporting the concentrated nanofiltration retentate contained in the storage tank to the means for combining the retentate on the nanofiltration membrane with the retentate on the reverse osmosis membrane. The means is preferably a conduit that connects the storage container to the means used to combine the two retained portions.

In one embodiment, the means for discharging the microfiltration permeate from the region of the microfiltration module is in close association with the means for feeding the feedstock to the nanofiltration membrane module. These means are usually formed by a piping system, preferably with a pump in place, for discharging the microfiltration permeate into the nanofiltration membrane module. In another embodiment, the means for draining the microfiltration permeate from the area of the microfiltration membrane module may be connected to the means for feeding the microfiltration permeate or feedstock to the membrane module for performing reverse osmosis. These associated means can usually be connected to a piping system, preferably a downstream pump, which serves to transport the microfiltration permeate to the reverse osmosis membrane module. According to another embodiment, the means for draining the permeate from the nanofiltration membrane from the region of the nanofiltration module can be combined with the means for feeding the feedstock onto the membrane for performing reverse osmosis. These associated means typically form a conduit or duct system, preferably with a pump in place, for introducing the feedstock into the reverse osmosis membrane module.

DETAILED DESCRIPTION OF THE INVENTION

The apparatus of the present invention will be illustrated in detail with reference to the accompanying drawings, which will also show the process for removing alcohol from the natural mashed beverage raw material of the present invention, consisting of a microfiltration step, a nanofiltration step and a reverse osmosis step. The detailed embodiments shown in these figures do not limit the scope of the invention.

Briefly, Figure 1 illustrates an apparatus of the present invention comprising the above three steps, i.e., microfiltration step, nanofiltration step, and reverse osmosis step, further showing recycling of the retained fraction from the nanofiltration membrane module and recycling the retained. % of the reverse osmosis membrane.

Figure 2 illustrates an apparatus in which the nanofiltration and reverse osmosis steps are used and the process of the present invention is carried out according to this variant, wherein the retained fraction of both steps is recycled.

FIG. 3 illustrates an apparatus in which the microfiltration and reverse osmosis steps are used, and the process of this variant of the invention recycles the retentate from the reverse osmosis step.

As already mentioned, Figure 1 illustrates a device according to the present invention for removing alcohol from natural fermented beverages consisting of a microfiltration membrane module, a nanofiltration membrane module and a reverse osmosis membrane module. According to this Figure 1, a feedstock, which is a fermented beverage material from a natural source, is fed to a microfiltration membrane module 13 in which a microfiltration membrane 14 is arranged via a pipe 11 in which the pump 12 is arranged. The feedstock is divided into a retained fraction, which usually contains high molecular weight proteins and beta-glycans, which is discharged from the apparatus via line 15. The permeate that has been released through the microfiltration membrane 14 is a natural fermented beverage with low protein and beta-glycans concentration. compared to the feedstock. This permeate is withdrawn from the microfiltration membrane module 13 via a line 16 with a valve 17 in place to control the flow of liquid to the first storage tank 18. The liquid is fed to the storage tank 18 via a line 19. The liquid from the first storage tank is discharged via a line 20, the flow of which from the first storage tank 18 is controlled by a valve 21. The raw material withdrawn from the first storage tank 18 is via a conduit 22 is fed to a nanofiltration membrane module 23, in which a nanofiltration membrane 24 is arranged. The conduit 22 includes a pump 25 that serves to pressurize feedstock supplied to the nanofiltration membrane module 23. The fraction retained in the nanofiltration membrane module 23 The valve 17 is included here to allow the fraction retained in the nanofiltration and discharged through the conduit 26 to be recycled to the first storage tank 18. Permeate from this nanofiltration membrane module At 23, it is discharged via line 27 and then passed through a valve 28. through which the flow rate to the second storage tank 29 is controlled. This nanofiltration permeate is introduced into the second storage tank 29 via line 30. The content of this second storage tank 29 is The flow of raw material from the second reservoir 29 is regulated by the valve 32. Through the conduit 33 it is possible to drain the liquid from the second reservoir 29 to the reverse osmosis membrane module 34, in which the reverse osmosis membrane is arranged. The conduit 37 discharges the retained portion from the region of the reverse osmosis membrane module 34 and returns it to the storage tank 29 while passing through the valve 28. The permeate obtained from the reverse osmosis membrane unit 34 is discharged from the device through line 38. After the nanofiltration membrane retentate has been concentrated to the desired level, the nanofiltration retentate is transported via line 20 and passed through valve 21 to line 39 to transport the nanofiltration concentrate to the mixing tank 40. The concentrate obtained in reverse osmosis is then Once the necessary ethanol concentration has been reached, it is withdrawn from the storage tank 29 via line 31 and, after passing through the valve 32, is fed to line 41 through which the reverse osmosis concentrate is discharged to the mixing tank 40 in which the nanofiltration retained the proportion retained in reverse osmosis mixes to reconstitute the alcohol-free natural fermented beverage. A water treatment source 42 is connected to the second storage tank 29 via line 43. From the mixing tank 40 the product is discharged via line 44.

