GB2608607A - Hop essential compounds extraction and separation unit - Google Patents

Hop essential compounds extraction and separation unit Download PDF

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GB2608607A
GB2608607A GB2109677.1A GB202109677A GB2608607A GB 2608607 A GB2608607 A GB 2608607A GB 202109677 A GB202109677 A GB 202109677A GB 2608607 A GB2608607 A GB 2608607A
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tank
unit
solvent
reaction tank
mixture
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Jose Torrealba Victoria
Draghi Agustin
Mercado Daniel
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12CBEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C3/00Treatment of hops
    • C12C3/04Conserving; Storing; Packing
    • C12C3/08Solvent extracts from hops

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Abstract

A method of preparing extracts from plants and/or plant material, comprising combining whole hops, plant or plant material with water and ethanol under an inert atmosphere and heating the mixture to up to 70°C at a pH of 7.5-8.5; milling the mixture under an inert atmosphere to comminute the hops; maintaining or increasing the temperature to up to 70°C at a pH of 7.5-8.5; removing the milled hop solids to produce a homogenous extract; adjusting the pH of the extract to 4-4.5. A unit for performing the method is disclosed, the unit comprising a dosing tank 1 connected to a reaction tank 3; a solvent tank 2 connected to the reaction tank; a reaction tank where plant and/or plant materials are mixed with a solvent and a pH modifier 11 via inline injection; several pumps to drive the liquid-solid mixture through the unit; a colloid mill 13 and a heat exchanger 14 connected to the reaction tank to form a loop; a decanter 5 to separate solids from the liquid; a filter/separator 16 connected to a product tank; a second pH modifier 11.1 that modifies the pH of the mixture in the product tank; and a waste tank 9.

Description

Hop Essential Compounds Extraction and Separation unit
Description Field
The present invention relates to a method and a unit whereby essential compounds are extracted from plant and plant materials, for example the hop pellets or flowers to be used in the production of alcoholic and non alcoholic beverages, such as beer and similar products. Specifically, the invention relates to a method and a unit for the extraction of essential components from plant and plant materials such as hops.
Background
Active and desired compounds from the main ingredients (plant and plant materials) in commercial beverages can be extracted in order to be added at the desired stage of the production process. In the brewing process, hops are the key ingredient that adds aroma, flavor and bitterness. These essential qualities of hop oils, once extracted from the hops, can be further manipulated or used as desired by the manufacturer.
The main and most common method used in the addition of hops to hoppy beer, consists of the direct addition of hop pellets or flowers to the beer fermentation vessel (dry hop process). The hop is added to the fermentation tank at around 10 to 20 degrees Celsius at a pH between 3.5 and 5.5, depending on the specific fermentation parameters.
When hop pellets or flowers are directly added to the beer fermentation vessel, as mentioned above, there is a low level of extraction of desired essential compounds; this is mainly due to the physiochemical conditions of the beer tank, i.e. temperature, pH and the liquid-solid contact in the maturation and fermentation tanks. Most importantly when dry hop is added to the fermentation/maturation tank, the pellets/flowers absorb a considerable amount of liquid, in this case beer. As a result, the total amount of desired final product obtained from the process decreases.
Pellets/flowers when added to the fermentation/saturation tank have a humidity of 7% to 12% approximately. When removed from the fermentation/maturation tank the hops are in a supersaturated condition, which indicates a high level of absorption of beer product. For example, it has been observed that a dry hopped beer process with 6 grams per litre of hops, produces approximately 10% less beer than a non-dry hopped beer process in the same conditions; between 10 and 15 litres of beer are wasted per kilogram of hops added during the standard dry hop proceed.
When analyzing the residual hop waste, a high percentage of essential compounds (of aroma and flavor) are found. The essential compounds are not extracted in its entirety during the fermentation/maturation process as desired in the fermentation/maturation tank, which means that large quantities of hops are being disposed with a high level of essential compounds not extracted.
Brief Description
A method of producing a liquid with the essential and desired compounds present in plant and plant derived materials, particularly but not limited to hop essential compounds for the usage in alcoholic and nonalcoholic beverages, such as beer.
Plant and plant materials, for example hop pellets/flowers are mixed with a solvent in a reaction tank. The solvent, which original pH has been previously modified in some cases (see drawing 3, 4 and 5, note that for drawing 2 the pH modification is a manual process that occurs in the solvent tank), is pumped into the reaction tank.
The reaction tank, a colloid mill and a heat exchanger are connected in series to form a loop where the hops/plants are milled, and the temperature of the mixture is gradually increased. The mill decreases the size of the plant particles and the heat exchanger increases the temperature of the mixture.
