EP0328596A1 - Process for selective removal of volatile substances from liquids and installation and device for implementing the process - Google Patents

Process for selective removal of volatile substances from liquids and installation and device for implementing the process

Info

Publication number
EP0328596A1
EP0328596A1 EP19880907142 EP88907142A EP0328596A1 EP 0328596 A1 EP0328596 A1 EP 0328596A1 EP 19880907142 EP19880907142 EP 19880907142 EP 88907142 A EP88907142 A EP 88907142A EP 0328596 A1 EP0328596 A1 EP 0328596A1
Authority
EP
Grant status
Application
Patent type
Prior art keywords
membrane
permeate
flow
separation
cross
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP19880907142
Other languages
German (de)
French (fr)
Inventor
Walter Gresch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bucher-Guyer AG
Original Assignee
Bucher-Guyer AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis, ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/025Reverse osmosis; Hyperfiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis, ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/24Dialysis ; Membrane extraction
    • B01D61/246Membrane extraction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis, ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58Multistep processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D63/00Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/08Flat membrane modules
    • B01D63/082Flat membrane modules comprising a stack of flat membranes, e.g. plate-and-frame devices
    • B01D63/084Flat membrane modules comprising a stack of flat membranes, e.g. plate-and-frame devices at least one flow duct intersecting the membranes
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12GWINE; OTHER ALCOHOLIC BEVERAGES; PREPARATION THEREOF
    • C12G3/00Preparation of other alcoholic beverages
    • C12G3/08Preparation of other alcoholic beverages by other methods for varying the composition of fermented solutions, e.g. by reducing the alcohol content
    • C12G3/085Preparation of other alcoholic beverages by other methods for varying the composition of fermented solutions, e.g. by reducing the alcohol content using membranes, e.g. by ultra filtration, by dialysis, by osmosis, by inverse osmosis, by electrodialysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis, ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/145Ultrafiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis, ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/147Microfiltration

Abstract

Zum selektiven Entfernen von flüchtigen Stoffen aus Flüssigkeiten wird die Ausgangsflüssigkeit einer Querstrom-Membrantrenneinrichtung (2) zuge führt, in der das aus Wasser und flüchtigen Stoffen bestehende Permeat durch er höhten Transmembrandruck und Konzentrationsdifferenz abgetrennt wird. For selectively removing volatile substances from liquids, the output fluid of a cross-flow membrane separation means (2) is supplied leads, in the existing of water and volatile substances permeate is separated by he creased trans-membrane pressure and concentration difference. An schliessend wird das Permeat in eine weitere Flüssig-Flüchtig-Trenneinrichtung (8) geleitet, in welcher der Alkohol heraus destilliert wird. On closing the permeate is passed into a further liquid volatile separation device (8), in which the alcohol is distilled out. Das nur noch aus Wasser, Salzen, Säuren und Extrakte bestehende Permeat wird danach in die Querstrom- Membrantrenneinrichtung (2) zurückgeführt, wo es die Permeatseite im Gegenstrom zum Retentatfluss druchströmt. The existing only of water, salts, acids and extracts permeate is then recycled to the cross-flow membrane separation means (2), where it druchströmt the permeate side countercurrent to the retentate flow. Über schüssiges Permeat kann in die entalkoholisierte Ausgangsflüssigkeit eingeleitet werden. About schüssiges permeate can be introduced into the de-alcoholized starting liquid. Durch das erfindungsgemässe Verfahren wird die Wirtschaftlichkeit der Anlage und die Qualität des Endprodukts erheblich verbessert. The inventive method, the efficiency of the system and the quality of the final product is greatly improved.
Abstract Abstract
To selectively remove volatile substances from liquids, the original liquid is introduced into a cross-flow membrane filter (2) in which the permeate consist ing of water and volatile substances is separated as a result of increased trans- membrane pressure and concentration difference. To Selectively remove volatile substances from liquids, the original liquid is Introduced into a cross-flow membrane filter (2) in Which the permeate consist ing of water and volatile substances is separated as a result of Increased trans-membrane pressure and concentration difference. The permeate is then passed into another liquid-volatiles filter (8) where the alcohol is removed by distilla tion. The permeate is then passed into another liquid-volatile filter (8) where the alcohol is removed by Distilla tion. The permeate which by then contains only water, salts, acids and extracts, is recycled into the cross-flow membrane filter (2) where it flows across the per meate side in countercurrent to the residue flow. The permeate Which by then contains only water, salts, acids and extracts, is recycled into the cross-flow membrane filter (2) where it flows across the meate by side in countercurrent flow to the residue. Excess permeate can be intro duced into the de-alcoholized original liquid. Excess permeate can be intro duced into the de-alcoholized original liquid. The cost-effectiveness of the instal lation and the quality of the end product anre considerably enhanced by the process. The cost-effectiveness of the instal lation and the quality of the end product ANRE considerably enhanced by the process.