Figure 2 illustrates an apparatus of the present invention comprising a nanofiltration membrane module and a reverse osmosis membrane module. The natural fermented beverage is introduced via line 19 into the first storage tank 18, passing through the valve 17. The natural fermented beverage is discharged from the first storage tank 18 via the line 20, wherein the flow of liquid from the first storage tank 18 is controlled by the valve 21. 22, the natural fermented beverage is discharged to the nanofiltration membrane module 23, in which the nanofiltration membrane 2.4 is arranged. A pump 25 is included in said pipe. which serves to pressurize said natural fermented beverage material to a suitable pressure to facilitate permeate transport through the nanofiltration membrane 24.

The fraction retained on the nanofiltration membrane is discharged from the nanofiltration membrane module 23 via line 26 and is recycled to the first storage tank

The permeate from the nanofiltration module 23 is withdrawn via line 27 and, after passing through the valve 28, is passed to a second storage tank 29. This permeate is introduced into said second storage tank 29 via line 30. Permeate from the nanofiltration from this tank 29 is discharged via a line 31 to which a valve 32 for regulating the flow of liquid from said second storage tank is connected

29. Through the conduit 33, the raw material is removed from the second storage tank 29 to the reverse osmosis membrane module 34, in which the reverse osmotic membrane 35 is arranged.

which serves to pressurize the feedstock supplied to the membrane module 34 to conduct reverse osmosis. The permeate from the reverse osmosis membrane module 34 is removed via line 38. The portion retained in the reverse osmosis membrane module 34 is discharged from the reverse osmosis membrane module 34 via a line 37 that is connected to a valve 28 in the line to direct the recycled reverse osmosis retained portion back to the second storage tank 29 The contents of the first reservoir 18, after it has been concentrated to the desired level, are discharged from the first reservoir through line 20, which portion then passes through a valve into line 39 which is connected to the mixing tank 40.

thereby bringing the collected nanofiltration concentrate to the mixing phase in this mixing container 40. The reverse osmosis concentrate in which the ethanol has been concentrated to the desired level is removed from the second storage tank 29 via line 31 and passed through valve 32 to line 41, via wherein the reverse osmosis concentrate is fed to a mixing container 40 in which it is mixed with the nanofiltration concentrate. A water treatment source 42 is connected to the second storage tank 29 via a conduit 43, thereby providing a treatment water supply to said second storage tank 29. From said mixing container 40 the product is discharged via line 44.