After the first extraction, which occurs in the reaction tank, the liquid and solid phases are separated. The separation process comprises several steps to finally obtain the desired liquid enriched with essential compounds/oils, and a slurry containing the majority of the solid hop particles and a small amount of the enriched liquid solvent. Once the solid and liquid phases are separated, the liquid phase may be filtered and deposited in a collection tank. The liquid enriched with essential oils is then submitted to a pH modification, depending on the specific desired fermentation \maturation conditions, and used in the brewing/manufacturing process as required.
The mixture of solid particles and solvent (slurry) is then used in the second extraction process, where it is combined with a pure solvent and may be combined with additional hops. The parameters of the second extraction process may be similar to the first one, and the number of extraction phases depends on the efficiency of each phase, the size of the equipment and the configuration of the process. Once the last extraction is completed, the solids deposited at the bottom of the decanter are removed and deposited in a waste tank.
Drawings The different applications of this invention are presented below, including different levels of complexity and extraction capacity, from the most basic (drawing 2) to the most complex (drawing 5). The present invention can be adapted to breweries with different production capacities, from micro-breweries to big scale breweries, to improve their dry-hop process efficiency. The process includes two different phases and each phase includes different processes (see drawing 1). During phase one, an extraction phase, where the essential compounds are transferred from the solid material (hops, plant material, etc.) to the liquid solvent. During phase 2, a separation phase, the liquid solvent, enriched with essential compounds, is separated from the residual solid plant/hop particles.
Drawing 2 Drawing 2 shows the simplest application of the invention. In this case the extraction phase comprises a reaction tank (item 3) where the liquid solvent is injected at the specific temperature and pH, pH modification is a manual process that occurs in the solvent tank. The solid material (hops, plants, etc.) is then transferred from the hop dosing tank (item 1) to the reaction tank (item 3) to be mixed with the solvent in a closed recirculation loop.
Once the extraction process is complete, the liquid-solid mixture is transferred to the decanter (item 5), where the separation of liquid from the solids occurs by gravity. The liquid obtained has a high concentration of essential compounds, which can be used in the brewing process after the final pH modification. The solid particles, which contain a small amount of liquid with essential compounds, can be re-injected in the reaction tank for reutilisation or transferred to the waste tank (item 9) for disposal.
Drawing 3 Additional equipment is required for a higher scale operation as the one shown in Drawing 3, these are: colloid mill (item 13), heat exchanger PH1 (item 14), pH modifier tank (item 11 & 11.1), dosing pump (item 12 & 12.1), pump S (item 10) and filter/separator (item 16).
The process is similar to the one previously shown in drawing 2, the main differences are: * The solvent is injected into the reaction tank (item 3) by pump S (item 10), the pH modifier is then injected into the solvent stream from pump S (item 10) by the dosing pump (item 12 & 12.1).
* The temperature of the fluids in the reaction tank (item 3) is increased by recirculating the stream of fluids from the heat exchanger PHE1 (item 14). Additionally, the particle size of the solids are reduced by a colloid mill (item 13) connected in series between the reaction tank (item 3) and the heat exchanger PH1 (item 14).
* The solvent enriched with essential compounds is then pumped by pump 3 (item 7) through the filter or separator (item 16); the specification and capacity of the filter will depend on the requirements of the process.
* The fluid recovered from the bottom of the decanter, containing most of the remaining solid particles, is then pumped back to the reaction tank (item 3) by pump 2 (item 6) for further extractions.
This process is repeated until the desired concentration of essential compounds is obtained. Drawing 4 The process is similar to the one previously shown in drawing 3, the main difference is: * An additional heat exchanger PH2 (item 17) is included. This equipment allows for heat to be transferred between the stream of fluids from the heat exchanger PH1 (item 14) and the stream of solvent from pump S (item 10). As a result, the solvent is preheated before injection into the reaction tank (item 3).
Drawing 5 Drawing 5 shows a more complex application of the invention, which increases the efficiency of the extraction process, and therefore the concentration of essential compounds in the final product. The extraction is carried out using a multi-stage counter current continuous solid liquid extraction process. This application comprises two extraction phases and two separation phases in a series arrangement as follow: Extraction 1 -Separation 1-Extraction 2 -Separation 2. Additional phases can be included if required.
The process is similar to the one previously shown in drawing 4, the main differences are: * Fluids contained in the product tank (item 8.1) are driven back to the reaction tank 1 (item 3) by Pump R (item 18). In this way the extraction process is carried out using a solvent enriched with the essential compounds extracted from the hops/plants.
* The fluids from the bottom of the Decanter 1 (item 5) are driven to the reaction tank (item 3.1) by pump 2 (item 6); in this way the remaining essential compounds from the first separation process are used for further extractions, in combination with additional solvent from the solvent tank (item 2), which is driven by Pump S (item 10) and preheated by PHE 2 (item 17).
