WO2018182430A9 - Procédé d'élimination d'un ou plusieurs composés à partir d'un distillat et systèmes et appareil associés - Google Patents

Procédé d'élimination d'un ou plusieurs composés à partir d'un distillat et systèmes et appareil associés Download PDF

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Publication number
WO2018182430A9
WO2018182430A9 PCT/NZ2018/050037 NZ2018050037W WO2018182430A9 WO 2018182430 A9 WO2018182430 A9 WO 2018182430A9 NZ 2018050037 W NZ2018050037 W NZ 2018050037W WO 2018182430 A9 WO2018182430 A9 WO 2018182430A9
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WO
WIPO (PCT)
Prior art keywords
distillate
treatment substance
samples
compounds
distillation
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PCT/NZ2018/050037
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English (en)
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WO2018182430A1 (fr
Inventor
Malan VAN ROOYEN
Original Assignee
Van Rooyen Malan
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Publication date
Application filed by Van Rooyen Malan filed Critical Van Rooyen Malan
Publication of WO2018182430A1 publication Critical patent/WO2018182430A1/fr
Publication of WO2018182430A9 publication Critical patent/WO2018182430A9/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00—Preparation of other alcoholic beverages
    • C12G3/08—Preparation of other alcoholic beverages by methods for altering the composition of fermented solutions or alcoholic beverages not provided for in groups C12G3/02 - C12G3/07
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
    • C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation

Definitions

  • the present invention relates to a method of removing one or more compounds from a distillate, and systems and apparatus therefor.
  • Distillation is the process of separating a mixture of liquids into different fractions.
  • the fractions may contain a wide range of compounds, potentially at different concentrations. Accordingly, distillation finds widespread use in a variety of important industries.
  • One particularly important application of distillation techniques is the production of alcoholic beverages. In these applications, the distillation process is used to create a fraction having a comparatively higher alcohol content than the starting liquid / mixture.
  • the comparatively higher alcohol content fraction is often referred to as a 'distillate'.
  • the starting mixture can be prepared from a number of different ingredients.
  • the characteristics and properties of the starting ingredients contribute to the flavor profile of the alcoholic beverage produced using the distillation method.
  • starting ingredients generally include a carbohydrate source (such as sugar) in combination with yeast.
  • a fermentation process by the yeast is used to produce a solution having a comparatively low alcoholic content.
  • Natural limitations to yeast production prohibit production of a solution having an alcohol content over approximately 14-15% using fermentation.
  • a distillation process is used to produce a liquid having a comparatively higher alcohol content than that which it is possible to produce using a fermentation processes only.
  • distillation processes indiscriminately transfer compound(s) into the distillate if those are volatile at the temperature(s) at which distillation occurs. Therefore, a distillate will normally contain a number of compounds which contribute detrimentally to the flavor profile of the distillate (and eventual alcoholic beverage made using that distillate).
  • a distillate may be treated using a physical filter media such as a carbon filter.
  • the filter can affect the flavor, such as by removing compounds which would otherwise contribute to a distillate's flavor e.g. the filter removes compounds which provide a drink with (or contribute to) its desired flavor.
  • the filtering process can also be time consuming, and it is not uncommon for at home filtering systems to take up to 72 hours to filter between 7 to 8 liters of distillate. This increases the labour / time involved in producing a volume of distillate and therefore makes the process less appealing.
  • a second method to reduce or eliminate compounds from a distillate is to perform a second distillation to produce a second distillate, and potentially even a third distillation to produce a third distillate.
  • these processes can be time consuming and / or introduce additional costs. Accordingly, it is as an object of the present invention to provide an improved distillation method, and / or method of producing an alcohol beverage using a distillation process.
  • a method of removing one or more compounds from a distillate including the step of jetting a treatment substance into the distillate.
  • a system for use in removing one or more compounds from a distillate including a reservoir, a dosing apparatus, wherein the reservoir and dosing apparatus are configured with respect to each other to in-use jet a treatment substance into a distillate in the reservoir.
  • the present invention relates to methods, systems and / or apparatus for use in producing alcoholic beverages for consumption by humans. Reference herein will be made as such. However, this should not be seen as limiting on the scope of the present invention as alternatives are also envisaged as being within the scope of the present invention. For instance, it is envisaged that the present technology could be used in removing compounds from a distillate to have desired flavor / taste profiles such as for use in a foodstuff, perfume, air freshener or the like.