Description

A method of selectively removing volatile Stof¬ fen from liquids, as well as conditioning and means for performing the method

The invention relates to a method for selectively removing volatile substances from liquids, in particular of alcohol beverages such as wine, beer or fermented fruit juices pass through Membrantrennver¬ and at least one further separation process.

In the dealcoholization of liquids unter¬ (0.5%) is deposited between alcohol reduction (eg 40%) and total dealcoholization. Here, the characteristic flavors of Ausgangs¬ liquid, such as wine or beer, remain unchanged as possible in ental¬ koholisierten drink.

To achieve this goal, thermal processes have become known, which have evolved from evaporation plants her¬ out. A known plant for Gewin¬ voltage of non-alcoholic wine comprises a multi-stage evaporator in which the alcohol is evaporated together with the flavorings. The condensate is a distillation column supplied with a plurality of release agents, in which the alcohol is distilled out. Thereafter the separated aroma substances are again mixed with the ent drunken wine. The disadvantage of the known thermal process be¬ is that infol¬ arise ge the thermal load geschmacksvermindernde cooking products and an undesirable taste in Nebenge- dealcoholized beverage occurs. Removing Serde is the energy requirements for thermal processes very high and the system, particularly when using multiple stages of evaporation and a distillation column with multiple Trennstufeh relatively expensive.

It membrane separation processes for Entalkoholi- tion of liquids are also known, in which the alcohol by reverse osmosis in Querstrommembranver¬ drive from the source liquid, such as wine or beer, is filtered out. With the addition of Was¬ ser to be dealcoholized liquid is passed by means of a circulating pump through the membrane filter modules. The volatiles out of the way of diafiltration are eliminated ausge¬ together with the water on the permeate side of the membrane filter module. To improve performance, a concentration or pre-concentration of the retentate is also oft¬ repeatedly performed. Since in these known Mem¬ branverfahren no heat treatment is performed, the resultant with the thermal process by-products or cooked flavor is not present. With increasing Konzen¬ tration, however, the flavoring substances contained in the liquid Ausgangs¬ diffuse through the membrane of the membrane filter module, in particular if the membrane is not true exactly abge¬ to the starting liquid. The result is a change in flavor of the drink, which alcoholisation deteriorated with increasing decision. This means that, for example, wine loses its characteristic Ge in total dealcoholization by membrane filtration taste.

Another known method for Ξntalkoholisie- tion by liquids is the dialysis method (EP-OS 0,021,247). In contrast to reverse osmosis processes in which the transmembrane pressure acts as the driving force for the permeate flux through the membrane, the separation of the alcohol from the raw liquid is carried out in the dialysis process practically solely by the Kon¬ zentrationsunterschiede of the two separated by a diaphragm liquids. To be dealcoholized source liquid flows through the retentate side of the dialysis module. On the permeate water is passed in countercurrent to the retentate flow through the dialysis module. Due to the de Konzentrationsunterschie¬ the volatiles contact (alcohol) from the re tentat through the membrane and be abge¬ together with the water on the permeate side as a dialysate leads. In the same manner as the reverse osmosis tre¬ other ten with the diffusion of the alcohol, nieder¬ molecular substances, in particular flavoring substances through the membrane into the dialysate over. When Gewin¬ voltage of low-alcohol beverages this Aro¬ have maverluste on the overall character of the drink no significant impact. In contrast, suffers considerably in the total-dealcoholation by dialysis of flavor character and richness of the starting product. Moreover, given by the operating principle, low specific power of the system decreases significantly with increasing reduction in the alcohol and the energy consumption increases accordingly. The Dia¬ analysis method is thus suitable for the Total Ental- not koholisierung.