The number of extraction-separation phases to be used will depend on the desired efficiency of the process.
Detailed Description of the invention
The present invention is described below with specific references to the extraction of essential compounds from hop pellets or flowers. However, the present invention can be applied to the extraction of essential compounds from any plant, plant parts/materials or similar.
The present invention consists of a process and a unit, as shown in drawing 1. The invention comprises a solvent tank, several pumps, a reaction tank, a hop dosser tank, a colloid mill, several heat exchangers, decanters, a waste tank, a filter/separator and a final product tank.
Temperature The proposed invention comprises a method and unit whereby essential compounds from plant and/or plant materials, hop pellets or flowers are extracted using a solvent, preferably ethanol and water, at a maximum temperature of 70 degrees Celsius. It is not desirable to exceed this temperature given the boiling point of ethanol is 78 degrees Celsius. The operating temperature of the process is between 66 to 70 degrees Celsius. The process can also be operated in the following ranges of temperature: between 25 and 40 degrees Celsius, between 41 and 65 degrees Celsius and between 71 and 85 degrees Celsius A previous study, Kishimoto 20081, showed that the behavior of hop oils is altered during the wort boiling process; the majority of hop essential oils escape when the hops are submitted to 100 degrees Celsius or higher. The research also shows that the levels of myrcene and linalool fell rapidly during boiling; these are the essential compounds with the lowest boiling points. Note that Linalool is one of the most intense odor active components. Based on the above-mentioned results, we can conclude that in order to preserve key essential oils/compounds, which provide a wide range of aromas and flavor, the hops must not be exposed to a temperature higher than 70 degrees. Yield
This invention proposes a method and a unit whereby key essential compounds found in plant and/or plant materials, specifically hops, are extracted. These essential compounds provide aroma and flavour such as but not limited to: citrus, earthy, tropical fruits, sweet fruits, red fruits, pine, spice, flowers, watermelon, apple, pears, etc. These compounds are traditionally obtained at smaller concentrations during the dry hop process in order to obtain the before mentioned aromas and flavours. The yield of the proposed invention comprises a liquid with a concentration of hop essential compounds higher than the traditional dry hop process, and with higher extraction efficiency. The particular extracted essential compounds include, but are not limited to: 13-Myrcene Limonene Linalool a-Humulene Geraniol 8-Pinene Caryophyllene P-Farnesene 13-Eudesmol 8-Damascenone Alpha acids Beta acids The final output from the present method and unit is a homogeneous mixture to be added into the fermenter during the brewing process in order to provide flavour and aroma to alcoholic and non alcoholic beverages.
Pressure The entire system, except for atmospheric tanks such as the solvent tank and pH modifier tank, will be pressurized to a maximum of 0.5 bar.
The proposed invention comprises a pH modification of the solvent before the extraction phase. At this stage the normal pH level to be used is between 7.5 and 8.5, it can also be operated within the following ranges of pH: between 6 to 7.5 and between 8.6 to 10.
A second pH modification occurs after the separation phase, on the final product. At this stage the level of pH to be used is between 4 and 4.8.
1 T.K (2008, July 23). Hop-Derived Odorants Contributing to the Aroma Characteristics of Beer.
Process A method of producing an extract with the essential and desired compounds present in plant and plant derived materials, particularly hop essential compounds to be used in the production of alcoholic and non-alcoholic beverages. The present invention proposes the setting of different parameters throughout the extraction process to benefit from the biochemical reactions and characteristics of the essential compounds.
The method comprises the following steps.
Plant material/products, for example hop pellets/flowers are added to the hop dosing tank. The first addition of plant material is loaded on to the hop dosing tank and introduced into the reaction tank. Once the reaction tank is filled with the desired solvent, the plant material is introduced to the reaction tank gradually and mixed with the solvent using an agitator.
A solvent, which may be a mixture of ethanol and water is pumped to the reaction tank, the solvent's pH is increased via a pH modifier, e.g. potassium hydroxide, sodium hydroxide or sodium bicarbonate. It has been shown that the efficiency of the extraction of essential compounds is increased when the pH of the media is alkaline, specifically between 7.5 and 8.5, depending on the specific profile of the desired essential compound that is being extracted.
Ethanol extraction may be optimized by varying the levels of pH and/or temperature and/or strength of the ethanol solvent. It has been found that at a high pH, the carboxylic acids found in lupulin are soluble in lower concentrations of ethanol/water, and that under these conditions there is a more complete extraction of total hop essential compounds as shown by gravimetric determination. We assume that the essential compounds are constantly transforming during the brewing process; for example, geraniol can be transformed into citronellol and nerol by the yeast present in the brewing process, and alpha-terpineol, which can be formed from linalool and linalool is also a product of geraniol during fermentation (see drawing 6).