  • the method may include the step of preparing a base mixture.
  • the base mixture may be any liquid or other substance which can be distilled to produce at least one fraction.
  • the base mixture may be referred to as "a wash" by one skilled in the art.
  • the base mixture may be a solution containing sugar (carbohydrates) and other ingredients to provide a desired flavour profile to a distillate produced using the base mixture.
  • Yeast may be added to the solution, and a fermentation process used to produce a liquid mixture having a comparatively low alcohol content (%abv).
  • the base mixture may be produced by dissolution of a sugar such as sucrose in water.
  • carbohydrate sources may be used such as fruit and / or vegetable mixtures.
  • the method according to the invention includes the step of performing a distillation process on the liquid mixture to produce a distillate.
  • the distillation process may occur using any known distillation technique and / or apparatus.
  • the parameters of the distillation process, and features of the distillation technique and apparatus are as should be understood by one skilled in the art.
  • the distillation process includes the step of collecting at least a portion of vapor produced by the distillation process.
  • the vapor is condensed using a condenser to produce the distillate.
  • jetting should be understood as meaning introducing a stream of the treatment substance into the distillate.
  • jetting of the treatment substance into the distillate occurs under pressure, so as to create a comparatively fast flow of the treatment substance and/or be of a sufficient force to agitate the distillate.
  • jetting of the treatment substance into the distillate may cause or promote volatilisation of at least one compound in the distillate. Volatilisation may provide an agitation effect. It is also possible that the process of jetting the treatment substance adjusts the equilibrium of the distillate towards a position in which favors or promotes volatilization of the compound(s).
  • Reducing or eliminating of compounds from a distillate may be useful to reduce or eliminate undesirable compounds from the distillate, which may provide an alcoholic beverage having a more pleasant or desirable flavor profile and perceived taste.
  • the present invention may reduce or eliminate the need to perform second and / or third distillation steps to reduce or eliminate compounds from a distillate. Accordingly, the invention may reduce the costs and time associated with producing an alcoholic beverage having a desired flavor and / or taste profile. Yet a further advantage of the present invention is that it provides an alternative to using physical filter media such as charcoal filters, to remove compounds from a distillate. Again, this may reduce the costs and time associated with producing an alcoholic beverage having a desired flavor and / or taste profile. It may also improve the environmental sustainability of producing alcoholic beverages by eliminating use of consumables such as carbon / charcoal filters. Alternatively, the present invention may be better suited to reducing or eliminating at least one compound from a distillate. As a result, the invention may produce an alcoholic beverage having a desired flavor and / or taste profile.
  • treatment substance should be understood as meaning a substance which can and is jetted into the distillate.
  • the treatment substance may promote or cause compounds to evaporate or volatilize out of the distillate.
  • the treatment substance may be water.
  • This treatment substance is advantageous as it does not provide an undesirable contribution to the flavor of the alcohol.
  • water is safe to drink and therefore does not pose a health risk to those people that may consume a beverage produced according to the invention.
  • Water may also be useful as it can be at least partially removed from the distillate using a second distillation process.
  • the treatment substance may be pre-treated, e.g. water may be filtered and / or distilled, prior to being jetted into the distillate.
  • the treatment substance may include one or more additives which further promote the volatilization of compounds from the distillate.
  • the treatment substance may have a temperature in the range 10 - 65°C when it is jetted into the distillate.
  • the step of jetting the treatment substance into the distillate may occur incrementally.
  • aliquots of the treatment substance may be jetted into the distillate sequentially.
  • the method may include jetting of multiple volumes of the treatment substance into the distillate.
  • each of the aliquots provide a desired volume for the treatment substance to be jetted into the distillate.
  • a period of time is provided between each of the aliquots.
  • the period of time may be any amount of time such as between 2 minutes to 40 minutes.
  • the period of time may decrease or increase between subsequent aliquots e.g. the following may be used :
  • a period of 10 m inutes is provided between the first aliquot and the second aliquot, and a period of 2 minutes is provided between the second aliquot and the third aliquot It is envisaged that the period of time is sufficient to substantially or completely allow bubbles created by jetting to disappear.
  • the bubbles contain volatiles which are being removed from the distillate by the step-wise introduction of the treatment substance.
  • jet treatment process can be easily upscaled to accommodate larger batches liquids to be treated by the method of the present invention.