It has been known a process for the dealcoholization of wine, which consists of a combination of dialysis method and thermal method. The wine as the starting liquid flows through the re tentatseite of the dialysis module and gives the alcohol due to the differences in concentration by the Mem¬ brane from passing to the dialysate which flows through the permeate side of the dialysis module in countercurrent to the retentate flow. The dialysate is introduced into a Destillierko¬ lonne, in which a further separation of the alcohol from the dialysate by vacuum distillation at nie¬ Driger temperature. The remaining characterized in rezirkulie¬ leaders dialysate valuable substances cause ei¬ nen only a small concentration difference for Reten¬ did, so that after a certain start-up time and Errei¬ chen the balance essentially only Alko¬ hol from the retentate into the dialysate diffused and a considerable part of the valuable substances in the retentate remains. The disadvantage of this method is that dialysis in¬ follow with increasing alcohol reduction performance significantly decreases, so that in total Ental- the economy of the plant is no longer koholisierung -guarantees.

The invention is therefore the object of the fluids known processes for dealcoholization of Flüs¬ avoid disadvantages inherent and improve the efficiency of the system and the quality of Pro¬ domestic product not only in the reduction of alcohol, but also in the total dealcoholization.

This object is achieved according to the invention in that the existing mainly of water and volatile substances permeate separated by compared to Dialyseverfah¬ ren increased transmembrane pressure and difference by Konzentrations¬ of the source liquid, subsequently the alcohol by at least one further liquid-volatile separation process is removed and then the resulting residue least partially ren in the permeate circuit between Membrantrennverfah¬ and at least one of the further liquid-volatile separation process is returned.

Further advantageous and expedient embodiments of the invention are given in the patent claims.

The advantages achieved by the invention are ins¬ special is that the drawbacks of the known methods while maintaining their benefits by the inventive combination of reverse osmosis, Dia¬ to analysis and can largely eliminate thermal processes. The inventive cross flow Membrantrenn¬ device is constructed so that the liquid is carried Flüch- tig separation through the membrane by dialysis against the increased transmembrane pressure and Kon¬ zentrationsdifferenz. The driving force is the transmembrane pressure, which substantially improves the given for the pure Dia¬ lysis method of low power and the resulting alcohol with increasing reduction in power loss is greatly reduced. A wei¬ more excellent advantage is that the passing the alcohol through the membrane flavorings, Sal¬ ze, process acids and extracts after removal of the alcohol by at least one further liquid-volatile Trenn¬, driving, for example, thermal distillation, Membrenver- remain in the permeate and a portion of the permeate is recycled back into the retentate. This blei¬ ben obtained largely unverän¬ changed in the initial liquid, for example in the wine ent preserved, original flavor and bouquet substances even in total dealcoholization. The invention is explained in the following description and the drawing illustrating various embodiments in detail. Show it:

Fig. 1 is a schematic representation of the inventive system,

Fig. 2 shows the installation according to Fig.l with a vor¬ connected reverse osmosis Einrich¬ processing for pre-concentration of the Aus¬ duct fluid,

Fig. 3 shows a longitudinal section through a domestic he dungsgemäss.modifiziertes hollow fiber reverse osmosis module,

Fig. 4 shows a longitudinal section through a modified According to the invention Umkehros- mose-tube module,

Fig. 5 is a section strung each other by a plurality of an¬, modified reverse osmosis plate modules according to the invention,

Fig. 6 is a section through the reverse osmosis module plate according to the line VI-VI in Figure 5,

Fig. 7 is a section along the line V I-VII in Figure 5,

Fig. 8 a section through the reverse osmosis module plate according to the line VIII-VIII in Figure 6 and FIG. 9 shows a section according to line IX-IX in Fig.7.