The reaction tank (item 3), colloid mill (item 13) and the heat exchanger (PHE 1, item 14) form a loop where the plants or plant materials, in this case hops, are milled and the temperature is gradually increased. The mill reduces the size of the plant particles, which increases the particle contact surface with a solvent. The heat exchanger increases the temperature in order to guarantee an increase in the solubility and extraction of the essential compounds of the plant material. This results in an increase in extraction efficiency.
As previously mentioned, the reaction tank, colloid mill and heat exchanger form a loop where constant recirculation is performed until the desired temperature of the fluids is reached. For example, an applicable recirculation schedule may be as follows: a first step of 20 minutes at 38 degrees Celsius, a second step of 35 minutes at 55 degrees Celsius and a third step of 10 minutes at 68 degrees Celsius.
After the first extraction, which occurs in the reaction tank (item 3), the liquid and solid phases are separated. The separation process comprises several steps to finally obtain the desired liquid enriched with essential components/oils, and a slurry containing the majority of solid hop particles and a small amount of the enriched liquid solvent.
For the extraction process depicted in drawing 2, the solid-liquid mixture is driven by pump 1 (item 4) from the reaction tank to the decanter (item 5), the solvent is added to the reaction tank at the extraction temperature. For the extraction process depicted in drawings 3, 4 and 5 the solid-liquid mixture is driven by pump D (Item 15) from the reaction tank (item 3) to the decanter (item 5), while going through a heat exchanger PHE 1 (item 14 drawing 3, 4 and 5), which increases its temperature. The solid and liquid phases are separated in the decanter by gravity, due to the differences in density between the solid particles and the liquid.
Once the solid and liquid phases are separated, the liquid phase is extracted via a piping system connected to one side of the decanter. This liquid enriched with especial oils is then driven by pump 2 (item 6) through a set of filters/separator (item 16) and finally to the product tank (item 8). The objective of filtering the liquid is to obtain a final product containing the minimum amount of solid particles possible.
The liquid enriched with essential compounds and/or oils deposited in the product tank is then submitted to a pH modification (item 11.1), the pH level will depend on the specific desired conditions of the brewing process.
The mixture of solid particles and solvent (slurry) deposited at the bottom of the decanter (item 5) is then driven by pump 2 (item 6) to start the second extraction process. In the second extraction process, the slurry is combined with a pure solvent and may be combined with more plant material. The parameters of the second extraction process may be similar to the first one, and the number of extraction phases depends on the efficiency of each phase, the size of the equipment and process configuration. Once the last extraction phase is completed, the solids deposited at the bottom of the decanter are removed and deposited in a waste tank (item 9).
Item 1: Hop Dosing Tank (Hopper unit).
Plant, plant materials or hops are introduced into the reaction tank (item 3) via one or more hop dosing unit (item 1).
A hopper unit is a funnel-shaped or tapered container, which function is to be a reservoir of solid matter to be used for extraction of aromatic compounds or desirable profile of flavors. The hopper unit is adapted to the reaction tank, so it discharges the solid material by gravity or any other driving system, e.g. pneumatic. One or more hopper units may be connected in series for this purpose.
As explained in item 3 (below), the reaction tank is a pressurized vessel, which isolates the solid-liquid mixture from the external environment. Thus, the hopper unit is adapted to be able to discharge the solid material into a pressurized environment, such as the Reaction tank.
The hopper unit comprises a pneumatic system, which permits the evacuation of all environmental oxygen once the solid matter to be used for extraction has been deposited in the reservoir, by creating a positive flow of gas, such as CO2, nitrogen or any inert non-oxidative gas, before the material is transferred to the Reaction tank. Thus, the oxidation of the solids within the system is reduced or eliminated.
Item 2: Solvent tank The purpose of this tank is to be a reservoir of liquid solvent at ambient pressure, which feeds the injection pump S (item 10).
The solvent may be a mixture of ethanol and water with less than 50% v/v, preferably below 20% v/v and ideally between 10% to 4% v/v. The ratio ethanol to water depends on the specific profile of the desired essential compound to be extracted. Solvent concentration may vary for every new cycle of reutilized hops coming from the decanter (item 5). Ethanol is the preferred solvent, however any solvent extract may be used; such as but not limited to water, isopropanol, industrial methylated spirit and acetone.