  • Figure 1 is a flow chart showing steps in a representative method according to an aspect of the present invention
  • Figure 2 is a table summarizing results of analysis of samples produced according to the
  • Figure 3 is a chart showing the result of the table of figure 2;
  • Figure 4 is a chart showing concentrations of selected compounds as shown in Figures 2 and 3;
  • Figure 5A is a chart showing concentration of compounds present in samples produced by jetting a comparatively cold treatment substance according to the present invention
  • Figure 5B is a chart showing concentration of compounds present in samples produced by jetting a comparatively hot treatment substance according to the present invention.
  • Figure 6 is a table summarizing sensory evaluations of samples produced according to the
  • Figure 7 is a first perspective view of an apparatus according to an aspect of the invention.
  • Figure 8 is a second perspective view of an apparatus according to an aspect of the present invention.
  • Figure 9 is a first side view of an apparatus according to an aspect of the present invention.
  • Figure 10 is a second side view of an apparatus according to an aspect of the present invention.
  • Figure 11 is a top view of an apparatus according to an aspect of the present invention.
  • Figure 12 is a side view of an apparatus according to an aspect of the present invention having a cover in place;
  • Figure 13 is a second side view of an apparatus according to an aspect of the present invention having a cover in place;
  • Figure 14 is a side cross-sectional view of an apparatus according to an aspect of the present invention.
  • Figure 15 is a perspective view of an apparatus according to an aspect of the present invention in use.
  • Figure 16 is a perspective view of an alternate embodiment of the present invention.
  • Figure 17 is a perspective view of an alternate embodiment of the present invention.
  • Figure 18 is an exploded view of an alternate embodiment of the present invention.
  • Figure 19 is a top view of an alternate embodiment of the present invention.
  • Figure 20 is a bottom view of an alternate embodiment of the present invention.
  • Figure 21 is a perspective view of an alternate embodiment of the present invention.
  • Figure 22 is a side view of an alternate embodiment of the present invention.
  • Figure 23 is a further perspective view of an alternate embodiment of the present invention.
  • Figure 24 is a further perspective view of an alternate embodiment of the present invention.
  • Figure 25 is a top view of the user interface of an alternate embodiment of the present invention.
  • Figure 26 is a representative GC trace showing identified peaks
  • Figure 27 is a chart showing the total impurities for the "first further set of samples" before and after processing with different jetting treatments according to an aspect of the present invention
  • Figure 28 is a chart showing the overall impurities in the distilled "second further set of samples" prepared by the laboratory before and after jetting treatment of the present invention.
  • Figure 29 is a chart showing the first distillation of the "second further set of samples" prepared by the laboratory, and effect of jetting treatment of the present invention.
  • Figure 30 is a chart showing the second distillation of the "second further set of samples"
  • Figure 31 is a table summarising GC analysis of samples produced according to an aspect of the invention.
  • Figure 32 is a table summarizing the mass balance on ethanol for water injection and redistillation of the "second further set of samples" prepared by the laboratory;
  • Figure 33 is a table showing various nozzle sizes tested at various pressures according to the present invention.
  • Figure 33 is a chart showing the results of the nozzle sizes tested as shown in Figure 31.
  • Figure 1 shows the representative steps in a method of reducing or eliminating a compound from a distillate.
  • the method of Figure 1 is adapted to produce a distillate which is, or may be used as an ingredient in, a beverage for consumption by a person.
  • a wash is prepared using a method as should be known to one skilled in the art.
  • Preparing the wash may involve adding ingredients or additives which may provide a desirable flavour or taste to the distillate or a beverage made therefrom.
  • a distillation process is performed using a distillation system. The details of the distillation process vary according to the size of apparatus, heat source, volume of wash, and alcohol
  • the distillation process may be performed using a system and apparatus therefor as described below. Alternatively, the distillation process may be performed using any suitable apparatus. The distillation process involves collecting the distillate produced.
  • step three a treatment substance in the form of water is jetted into the distillate collected at step 2.
  • An optional fourth step (step 4) may be used in which the distillate is redistilled after the treatment substance has been jetted therein.
  • the dosing apparatus (100) includes a main body (102) which defines a cavity (104).
  • the main body (102) generally has a frusto-conical shape with a lower portion (106) tapering towards a lower opening (108) into the cavity (104).
  • a skirt (110) is fitted over the lower portion (106).