In the embodiment of Fig. 1 to the ental¬ koholisierende wine is introduced via a feed line 1 into the retentate side of a cross-flow membrane separation unit 2. The cross-flow membrane separation unit

2 consists of one or more cross-flow membrane modules 3, in which mainly alcohol and water as so¬ first in a non-negligible mass training addition, undesirable flavors, salts, reindeer Säu¬ and extracts are separated from the wine. The specific structure of the cross-flow membrane modules 3, which cause a liquid-volatile separation due to the transdiaphragm brand rucks and the concentration difference will be described later. In cross-flow membrane module

3 of the wine flows through the separate from the permeate side by a membrane 4 retentate in Pfeilrich¬ tung 5 and leaves after separation of the volatile Stof¬ fe as entalkohlisierter or reduced alcohol wine through the discharge pipe 6, the cross-flow membrane module 3. The of alcohol, water next fen also Aromastof¬, salts, acids and extracts existing permeate is composed via a permeate-discharge line 7 into a weite¬ re liquid volatile separation device 8, for example approximately in Ausfüh¬ from a distillation column, out ein¬. In the distillation column the alcohol from the permeate is distilled at low temperatures, which are made possible by a vacuum pump. 9 Via a return line 10 and a buffer tank 11 is composed of the flavoring agents, salts, acids and extracts residue recycled to the membrane module 3, the cross-flow-membrane separation unit. 2 Circulation pumps 12 and 13 in the return line 10 to ensure that the permeate side of the Permeat¬ cross-flow membrane module 3 flows in the direction of arrow 14 in countercurrent to the retentate flow.

Although the membrane 4 is selectively chosen for the separation of alcohol, due to contact of the initial concentration difference between retentate and permeate initially together with the alcohol and water also Aro¬ mastoffe, salts, acids, and extracts from the wine in the permeate over. As the concentration of these substances, which remain after separation of the alcohol in the liquid volatile separation device 8 in the permeate, the concentration difference is reduced, so that diffuse, after reaching the equilibrium, the value of the substances referred only to an insignificant extent in the permeate "and thus the dealcoholized wine are included. the effect is improved by adding flavorings, salts, acids and extracts corresponding to the ingredients of the Wei¬ nes, for Puffe-rtank 11 and / or connecting lines in the Ver¬ 10 and / or pumps 12, 13. these substances can be obtained from the rezirkulie¬ leaders permeate or excess permeate or mixed together synthetically by enrichment by distillation or membrane processes.

The membrane module 3 is operated smoothly brand with an increased transdiaphragm which is above 5 bar. The driving force for the diffusion of alcohol is thus less the difference in concentration between the retentate and Per¬ meat but primarily the pressure which is required to overcome the osmotic counterpressure of the alcohol. The osmotic counterpressure of salts, acids, expression rate wings and flavors increases with increasing con- centration in the permeate to, so that will be lost over the pure reverse osmosis less valuable materials and only diffused after a certain start time essentially alcohol into the permeate.

From the liquid-volatile separation device 8, a connecting line 15 to the discharge pipe 6 for the Re¬ leads tentat. By connecting line 15 to the dealcoholized wine is supplied überschüs¬ Siges permeate after passing through the liquid-volatile separation device 8, which is thereby enriched with additional useful materials. With increasing transmembrane pressure, the permeate volume increases. The result is that more permeate has to be discharged as a surplus through the connecting line 15th This increases the concentration of the recirculated through the recirculation line 10 in the permeate from Ver¬ ratio to the concentration in the retentate. Thus the concentration gradient and thus the amount that diffuses from the retentate into the permeate increases. The Wertstof- fe in excess permeate are indeed due to the gerin¬ gen thermal load in the distillation column is designed as a liquid-volatile separation device 8 is not of the same quality as originally vorhan¬ in the wine. It is therefore to optimize between performance and quality, especially when mast open without adding Aro¬, salts, acids and extracts are working to rezirkulie¬ leaders permeate. It has herausge¬ assumed that bar a very high quality compared to the rei¬ NEN dialysis method is achieved at a significantly increased throughput at a transmembrane pressure in the range 5 to 25 With the addition of flavorings, salts, acids and extracts for recirculating permeate the permissible for reverse osmosis systems pressure can be used aus¬ and thus additional improvement in performance can be achieved with good quality. At a lower alcohol reduction, for example to 50% of the original content, at lower Quali¬ meats can be dispensed to the wine tätsansprüchen on the return of the excess-per. Instead, 2 drinks dilution water can be fed to the retentate prior to entering the cross-flow membrane separation device. The result is that by using the same facility a less gentle distillation can be carried out, resulting in increased performance and savings in energy costs.