The solvent tank comprises a control system, i.e. a control valve, which allows for accurate control of the amount of liquid fed to the injection pump at all times. The liquid is evacuated through ports or openings connected to a piping system, which permits the circulation from the tank to the injection pump. The solvent tank may comprise an internal heating system to increase the temperature of the solvent before injection, to improve mixing and the extraction of aromas and flavors.
Item 10: Injection pump (Pump S) The purpose of this equipment is to pressurize the liquid solvent from the solvent tank (item 2) and inject it into the reaction tank (item 3).
This pump increases the pressure of the solvent, initially at ambient pressure, to the pressure of the reaction tank (item 3) for mixing with the solids to be extracted.
Item 3 3.a and 3.1: Reaction Tank (Hydration tank/Mixing tank) A reaction tank where a solid-liquid mixture is contained. The plant, plant parts, hops or hop pellets to be used for the extraction of aromatic compounds or desirable profile of flavors, are introduced in this tank, along with a liquid solvent, for hydration.
The purpose of the tank is to expose the plant, plant parts, hops or hop pellets to the liquid solvent. Thus the solid parts are wetted or hydrated in the tank; a mixing unit may be adapted to the tank to facilitate hydration.
The tank is adapted to be internally pressurized by a positive gas flow, which purpose is to isolate the solid-liquid mixture within the tank from the external environment. This prevents the oxidation of the solids within the tank, which could occur due to exposition to environmental oxygen. Thus, the tank is designed to permit initial positive gas pressurization, and to maintain a subsequent positive gas flow, such that positive internal pressure is maintained during operation. The gas flow system is designed to allow for control and monitoring of the amount and type of gas flowing within the tank at all times.
The transfer of solid material from the hop dosing tank/hopper unit (item 1) to the reaction tank is carried out through an opening located at the top of the tank, so the material is discharged by gravity or any other driving system, e.g. pneumatic.
A liquid injection system is also connected to the tank to allow for the injection of pressurized liquid solvents from pump S (item 10) into the tank.
The solids have a specific residence time within the tank to allow for the surface of plant, plant parts, hops or hop pellets to be fully wetted; this time depends on the tank capacity and the amount of solid-liquid mixture being processed. The mixture exits the tank, by the effect of gravity, through ports or openings connected to a piping system, which permits the circulation from the tank to the colloid mill (item 13).
Item 11: pH Modifier tank The purpose of this tank is to be a reservoir for the pH modifier to be injected to the solvent stream before the reaction tank (item 3). The liquid from this tank feeds an injection pump, which increases the pressure to the pressure of the Reaction tank.
Item 12: Dosing pump This pump increases the pressure of the pH modifier from ambient to the pressure of the Reaction tank (item 3).
Item 13 and 13.1: Colloid mill The purpose of this device is to reduce the plant particles size and mix them with the solvent to form a more homogeneous fluid, which increases the contact area between the solvent and the plant particles coming from the Reaction tank. A typical particle size after processing by the colloid mill is approximately 50 microns.
Item 14 and 14.1: Heat exchanger (PHE 1) The purpose of this equipment is to increase the temperature of the solid-liquid mixture at the output of the colloid mill (item 13). The output temperature of this equipment depends on the desired product to be extracted.
Item 17: Heat exchanger (PHE 2) The purpose of this equipment is to reduce the temperature of the solid-liquid mixture after recirculating the fluids back to the reaction tank (item 3), and before the separation process, which occurs in the decanter (item 5). Additionally, this equipment allows for the solvent to be heated up before injection into the reaction tank.
Item 15 and 15.1: Pump D The purpose of this equipment is to increase the pressure of the process fluids at the output of the second heat exchanger PHE-2 (item 17) and PHE-1 (item 14) to the specified pressure in the decanter (item 5). This pump drives the solid-liquid flow, ensuring that the mixture from PHE-2 and PHE-1 feeds the Decanter.
Item 5 and 5.1: Decanter This phase of the process comprises a decanter where the solid-liquid mixture is finally contained after the extraction process has been completed. The purpose of this container is to facilitate the separation, by gravity, and subsequent extraction of liquid and solid phases. The separation process mainly depends on the difference of density between both phases and the residence time of the mixture within the container.
After separation, the liquid phase rests at the highest level within the decanter, while the solid phase sits at the bottom. This allows the independent extraction of both phases; the solid phase is extracted from the bottom of the decanter, while the liquid is extracted from a higher level, which depends on the design of the equipment.
At this stage of the process, the liquid phase is a solvent enriched with oils, acids and other compounds extracted from the plants, plant parts, hops or hop pellets. The solid phase is mainly formed by the remaining plant particles, which were crushed and reduced in size in the colloid mill (item 13), and a small amount of enriched solvent.