Fig. 3 shows an apparatus for removing alcohol from a natural fermented beverage raw material according to the present invention, comprising a microfiltration membrane module and a reverse osmosis membrane module. Into this apparatus, the natural fermented beverage raw material is fed via a pipe 11 in which a pump 12 is provided to pressurize the natural fermented beverage raw material, and the raw material is first fed to a microfiltration membrane module 13 in which the microfiltration membrane 14 is provided. The natural fermented beverage is passed to the microfiltration membrane 14. at this stage, the fraction retained by the membrane, which has a high concentration of high molecular weight proteins and betaglycans, is separated from the raw material and is removed from the microfiltration membrane module 13 via line 15. The permeate with a substantially lower concentration of proteins and betaglycans is discharged from this microfiltration membrane module 13 via line 16. The permeate flow from the microfiltration membrane module 13 is regulated by valve 28. after passing the valve, this microfiltration Ultrafiltration permeate being discharged via line 30. into which the permeate withdrawn into the storage tank 29th

The liquid from the storage tank 29 is discharged via a line 31, which is passed through a valve 32 to control the flow of liquid from the storage tank 29. The valve 32 also directs the flow of liquid into the line 33. in which a pump 36 is arranged, and through this line, the liquid is fed to the reverse osmosis membrane module 34 in which the reverse osmosis membrane is provided.

35. In the reverse osmosis module 34, a permeate containing a higher ethanol concentration than the ethanol concentration in the feedstock is separated from the liquid, the permeate being withdrawn from the reverse osmosis membrane module via line 38.

The fraction retained in reverse osmosis, which has a lower ethanol concentration but a higher concentration of flavor and flavor compounds, is withdrawn from the reverse osmosis membrane module 34 via line 37. This line 37 is connected to a valve 28 that directs this recycled The reverse osmosis retentate stream is returned to the reservoir 29. A reservoir 29 is connected to the reservoir 29 via a conduit 43, which replaces the permeate withdrawn from the membrane module to reverse osmosis with water.

When the desired level of ethanol in the storage tank 29 has been reached, the contents of this tank are discharged via line 31 and passed through a valve 32, which directs it to line 41 for discharging the product obtained therefrom.

Claims (9)