In addition to the removal of undesirable volatile Stof¬, fen as alcohol from liquids, the inventive method also allows for the separation of valuable volatile materials, for example, use aroma substances from liquids to advantage. In the first case, the diaphragm 4 of the cross-flow membrane module 3 must have a high salt retention, while the salt-Rückhaltevermδgen should be as low in the aroma recovery. With appropriate design, it is therefore by changing the cross-flow membrane modules Mo¬ possible einzuset¬ same plant during the harvest campaign for aroma recovery and post-season for the dealcoholization of fermented fruit juices zen. In contrast to the purely thermal aroma recovery, the quality is significantly improved with the inventive method, since no thermal, but a cold separation of the aroma components from the fruit juice is carried out. Through this versatile use of the inventive system whose Wirtschaftlich¬ ness is greatly improved, which temen with the known Sys¬ is not possible. If the inventive method is used for obtaining a concentrated alcohol-liquid, it is expedient, the cross-flow membrane separation unit 2 is a conventional reverse osmosis device 16 sigkeit for preconcentration of Ausgangsflüs¬, for example raw juice upstream in (Fig.2). The pre-concentration is preferably carried out only to the extent that the aroma losses resulting are insignificant. The raw juice, which is preferably already cleared by an upstream, not shown ultra- or microfiltration device, the reverse osmosis unit 16 is supplied to aufkon¬ centered. The concentrate is fed via a line 17 into the retentate supply line 1 of the cross-flow membrane separation unit. 2 In a Vor¬ concentration to about 50% and a relatively high pressure Trans¬ membrane cross-flow membrane separation unit 2 is achieved an improvement in quality at high throughput. The reason is that in the preconcentration 16 are formed only small losses of valuable materials by reverse osmosis device, but holisierung and thus occurs a strong reduction of the permeate in the Entalko- a reduction of the excess permeate. This in turn has an increased Konzen¬ concentration of valuable materials in the recycling of the permeate into the cross-flow membrane separation device 2 for a row.

In case of strong pre-concentration in the reverse osmosis Ein¬ device 16, it is advantageous because of the resulting höhe¬ ren losses of valuable substances, a part of the permeate through a line 18 into the permeate drainage duct 7 of the cross-flow membrane device 2 einzuspei¬ sen. It has been found that by the preconcentration by means of the reverse osmosis device 16, the cross-flow membrane separation unit 2 capitalization for Entalkoho- or aroma recovery can be built much smaller and consequently the nachfolgen¬ de liquid volatile separation device 8 can be made smaller. The reverse osmosis device 16 connected vor¬ ultra- or microfiltration device is a prerequisite for clean juices to place the tube modules for pre-concentration by reverse osmosis device 16 also cheaper Nicht¬ pipe modules, for example, hollow fiber , winding or disk Mo¬ modules being able to use.