Item 7 and 7.1: Pump 3 This equipment drives the extracted liquids, which contained a small amount of suspended solids, from the Decanter (item 5) through the Filter/separator (item 16) and finally to the product tank (item 8). It increases the pressure of the extracted liquids at the output of the Decanter to the specified pressure of the Product tank.
Item 16: Filter/Separator The purpose of this equipment is to remove solid particles from the solvent enriched with oils obtained after the separation process. The minimum size of the particles removed by this equipment depends on the specific requirements of the final product.
Item 8 and 8.1: Product tank The purpose of this tank is to be a reservoir for the final filtered product obtained from the extraction process, a solvent enriched with oils, acids and other compounds extracted from the plants, plant parts, hops or hop pellets.
The tank is adapted to be internally pressurized by a positive gas flow, which purpose is to isolate the liquid within the tank from the external environment. Thus, the tank is designed to permit initial positive gas pressurization, and to maintain a subsequent positive gas flow, such that positive internal pressure is maintained during operation. The gas flow system is designed to allow for control and monitoring of the amount and type of gas flowing within the tank at all times.
The liquid is evacuated through ports or openings connected to a piping system, which permits the extraction in isolation from the environment.
Item 11.1 and 11.2: pH Modifier tank The purpose of this tank is to be a reservoir of pH modifier to be injected to the product tank (item 8). The liquid from this tank feeds an injection pump, which increases the pressure to the pressure of the product tank.
Item 12.1 and 12.2: Dosing pump This pump increases the pressure of the pH modifier from ambient to the pressure of the product tank (item 8).
Item 6 and 6.1: Pump 2 The purpose of this equipment is to increase the pressure of the slurry at the lower output of the Decanter (item 5) to the specified pressure of the reaction tank (item 3). This pump drives the solid-liquid flow, ensuring that the mixture from the decanter (item 5) is fed back or recirculated to the reaction tank (item 3).
Item 9: Waste tank The slurry from the lower output of the decanter (item 5) is driven by pump 2 (item 6) into the waste tank for final removal at a later stage, depending on the capacity of the tank.
As said before, the solid phase is mainly formed by the remaining plant particles, which were crushed and reduced in size in the colloid mill (item 13), and a small amount of enriched solvent.
A valve downstream, Pump 2 allows for accurate control of the amount of slurry deposited in the tank. Item 4: Pump 1 (drawing 2) The purpose of this equipment is to increase the pressure of the process fluids at the output of the Reaction tank (item 3) to the specified pressure in the decanter (item 5). This pump drives the solid-liquid flow, ensuring that the mixture from Reaction tank feeds the Decanter.
Item 18: Pump R This equipment drives the extracted liquids from the Product tank (item 8.1) to the Reaction tank 1 (item 3) for recirculation. It increases the pressure of the extracted liquids at the output of the Product tank to the specified pressure of the Reaction tank.
Examples
The efficiency of the invention is further described by the examples below. Hop essential compounds were extracted according to key parameters described by the invention above.
For all examples below, the Citra hop variety was used as the raw material. This variety is one of the most widely used by beer manufacturers, note the process can be applied to any type of hop flowers, pellets or other organic raw material. For all examples an amount of 10 grams of hops per liter of solvent was used.
The sample obtained for each trial was analyzed by means of gas chromatography using the ASBC Hops-17 method. Specifically, three essential hop compounds were analyzed in the gas chromatography to determine the concentration obtained in each trial. The three essential compounds specified below were selected for analysis as these are deemed to be key compounds of interest in the production of hopped beverages, according to the details below: B-Myrcene: This is the most abundant essential oil found in hops, approximately 60% to 70% of total essential oils found in hops is p-Myrcene. This compound provides fruity and earthy aromas and flavors.
Linalool: This compound represents approximately 0.8% of total hop oil composition. It provides important woody, lavender, sweet orange and strong floral citrus aromas and flavors.
Geraniol: This compound represents approximately 0.3% of total hop oil composition. It provides important sweet, floral & rose and citrus aromas and flavors.
Example 1: Variation in temperature and time Example la: In a first trial an amount of hop pellets were mixed with a solvent consisting of ethanol and water 10% v/v at 40 degrees Celsius for a duration of 60 minutes in order to extract key essential compounds from the hop pellets.
In a second trial the same amount of hop pellets were mixed with a solvent consisting of ethanol and water 10% v/v at 15 degrees Celsius for a duration of 60 minutes in order to extract key essential compounds from the hop pellets.
Table 1: Concentration of key essential compounds obtained.