  • the skirt (110) is formed from a flexible or otherwise deformable material, for instance, the skirt may be constructed of rubber.
  • a top plate (112) is secured to the top of main body (102) so as to provide an upper limit to the cavity (104).
  • the dosing apparatus (100) includes an extractor assembly (120), a valve assembly (130) and a controller (140).
  • the extractor assembly (120) is configured to generate a flow of air out of the cavity (104) in-use.
  • the extractor assembly (120) includes an extractor conduit (122) which is connected to an aperture (not shown) in the top plate (112).
  • a flow tube (124) is attached to the extractor conduit (122).
  • a flow generator (126) is attached to an end of the flow tube (124).
  • the flow generator (126) may be any device which can create a flow of air through the flow tube (124) such as a fan or impeller.
  • the flow generator (126) is attached to an inlet end (127) of the flow tube (124).
  • the flow generator (126) may also be attached to the outlet end (128) of the flow tube (124) or to any point between the inlet end (127) and the outlet end (128).
  • the valve assembly (130) includes a connector (132) which is configured to connect to a conduit (not illustrated in the figures) which connects the dosing apparatus (100) to reservoir of a treatment substance (not shown in the figures).
  • the connector (132) may be a screw thread, clip-fit, or other connector which can connect to a conduit such as a hose.
  • the valve assembly (130) also includes a valve (134) which may be ball-type valve or another valve as should be known to one skilled in the art.
  • An actuator (136) is configured to move the valve (134) between an open configuration and a closed configuration.
  • a fluid may flow through the connector (132) and the valve (134). This enables the dosing apparatus (100) to jet a treatment substance.
  • the valve (134) prevents fluid flow through the connector (132) and the valve (134).
  • the dosing mechanism includes a dispensing conduit (138) connected to the valve (134).
  • a nozzle (139) is connected to the dispensing conduit (138) at end distal to the valve (134).
  • the nozzle (139) may be omitted therefore the end of the dispensing conduit (138) simply provides an aperture through which fluid the treatment substance may flow.
  • the dosing apparatus (100) includes a ventilation arrangement configured to provide a flow of fresh air into the cavity (104).
  • the ventilation arranged is provided by an aperture (150) formed in the top plate (112).
  • the ventilation conduit (152) is connected to the aperture (150).
  • the ventilation conduit (152) has an outlet (154) which is distal to the aperture (150). In-use the ventilation conduit (152) facilitates fresh air or other gases being provided into the cavity (104) distal to an inlet (not illustrated) to the extractor conduit (122).
  • the controller (140) is connected to the actuator (136) and the flow generator (126). In-use, the controller (140) is configured to engage the actuator (136) to move the valve between the open and closed positions, to thereby control fluid flow through the valve. In addition, the controller (140) can turn the flow generator (126) on and off to create a flow of air out of the cavity (104).
  • the controller (140) may be pre-programmed with predetermined programs for the actuator (136) and / or the flow generator.
  • the programs may include instructions to control components of the dosing apparatus (100) to perform at least one of the steps of:
  • the controller (140) may have a timer function.
  • the timer function may be used to determine how long the flow generator (126) has been in operation, and / or how much fluid has flowed through the valve (134).
  • the timer may be an electronic circuit (not shown) within the controller (140).
  • the timer function may be provided by alternatives such as a flow controlled valve which determines the volume of an aliquot of treatment substance.
  • the controller may also be configured to enable a user to vary parameters of the dosing apparatus. This may enable optimisation of its use or to better suit a user's needs.
  • the controller may include a user interface (not shown) which may take the form of at least one of a key pad, one or more dials and one or more switches.
  • the interface enables a user to control operation of the dosing apparatus (100) such as selecting a pre-programmed program, entering the parameters of a customised program, or to switch the doing apparatus (100) on or off.
  • the controller (140) includes a display such as an LCD screen or LCD lights (neither shown).
  • the display is configured to display the current state of the dosing apparatus (100) e.g. whether a program is in progress or completed.
  • the dosing apparatus (100) includes a sensor (not shown) configured to determine a level of fluid in a container with which the dosing apparatus (100) may be used.
  • the sensor (not shown) is connected to the controller (140).
  • the controller engages the actuator (136) to move the valve to a closed position. This will reduce the chances of, or completely prevent, inadvertent overflowing of the container during use of the dosing apparatus (100).