In Fig. 3 of the drawings, an embodiment of the cross-flow membrane module 3 for the cross-flow membrane separation device is Brant 2 presented in the form of a modified Hohl¬ fiber reverse osmosis module. The cross-flow membrane module 3 has "at its front end an inlet opening 19 for the to entalkohlisierende, DAS retentate forming starting liquid. An outlet is located at the opposite end of opening 20 for the retentate which has a the membranes 4-forming hollow fiber body of the cross-flow membrane module 3 flows through in arrow direction. 5 in the membranes 4 surrounding jacket 21 of the cross-flow membrane module 3 is located in the vicinity of the inlet port 19, a permeate Auslassδffnung 22 connected to the permeate is connected to discharge pipe 7 of the cross-flow membrane separation unit 2. at the opposite end of the Quer¬-flow membrane module 3, a permeate is in the casing 21 inlet opening 23 is arranged, the processing with the feeedback 10 of the cross-flow membrane separation unit 2 verbun¬ the is. the tendency austre¬ permeate on the outside of the membrane 4 accumulates in the space between the diaphragm and the outside jacket 21 and by J hströmt with the aid of circulation pumps 12 and 13, the permeate side of the cross-flow membrane module 3 ind direction of the arrow 14 in Gegen¬ stream to retentate flow.

Another embodiment of the cross-flow membrane-Mo¬ duls 3 for the cross-flow membrane separation device 2 is shown in Fig. 4 in the form of a modified reverse osmosis pipe module. An inner tube 24 of the cross-flow Mem¬ bran module 3, together with the diaphragm 4, the outlet opening 19 and the Ein¬ Auslassδffnung 20 for the Reten¬ tat on. The wall of the inner tube 24 is with translucent openings 25 to the membrane 4, through which can pass the permeate and surrounding in the space between inner tube 24 and an inner tube Mantel¬ pipe is collected 28th The jacket tube 28 has the outlet 22 for the permeate near the Einlassδffnung 19th At the other end of the cross-flow membrane module 3 is located in the casing 28, the Einlassöff¬ voltage 23, which is connected to the return line 10 of the cross-flow membrane separation unit. 2 With the aid of circulation pumps 12 and 13, the permeate flows through the space between the casing tube 28 and outer tube 26 in Pfeilrich¬ tung 14 in countercurrent to the retentate flow.

Figs. 5 to 9 show a further embodiment of the cross-flow membrane module 3, a reverse osmosis plate module, which plate consists of a plate member 29 and a terminally 30 between which the through Stützele¬ elements 31 supported membrane 4, consisting Trenn¬ of membrane 40 and membrane support 41, is arranged. The end plate 30 has a chamber 32 for the retentate and the plate member 29 to a space 33 for the permeate. The spaces 32 and 33 are each separated by the membrane 4 von¬ and the retentate and the Per¬ meat in opposite directions flow through. The plate member 29 has on its back a lug 34, to which a further plate member 29 can be attached. Through between the two Plattenelemen¬ th 29 arranged membrane 4 there are further Räu¬ me 32 and 33, which are to flow from the retentate or the permeate durch¬ (Fig. 6 and 7, arrows 5 and 14).

From Fig. 6 in conjunction with FIGS. 8 and 9 ersicht¬ Lich that the space 32 has at its upper right end of the inlet opening 19 for the retentate, and at its lower left end of the outlet opening 20 for the Re¬ tentat. Fig. 7 shows in conjunction with FIGS. 8 and 9, that in the space 33 at the lower right end of the permeate inlet opening 23 and at the top, lin¬ ken end of the permeate outlet 22 is located.

When lining up of several plate members 29, the Einlassoffnu gene 19 and the gene Auslassöffnun¬ 20 of the individual spaces 32 for the retentate through tubes or passages 35 (Fig. 8) and 36 (Fig. 9) mit¬ interconnected. The compound of the permeate inlet δffnungen 23 and the permeate outlet ports 22 of the individual spaces 33 is carried out respectively through tubes or passages 37 (Fig. 8) and 38 (Fig. 9).