Compound mg/L (milligrams Amount (mg/L) extracted at Amount (mg/L) extracted at of essential compounds per temperature at 40 degrees temperature at 15 degrees Liter) Celsius Celsius 13-Myrcene 9.70 4.35 Linalool 0.043 0.03 Geraniol 0.25 0.014
Example lb:
In a third trial the same amount of hop pellets were mixed and stirred with a solvent consisting of ethanol and water 10% v/v at 40 degrees Celsius for a duration of 360 minutes in order to extract key essential compounds from the hop pellets.
In a fourth trial the same amount of hop pellets were mixed and stirred with a solvent consisting of ethanol and water 10% v/v at 15 degrees Celsius for a duration of 360 minutes in order to extract key essential compounds from the hop pellets.
Table 2: Concentration of key essential compounds obtained.
Compound mg/L (milligrams Amount (mg/L) extracted at Amount (mg/L) extracted at of essential compounds per temperature at 40 degrees temperature at 15 degrees Liter) Celsius Celsius P-Myrcene 34.94 10.85 Linalool 1.05 0.08 Geraniol 0.4 0.34 It was observed that at 40 degrees a higher solubility and extraction was obtained in both example la and lb for all three compounds. The most efficient extraction was obtained at 40 degrees Celsius through mixing and stirring for a period of 360 minutes. Example 2: pH variation For pH variation another set of trials were performed.
In a first trial an amount of hop pellets were mixed with a solvent consisting of ethanol and water 6.5% v/v with a pH of 8.5 at 20 degrees Celsius (room temperature) for a duration of 120 minutes in order to extract key essential compounds from the hop pellets.
In a second trial the same amount of hop pellets were mixed with a solvent consisting of ethanol and water 6.5% v/v with a pH of 6 at 20 degrees Celsius (room temperature) for a duration of 120 minutes in order to extract key essential compounds from the hop pellets.
Table 3: Chemical composition of essential compound extract obtained for three key essential compounds.
Compound p/I. (microliters of Amount (WL) extracted at 8.5 Amount (WL) extracted at 6 essential compounds per pH pH Liter) p-Myrcene 108.4 51.45 Linalool 1.19 0.25 Geraniol 0.29 0.13 It was observed that a higher extraction of essential compounds was achieved when an alkaline pH of 8.5 is used. Most importantly, it was observed that the extraction of linalool increases approximately 500% when using a pH of 8.5 compared to an extraction using a more acidic pH of 6. It was also observed that the extraction of Geraniol and p-Myrcene increased approximately 100% when using a pH of 8.5. It was then concluded that an alkaline pH provides higher concentration of desired essential oils than the more acidic pH of 5 or less used in the traditional dry hop process.
Definitions 1) Essential compounds / essential oils: Essential oils that can be extracted from hops, plant and plant material such as but not limited to: linalool, geraniol, a-terpineo1,13-citronellol and nerol.
2) Hop Pellets/flowers/hops: Raw material commonly used in the brewing process.
3) Plant and/or plant materials: by this term it is meant the flowers and/or pellets of the hop plant Humulus Lupulus, commercially known as hops.

Claims (1)

  1. Claims 1) A method of a flavour and aroma compound essential extracts from plants and/or plant material, said method comprising: i) combining whole hops, plant or plant material with a solvent consisting of water and ethanol at ambient temperature in an inert atmosphere to form a mixture, and increasing the temperature of the mixture to a temperature of up to 70°C and a pH of 7.5 to 8.5; ii) milling the mixture of step i) to comminute the hops, said milling step being conducted in an inert atmosphere to form a milled mixture; iii) maintaining or increasing the temperature of the milled mixture, wherein said temperature is up to 70°C, and wherein said milled mixture remains under an inert atmosphere and a p1-1 of 7.5 to 8.5; and iv) removing the milled hop solids to produce a homogeneous extract of hop flavour compounds.v) after which the pH is modified to a range between 4 and 4.5 2) A method, according to any of the preceding claims, to extract essential compounds from hops and plants and/or plant materials to be used in the production of alcoholic, non alcoholic beverages and similar products, comprising of an extraction phase and a separation phase.3) A method, according to any of the preceding claims, whereby the parameters for the extraction of essential compounds from hops, plants and/or plant materials are not set or defined by the fermentation parameters of beverages such as beer and/or similar products, including but not limited to temperature and pH.4) A method, according to any of the preceding claims, which may be adapted to increase the efficiency of the extraction process by adding additional extraction and separation phases in series arrangement. The extraction is carried out using a multi-stage counter current continuous solid liquid extraction process.5) The invention, according to any of the preceding claims, comprises a unit to extract essential compounds from hops, plants and/or plant materials to be used in the production of alcoholic, non alcoholic beverages and similar products. The unit comprises of: i) A dosing tank (1) connected to a reaction tank (3).ii) A solvent tank that holds a solvent (2) connected to the reaction tank (3).iii) A reaction tank (3) where plant and/or plant materials are