  • FIG 15 shows a system (200) according to an aspect of the present invention.
  • the system (200) includes a dosing apparatus (100) as is discussed above, and a reservoir (202).
  • the reservoir (202) has a lid (204).
  • the dosing apparatus (100) is positioned so that the skirt (110) is inserted into an aperture (206) in the lid (204). In doing so, the nozzle (139) is inserted into a liquid (210) contained within the reservoir (202).
  • the outlet (154) is positioned above a top surface of the liquid (210).
  • the dosing apparatus (100) has a lower housing (160) formed by a lower portion (162) and a cover (164).
  • the lower portion (162) is attached to, or formed integrally to, the top plate (112).
  • the cover (164) may be releasably attached to the lower portion (162).
  • posts (166) are attached or integrally formed to, the lower portion (162) and / or the top plate (112).
  • the posts (166) include threaded apertures (not indicated) which are configured to engage with screws (not indicated in the Figures).
  • the screws may extend through corresponding apertures (not shown) in the cover (164) to thereby releasably secure the cover (164) to the lower portion (162).
  • the system (200) may be used to treat a distillate accordingly to the method described herein.
  • a distillate may be placed in the reservoir (202), and the lid (204) and dosing apparatus ( 100) positioned as described above.
  • a conduit is engaged to the connector to provide a supply of treatment substance for use by the system (200) in the method.
  • the controller (140) is used to select a mode of operation corresponding to the desired method to be used. This may determine the following:
  • FIG. 17 shows an alternative embodiment of a dosing apparatus (300) according to an em bodiment of the invention.
  • a ventilation arrangement (340) is provided by an aperture (342) in the top plate (112).
  • a flow generator (344) is connected to the aperture (342) and configured to in use generate a flow of air through the aperture, along the ventilation conduit, and out of the opening into the cavity (104).
  • the extraction assembly includes a conduit (350) attached to an aperture (not illustrated) in the top plate (112).
  • FIGS 18-25 show an embodiment of a dosing apparatus (400) according to a further embodiment of the present invention. Aspects of the dosing apparatus (400) are similar to those of the dosing apparatus (100) discussed above, and therefore like references refer to like components.
  • the dosing apparatus (400) is configured for use with a still (not shown in the Figures). For instance, the dosing apparatus (400) can be releasably attached to a reservoir (not shown in the Figures) forming part of the still (not shown). This should become clearer form the following discussion. However, it is also envisaged that the dosing apparatus (400) could be incorporated permanently into a separate vessel, or permanently attached to a vessel which is part of the still.
  • a ventilation arrangement (indicated generally by (440)) is provided by an aperture (442) on base plate (446).
  • a flow generator (444) is connected on top of aperture (442) and configured to in-use generate a flow of air through the aperture (442), along the ventilation conduit, and out of the opening into the still (not shown in the Figures).
  • the ventilation arrangement (440) includes a centrifugal fan (445), powered by brushless motor (402) and is configured to draw air from the air intake inlets (441) into centre of the base plate (446), through aperture (442). Air is also configured to be extracted via the aperture (442) from conduit (450).
  • An asymmetrically dispensing conduit (138) protrudes below the base plate (446) with a diameter outlet, and a controller (140) configured to give controlled periods of jetting treatments of a treatment substance to the dispensing conduit (138) via treatment substance inlet (432) on the dosing apparatus (400).
  • the centrifugal fan (445) is configured to create negative pressure inside the still (when in use), this in turn means fresh air will be drawn into the tank through the air intake inlets (441) and out through the conduit (450).
  • Treatment substance Inlet (432) includes a connector to receives the treatment substance which is to be jetted into the distillate.
  • the fan (445) plays a significant role in discarding impurities from the liquid as it assists in the extraction and discarding of air through conduit (450).
  • a standard hose (not shown) can be attached to the conduit (450), the other end of this hose can be extended out through a window or door to expel the vapors safely outside of the room.
  • Legs (410) are configured to securely attach the dosing apparatus (400) to a still (not shown).
  • Rubber liner (447) ensures the base plate (446) of the dosing apparatus (400) forms an effective seal onto the opening of the still (not shown).
  • Dispensing conduit (138) is configured to jet the treatment substance into the still during the treatment process.
  • the dosing apparatus (400) further includes a sensing means (indicated generally by (420)) to determine and measure the amount of liquid in the still.