patent claims (Revised version) A method of removing alcohol from a natural fermented beverage, comprising (A) optionally contacting the feedstock fed to the microfiltration and comprising the natural fermented beverage with a microfiltration membrane under conditions wherein the feedstock stream is divided into a microfiltration permeate having a lower concentration of high molecular weight haze compounds and a fraction retained by the microfiltration membrane having a higher concentration of high molecular weight haze compounds compared to the feedstock feed to the microfiltration, (B) optionally contacting the feedstock fed to the nanofiltration, and containing a natural fermented beverage or microfiltration permeate with a nanofiltration membrane which separates the fraction with a molecular weight ranging from 100 to 10 000, under conditions where the nanofiltration trickle stream is divided into a nanofiltration permeate having a lower concentration of flavor and flavor compounds and a fraction retained by the nanofiltration membrane with a higher concentration of flavor and flavor compounds compared to the feed stream of the nanofiltration feedstock, (C) at the reverse stage osmosis contacting a feed stream comprising a microfiltration permeate or a reverse osmosis membrane permeate nanofiltrate permeate which selectively permits ethanol and selectively retains the flavor-providing compounds under conditions where the feed stream introduced into the reverse osmosis phase is divided into a portion passed through the reverse osmosis membrane, which has a higher ethanol concentration and a lower content AND A method according to claim 1, characterized in that it comprises: (A) contacting the feed stream fed to the microfiltration and containing the natural fermented beverage ingredient with the microfiltration membrane, (B) contacting the feed stream fed to the nanofiltration and containing the permeate from the nanofiltration membrane microfiltration, (C) contacting the feed stream fed to the reverse osmosis and containing permeate from reverse osmosis membrane nanofiltration, and (D) recombining the reverse osmosis trap with the nanofiltration trap. - 2 aroma and flavor generating compounds, and a fraction retained by the reverse osmosis membrane having a lower ethanol concentration and a higher proportion of flavor and flavor delivery compounds, as compared to the feed stream fed to the reverse osmosis phase, characterized in that necessarily carrying out both said steps (A) and (B) or one of these steps, wherein in the case of step (B) the proportion retained in reverse osmosis and the proportion retained in nanofiltration are recombined in the subsequent step (C), wherein the microfiltration membrane has a pore size in the range of 0.1 to 1.0 µm, the nanofiltration membrane separates the fraction with a molecular weight ranging from 100 to 10,000 and the reverse osmosis membrane separates the fraction with a molecular weight ranging from 50 to 100. A method according to claim 1, characterized in that it comprises: (B) contacting the feed stream fed into the nanofiltration and containing permeate from the microfiltration with the nanofiltration membrane, (C) contacting the feed stream fed into the reverse osmosis and containing the permeate from the nanofiltration with the reverse osmotic membrane, and « (D) despreading retentate and the reverse osmosis ₁ with the retentate in the nanofiltration. The method of claim 1, comprising: (A) contacting the feed stream fed to the microfiltration and containing the natural fermented beverage ingredient with a microfiltration membrane, (C) contacting the feed stream fed to the reverse osmosis and containing the permeate from the nanofiltration with the reverse osmotic membrane. Method according to claim 2 or 3, characterized in that the nanofiltration retentate is recycled and re-contacted with the nanofiltration membrane to further concentrate the nanofiltration retentate. , Method according to one of Claims 1 to 5, characterized in that the fraction retained in the reverse osmosis is recycled and again contacted with the reverse osmosis membrane to separate further ethanol from the fraction retained in the reverse osmosis. 7. An apparatus for removing alcohol from a natural fermented beverage, comprising: (A) optionally one or more microfiltration modules, (B) optionally means for supplying a natural fermented beverage to said microfiltration module. (C) optionally means for draining the fraction retained in the microfiltration from the microfiltration module area, (D) optionally means for draining the microfiltration permeate from the microfiltration module area, (E) optionally one or more nanofiltration modules, (F) optionally means for feeding the natural fermented beverage (G) optionally means for removing the nanofiltration retentate from the nanofiltration module region, (H) optionally means for removing nanofiltration permeate from the nanofiltration module region, (I) at least one reverse osmosis membrane module comprising a membrane capable of selectively permeate ethanol and selectively retain aroma-forming and flavor-forming compounds contained in natural fermented beverages; (J) microfiltration permeate delivery means; or nanofiltration permeate into the reverse osmosis membrane module, (K) means for draining the reverse osmosis retained portion from the reverse osmosis membrane module region, (L) means for draining the reverse osmosis permeate from the reverse osmosis membrane module region, that if a microfiltration module is used, it comprises a membrane with a pore size in the range of 0.1 to 1.0 gm; if a nanofiltration module is used, it comprises a membrane separating a fraction having a molecular weight in the range of 100 to 10,000 and a module for reverse osmosis, it comprises a membrane separating a fraction with a molecular weight ranging from 50 to 100, and further, if parts (A), (B), (C) and (D) are used, then all are used simultaneously, if parts ( E), (F), (G) and (H), then the combinations are all simultaneously and either a set of parts (A), (B), (C) and (D), or a set of and parts (E), (F), (G) and (H), or both xyxo systems must be present, and furthermore if the set of parts (E), (F), (G) and (H) is used, the poxom is x need to use partx (M) which represents: (M) means for combining the fraction retained in the nanofiltration and the fraction retained in the reverse osmosis. 8. The apparatus of claim 7, further comprising: (N) a storage tank adapted to collect nanofiltration permeate from (H), (O) means for transporting the contents of the storage tank to the reverse osmosis membrane module, (P) means for recycling the portion retained in reverse osmosis to the storage tank, and (Q) means for adding water to the storage tank (N) to treat all or part of the reverse osmosis permeate volume. Apparatus according to claims 7 or 8, further comprising: (R) a second storage tank adapted to collect the feed to the nanofiltration module, which contains the natural fermented beverage material or permeate from the microfiltration membrane module, (S) means for recycling the nanofiltration retentate to the second storage tank (R), (T) means for transporting the contents of the second reservoir (R) to the nanofiltration membrane module, and (U) means for transporting the concentrated retentate contained in said second reservoir (R) to the means (M) for combining the retentate at the nanofiltration and the retentate at the reverse osmosis.