Claims

cLAIMS
A method for selectively removing volatile substances from liquids, in particular of alcohol beverages such as wine, beer or fermented fruit juices by membrane separation procedures and min¬ least one further separation process, characterized denotes ge that the existing mainly of water and volatile materials permeate through in the United pressure ¬ equal elevated to the dialysis method Transmembran¬ and separated by difference in concentration of the starting liquid, then the volatile material removed by at least one further Flüs¬ sig-volatile separation method, and then the resulting residue is at least partially moved into the permeate circulation between Membrantrenn¬ and at least one the further Flüs¬ sig-volatile separation process is returned.
2. The method according to claim 1, characterized in that in the separation pressure by increased Transmembran¬ and the permeate countercurrent flows through concentration difference to the retentate and the treiben¬ de force for the liquid-volatile separation vorwie¬ quietly an increased transmembrane pressure.
3. The method of claim 1 or 2, characterized gekenn¬ characterized in that the membrane separation process membran¬ technologically after the reverse osmosis process arbei¬ tet.
4. The method according to any one of claims 1 to 3, characterized in that the transmembrane pressure is more than 5 bar.
5. A method according to any one of claims 1 to 4, characterized in that the separation of volatiles from the ge through the membrane separation process wonnenen permeate by thermal distillation and / or one or more membrane processes er¬ follows.
6. A method according to any one of claims 1 to 5, characterized in that accumulating excess permeate the dealcoholized feedstock fluid is supplied.
7. AV lead according to any one of claims 1 to 6, da¬ by in that the process at Membrantrenn¬ mastoffe through the membrane passing Aro¬, salts, acids, extracts drive through Trennver¬ such as distillation, ion exchange membrane process or prior to recycle in are meat circulation enriched the Perfluorinated or that the running Permeatkreis- be added from the outside corresponding substances.
8. A method according to any one of claims 1 to 7, da¬ by in that the Ausgangsflüssig¬ ness before the dealcoholation Getränkeverdün¬ voltage is supplied water.
9. A method according to any one of claims 1 to 8, da¬ by in that the Ausgangsflüssig¬ ness prior to the separation pressure by increased Transmembran¬ and vorkonzen¬ lead by difference in concentration by a preceding Membrantrennverf is trated.
10. A method according to claim 9, characterized gekennzeich¬ net, that part of the permeate from the preconcentration the per- obtained by increased transmembrane pressure and due to concentration difference before the meat or to the further separation procedure is performed zu¬.
11. The method of claim 9 or 10, characterized gekenn¬ characterized in that the Ausgangsflussigkeit is clarified by membrane filtration by means of ultrafiltration or microfiltration prior to its preconcentration.
effected 12. installation for carrying out the method according to one of claims 1 to 11, characterized in that the predominantly pressure through increased Transmembran¬ and concentration difference caused liquid-volatile separation of Ausgangsflussigkeit in a cross-flow membrane separation means (2), the retentate side a is feed line (1) for the starting liquid and a Abfluss¬ line (6) for the at least partially entalko¬ holisierte source liquid and having permeate side a permeate-discharge line (7) with at least one further liquid-volatile separation means (8) connected Brant separation device from which the permeate through a return line (10) in the permeate loop between cross-flow membrane (2) and the further liquid volatile separation device (8) is returned.
13. Plant according to claim 12, characterized in that the cross-flow membrane separation means (2) is equipped with reverse osmosis membranes.
14. Plant according to claim 12 or 13, characterized gekenn¬ characterized in that said further liquid-volatile separation device (8) consists of a distillation column is be¬.
15 system between the further liquid volatile separation device (8) and the cross-flow membrane separation means (2) circulation pumps, one or more Um¬ according to one of claims 12 to 14, characterized in that the permeate circulation line in Rück¬ (10) ( 12, 13) are arranged.
16. Installation according to one of claims 12 to 15, characterized in that in the permeate outflow line (7) and / or in the permeate return line (10) at least one buffer tank (11) is arranged.
17. Installation according to one of claims 12 to 16, characterized in that a line (15) über¬ schüssiges permeate from the further liquid Flüch- tig separating device (8) in the retentate outflow line (6) of the cross-flow Membrantrennein¬ device (2) is initiated.