  • the sensing means (420) is provided by a float switch (421).
  • a float switch (421) is attached to dispensing conduit (138) and is in communication with the controller and is configured to activate when the level of liquid in the still reaches a pre-determined level.
  • the float switch (420) can be adjusted via adjustor (448) to any position along the dispensing conduit (138).
  • a controller (140) is also provided and configured to function in a similar manner to the controller (140) discussed above in relation to Figures 9-11.
  • the controller (140) includes a user interface comprising a number of buttons and LED indicators to provide input and information on the operation of the dosing apparatus (400). Representative examples of the configuration of the buttons and LED indicators will now be discussed. However, this discussion should not be taken as limited to the following features in any way.
  • buttons are present on the user interface and are adjacent to one another.
  • the first button is labelled as “start/stop” and is configured to turn the dosing apparatus on or off.
  • the second button is labelled as “mode” and is configured to cycle the dosing apparatus (400) through pre-programmed running modes.
  • a series of LED indicators are also provided which provide the user with information on the operation of the dosing apparatus (400) and enable the user to select of the preferred jet treatment programme to undertake.
  • the controller (140) contains a number of pre-programmed options and can be configured to perform at least one of the steps of:
  • the controller (140) may have a timer function.
  • the timer function may be used to determine how long the flow generator (444) has been in operation, and / or how much fluid has flowed through the dispensing conduit (138).
  • the timer may be an electronic circuit (not shown) within the controller.
  • the timer function may be provided by alternatives such as a flow controlled valve which determines the volume of an aliquot of treatment substance.
  • the controller (140) may also be configured to enable a user to vary parameters of the dosing apparatus (400). This may enable optimisation of its use or to better suit a user's needs.
  • the dosing apparatus (400) is connected to a power source using a power cord (not shown in the Figures).
  • the dosing apparatus (400) is connected to a reservoir of a treatment substance (not shown in the Figures) using a hose (not shown) having a connector (neither shown), which engages to the treatment substance Inlet (432) on the dosing apparatus (400).
  • the distillate (containing high % alcohol) to undergo jet treatment is then poured into the still (not shown).
  • the sensing means (420) is set to a desired level by adjusting float switch (421) to the desired predetermined final level of distillate to be achieved after the treatment substance has been jetted into the distillate.
  • the dosing apparatus (400) can then be placed on top of the opening of the still.
  • the preferred treatment programme is then selected and inputted into the system via user interface on the controller (140), e.g. injection time, injection volume etc.
  • the jet treatment will start once the start button is pressed (on the user interface), the centrifugal fan (445) will initiate and will run continuously during the treatment process. Timed intervals between jetting (as pre-programmed) will allow bubbles (containing volatized substances) to dissipate, this process is assisted by the continuous running of the centrifugal fan.
  • the jet treatment process will continue until the still is filled to desired level, triggering the float switch (421) to automatically switch off the dosing apparatus (400).
  • the mixture can then be subjected to a second distillation process to concentrate and purify the alcohol. After the second distillation has been completed the alcohol will be ready for final dilution to the desired level for consumption.
  • the liquid mixture was cleared using a commercially available fining agent sold under the brand name Turbo clear.
  • the resulting liquid mixture was subsequently distilled in a commercially available distillation apparatus sold under the model name T500 to produce three distillate batches.
  • the distillate batches were blended together to form a base spirit with an alcohol content of 91.5% by volume.
  • Quantitative analysis of samples was performed by gas chromatography and flame ionisation by liquid injection, using a Shimadzu GC-2014 equipped with a flame ionisation detector.
  • the invention may also be said broadly to consist in the parts, elements and features referred to or indicated in the specification of the application, individually or collectively, in any or all combinations of two or more of said parts, elements or features.
  • samples prepared according to the method of the present invention have significantly reduce concentrations of acetaldehyde, ethyl acetate, acetal and n-propanol compared to the concentration of these compounds present in "untreated" samples.
  • treatment using water of a relatively higher temperature provided increased reduction in concentration of compounds as compared to treatment using relatively colder water.
  • Figures 5A and 5B the sequential jetting of aliquots of water leads to further decreases in concentration of compounds.
  • Figure 6 shows a strong correlation between sensory tests of samples to the use of jetting a treatment substance. While sample SP4 has lower concentrations of compounds than SP2, it has a higher sensory rating, indicating that effect of comparatively small differences in concentrations of compounds is not a discernible difference. Further testing
  • a first set of samples (“a first further set of samples”) was prepared and sent to a laboratory for analysis. These samples were subject to a period storage and transportation in order to deliver the samples to the laboratory for analysis.
  • a second set of samples (“a second further set of samples”) was prepared in the laboratory prior to testing. Both the first set of samples and the second set of samples were prepared using the method discussed below. The results of tests on the "first further set of samples" and the "second further set of samples" are shown in Figure 27.
  • a commercially available Essencia Express Still was used for the distillation process.
  • the still has a nominal capacity of 20L.
  • a short reflux zone in the lid was packed with steel wool and cooled with an external water jacket over a 100mm length.
  • the vapor phase was passed through a 150mm length water jacketed condenser section.
  • the still was topped up where required to 20 litre volume before distillation.
  • the still was switched on and heated to around 78 degrees Celsius to distill alcohol.
  • the cut off temperature was set at 86 degrees Celsius.
  • a sample from the "first further set of samples” was then subjected to a re-distillation process to produce a "subsequent sample” for further comparative analysis.
  • a "second further set of samples” was also prepared for comparative analysis. 42 litres of distilled water at 30°C was mixed in a brewing barrel with 12 kg of white sugar and 480 g of Still Spirits Turbo Yeast Classic 8 making a final volume of 51 litres. The yeast sachet listed bentonite as an ingredient. The manufacturers of the yeast recommend additional use of activated carbon during fermentation and addition of a proprietary flocculent before distillation, but these additional additives were not included in this fermentation wash.
  • the fermentation was run for 6 days in a room with air temperatures ranging from 19 to 22°C.
  • the fermentation broth was maintained at 27 to 30°C using a thermostat controlled immersion heater.
  • the final broth measured 10% ethanol by density, however this may under-represent the true content due to other dissolved components.
  • the broth was distilled by decanting into the still in two batches. Distillation was run until the temperature reached 83°C producing 5.59 kg of distillate with 79% ethanol content. A sample of the first 200 ml_ of distillate was collected for analysis before being re-mixed with the bulk distillate for further processing. Water injection trials on "first further set of samples"
  • the first further set of samples (approximately 20 litres) was prepared according to the method described above and combined into a single vessel to mix uniformly and decanted back into 4 L bottles.
  • the ethanol content was measured to be 86% by hydrometer.
  • a "subsequent sample” was also provided with the first further set of samples for testing, the "subsequent sample” is referred to herein as a redistilled (no water injection) sample from the same "first further set of samples”.
  • the dosing apparatus (400) was provided to the laboratory for testing, together with a vessel having a working volume of approximately 15 L.
  • the first jet treatment run on the 'first further set of samples' (referred to herein as 'low pressure') used a centrifugal pump on a closed loop to provide pressure and flow of distilled water to the treatment system. The maximum pressure achievable with this system was 1.5 bar.
  • the second jet treatment run on the 'first further set of samples' (referred to here as 'mains pressure') used a connection directly to the council mains potable water supply and was run at 5.5bar. Run details are provided in Table 1 below.
  • the treatment system was first calibrated to deliver approximately 1 kg of water per injection. Time between injections was set at 5.5 minutes for all the runs.
  • the bubbles remained throughout the entire water injection process.
  • the bubbles were very fine, but for mains pressure were larger.
  • the ethanol content was measured to be 16% by hydrometer after jet injection, consistent to within 1% of the ethanol content calculated from the degree of water dilution of the original spirit.
  • Re-distillation A still was used to distill the water injection runs (1, 2 and 3, 4), carbon filtered spirits and the commercial vodkas, and the second further set of samples after jetting of a treatment substance as discussed above.
  • the still was weighed during distillation.
  • the weight loss during the first step with the open still was 110 g, and in the second step 2.32 kg.
  • the total amount of weight lost from the still was 2.48 kg.
  • the residual liquid phase after re-distillation typically had an alcohol content of between 3 and 4 %.
  • Samples were analysed by gas chromatography via the method described below to determine the relative peak areas for different compounds.
  • a selection of 1-propanol standards were prepared in water to determine a calibration curve for 1-propanol. Peak areas were scaled to 40% ethanol concentration based on the ethanol concentration of the sample measured by hydrometer, and scaled to an equivalent 1-propanol concentration using a calibration based on the 1-propanol standards.