18. Installation according to one of claims 12 to 17, characterized in that in the or the buffer tank (11) or the connecting cables (10) and / or in the circulation pumps (12, 13) additional Aromastof¬ fe, salts, acids, extracts that the materials of the wine Inhalts¬ at least approximately corresponding to be introduced.
19. Plant according to claim 18, characterized in that the additional flavorants, salts, acids, extracts are obtained by enrichment by distillation or membrane processes from the recirculating permeate or the excess permeate.
20. Installation according to one of claims 1 to 19, characterized in that the retentate Zuführ¬ line (1) with a known per se, the cross-flow-membrane separation unit (2) upstream reverse osmosis device (16) is connected, in which the feedstock fluid is preconcentrated prior to being fed to the cross-flow membrane separation means (2).
21. Plant according to claim 20, characterized in that a portion of the permeate of the upstream reverse osmosis device (16) via a line (18) into the permeate-discharge line (7) of the Quer¬ introduced flow membrane separating device (2) and the liquid-volatile separation device (8) is zuge¬ leads.
22. Plant according to claim 20 or 21, characterized gekenn¬ characterized in that the reverse osmosis device (16) is connected upstream of an ultrafiltration or microfiltration device for clarification of the source liquid.
23. Device according to one of claims 1 to 22, characterized in that the cross-flow Membran¬ separating means (2) of at least one Quer¬-flow membrane module (3), the tentatseite on the Re¬ an inlet opening (19) and a Aus¬ outlet opening (20) for the retentate and has the recirculating permeate through a Einlassöff¬ voltage (23) and an outlet opening (22) in the Gegen¬ or cross-flow to the retentate stream Permeat¬ the side of the cross-flow membrane module (3 ) flows.
24. A device according to claim 23, characterized gekennzeich¬ net, that the inlet opening (19) for the retentate and the Auslassδffnung (22) for the permeate in the flow direction in the region of the last third of the one end and the outlet opening (20) for the retentate and is the inlet opening (23) for the permeate in the range of the last third of the ande ren end of the cross-flow membrane module (3) assigns ange¬.
25. A device according to claim 23 or 24, characterized denotes ge that the Einlassδffnung (19) for the retentate to the supply line (1) and the outlet (20) with the discharge pipe (6) of the retentate is connected and the Auslassδffnung (22 is) device (7) for the permeate to the permeate and the Abflusslei¬ Einlassδffnung (23) with the residue is conduit (10) of the permeate side circuit connected.
26. Device according to one of claims 23 to 25, characterized in that the inlet openings (19, 23) and the outlet openings (22, 20) for reversal of retentate and permeate are interchangeable.
27. Device according to one of claims 23 to 26, characterized in that the cross-flow membrane module (3) is a hollow fiber, tube, or plate module.
28. Device according to one of claims 23 to 27, characterized in that the cross-flow Mem¬ bran module is equipped (3) aus¬ with reverse osmosis membranes.
29. Device according to one of claims 23 to 28, characterized that for supporting the membrane (4) of the designed as a reverse osmosis pipe module cross-flow membrane module (3) dienen¬ of the inner tube (24) a high density in accordance with a porosity of more than 5% of radial Durch¬ openings (27) for the permeate and having 'the inputs and Auslassδffnungen (23, 22) for the permeate circulation at the end of the reverse osmosis pipe module in "an inner tube (24) surrounding the tubular casing (28) are arranged.
30. Device according to one of claims 23 to 29, characterized in that the plates designed as a reverse osmosis module cross-flow membrane module (3) comprises two through the membrane (4) separate rooms (32, 33), located in the space (32) the outlet port (20) located at the obe¬ ren end in a corner of the inlet opening (19) and at the lower end in the opposite corner for the retentate and the permeate inlet port (23) in the space (33) at the lower end existing in the retentate on the same side of the inlet opening (19) area, and the permeate outlet (22) is arranged an¬ in the opposite corner of the room (33) at the upper end.
31. A device according to claim 30, characterized gekennzeich¬ net, that by-side installation of several cross-flow membrane modules (3) the spaces (32) in the region of the inlet openings (19) through passages (35) and in the area of ​​Auslassδffnungen ( 20) for the retentate through passages (36) and the spaces (33) in the region of the permeate inlet ports (23) and the permeate outlet (22) through passages (37) and (38) are connected together.
EP19880907142 1987-08-28 1988-08-24 Process for selective removal of volatile substances from liquids and installation and device for implementing the process Withdrawn EP0328596A1 (en)

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CH332887 1987-08-28

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