  • a standard calibration curve was prepared by analysing a range of dilutions of 1-propanol in water. Calibration samples were prepared on the day of analysis. Both analytical samples and calibration samples were analysed on the same day. The compounds present were quantified in terms of 1- propanol equivalent peak area. A typical analysis trace is shown in Figure 25. The saturated peak is ethanol, with minor peaks eluting later quantified.
  • Figure 27 shows the total impurities for the pre-prepared spirits before and after processing with different methods.
  • the mains pressure water injected and carbon filtered products had similar levels to the 'first further set of samples' indicating that the net effect was minimal for the supplied starting material.
  • this natural loss is an undesirable method and does not provide for a controlled means for the reduction of impurities in the distillate. Opening up the distillate for this natural loss of impurities to occur introduces the prospect of foreign matter being introduced into the distillate. Further, the speed of this loss of impurities is slow, taking a number of days or weeks to reduce down to the required level. This is in contrast to the present jet treatment process where only a number of hours is required to achieve the same reduction in compounds which could adversely contribute to the flavor profile of a beverage.
  • Figure 28 shows results of the "second further set of samples" prepared by the laboratory before and after jet treatment and after re-distillation. An intermediate sample after 9 of the 18 water jet treatments is also shown. The results indicate a reduction of about 35% in total impurities from the initial distilled sample.
  • Figure 30 shows the impurities in the re-distillation step after jet treatment of the "second further set of samples".
  • each of the components - including isoamyl alcohol is selectively concentrated and reduced from the initial distillate.
  • a mass balance on ethanol for water injection and re-distillation of the "second further set of samples" prepared by the laboratory is provided in Figure 32. 69% of the ethanol from the initial distillation is recovered in the injected and redistilled product. The remaining 31% is lost either in the residual aqueous phase or is lost by evaporation during the water injection process.
  • the calculation in Figure 32 indicates 5% is lost in the jet treatment process, however this calculation is very sensitive to the measured residual ethanol content in the aqueous phase which cannot be measured accurately using a hydrometer.
  • Weight loss measurements during jet treatment given in Table 2 above, indicate approximately 20 g of volatiles is vented with each one kg water injection. If this is predominantly ethanol and impurities (i.e. not water), then the overall loss of ethanol during the water injection process is estimated at 5-10%.
  • Nozzle size testing Further testing was conducted using various nozzle sizes to determine the effect of nozzle size on efficacy of the dosing apparatus (400).
  • the supplied base spirit was measured to be at 85% alcohol at 20 degrees Celsius using a Stevenson Reeves Spirit Meter. Preparation of the samples were in accordance with the same procedure described above.
  • the inventor proposes that this may be due to higher velocities of the jet treatment substance exiting the nozzle and / or increased turbulence of the flow of treatment substance created by the high flow rate.

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Abstract

La demande décrit des procédés, des systèmes et un appareil pour éliminer des composés à partir d'un distillat qui peuvent influencer négativement le profil d'arôme d'une boisson alcoolisée. Dans des formes préférées, une substance de traitement est projetée dans un distillat pour favoriser la volatilisation des composés. Un mode de réalisation préféré de l'invention concerne une unité qui est conçue pour projeter des aliquotes prédéterminées d'une substance de traitement dans un distillat.
PCT/NZ2018/050037 2017-03-26 2018-03-26 Procédé d'élimination d'un ou plusieurs composés à partir d'un distillat et systèmes et appareil associés WO2018182430A1 (fr)

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US2054006A (en) * 1934-09-06 1936-09-08 Edward Hyatt Wight Method of treating alcoholic beverages
US3698913A (en) * 1970-09-11 1972-10-17 Theodore Malinin Treatment of distilled alcoholic liquors
US20070248730A1 (en) * 2006-04-21 2007-10-25 Rick Wood Method and system for treating a distilled spirit
US20100297290A1 (en) * 2009-05-28 2010-11-25 Larue John Alternative method for rum production reducing pollution and bypassing upgrade of pollution controls
WO2014152924A1 (fr) * 2013-03-14 2014-09-25 Persedo LLC Conversion de contaminants dans un alcool- dans l'eau
JP5923679B1 (ja) * 2015-01-26 2016-05-25 有限会社情報科学研究所 還元発酵方法、還元発酵装置、酸化還元発酵方法、及び酸化還元発酵装置

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