mixed with a solvent whose pH has been modified by a pH modifier (11) via inline injection.iv) Several pumps that drive the liquid -solid mixture through the unit.v) A colloid mill (13) and a heat exchanger (14) connected to the reaction tank to form a loop.vi) A decanter (5) where the separation of liquids and solids occurs.vii) A filter/separator (16) connected to a product tank (8).viii) A second pH modifier (11.1) that modifies the pH of the mixture in the product tank (8).ix) A waste tank (9).6) The unit, according to any of the preceding claims, comprises one or more dosing tanks (hopper unit) (1) that may be connected in series, which is adapted through a pneumatic system to remove environmental oxygen and discharge solid material into the reaction tank (3) at an inert atmosphere.7) The unit, according to any of the preceding claims, comprises a solvent tank (2), which feeds the injection pump 5 (10) with a solvent, comprising a control system to control the amount of liquid fed to the injection pump S (10). The solvent tank may comprise an internal heating system to increase the temperature of the solvent before injection.8) The unit, according to any of the preceding claims, comprises a pH modifier tank (11), which is a reservoir for the pH modifier to be injected to the solvent stream before the reaction tank (3) in order to modify the pH of the solvent.9) The unit, according to any of the preceding claims, comprises a reaction tank (3) with an inert atmosphere, where a solid-liquid mixture is contained, the tank may contain a mixing unit (3.a).10) The unit, according to any of the preceding claims, comprises a colloid mill (13), which reduces the plant particles size.11) The unit, according to any of the preceding claims, comprises of a heat exchanger (14), which increases the temperature of the solid-liquid mixture at the output of the colloid mill (13).12) The unit, according to any of the preceding claims, comprises a reaction tank, a colloid mill and a heat exchanger that form a loop, where the mixture is recirculated in order to increase its temperature to a maximum of 70 degrees Celsius.13) The unit, according to any of the preceding claims, may comprise a second heat exchanger (17), which reduces the temperature of the solid-liquid mixture after recirculating the fluids back to the reaction tank and before the separation phase occurs. Additionally, this heat exchanger increases the temperature of the solvent before injection.14) The unit, according to any of the preceding claims, comprises a decanter (5) where the solid-liquid mixture is separated by gravity.15) The unit, according to any of the preceding claims, comprises a filter/separator (16), which removes the solid particles from the solvent enriched with oils obtained from the separation process.16) The unit, according to any of the preceding claims, comprises a product tank (8) with an inert atmosphere where the final filtered product is stored.17) The unit, according to any preceding claims, comprises a product tank (8), with an inert atmosphere where the final filtered product is stored, and where the liquid is evacuated through ports or openings connected to a piping system, which permits the extraction in isolation from the environment.18) The unit, according to any preceding claims, may comprise a second pH modifier tank (11.1), which acts as a reservoir of pH modifier to be injected into the product tank (8) in order to modify the pH of the filtered product.19) The unit, according to any of the preceding claims, comprises a waste tank (9) where the slurry from the lower output of the decanter is deposited for final removal.20) The unit, according to any preceding claims, comprises a loop whereby the slurry from the decanter (5) is recirculated and fed back to the reaction tank (3) for multiple cycles of recirculation.21) The unit, according to any of the preceding claims, may comprise a recirculation whereby the fluids from the bottom of the decanter 1 (5) are driven to the reaction tank (3.1) by pump 2 (6) so the remaining essential compounds from the first separation process are used for further extraction.22) The unit, according to any of the preceding claims, may be adapted to a smaller scale production process (drawing 2), which comprises a unit to extract essential compounds from plants and/or plant materials to be used in the production of alcoholic, non-alcoholic beverages and similar products. The unit comprises: * A hop dosing tank (1) connected to a reaction tank (3).* A reaction tank (3) where plant and/or plant materials are mixed with a solvent.* A decanter (5) where the separation of liquids from solids occurs.* A product tank (8) and a waste tank (9).* Several pumps that drive the liquid -solid mixture through the unit.23) The final output from the present method and unit according to any preceding claims is an homogeneous mixture that contains all hop essential compounds, to be added in the fermenter during the brewing process in order to provide flavour and aroma to alcoholic and non alcoholic beverages
GB2109677.1A 2021-07-05 2021-07-05 Hop essential compounds extraction and separation unit Pending GB2608607A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3891781A (en) * 1972-09-08 1975-06-24 Haarmann & Reimer Gmbh Process for the extraction of hops
US4490405A (en) * 1981-02-03 1984-12-25 Horst & Klotz Hopfenveredelung Gmbh Single step extraction of bitter principle and tannins from hops
WO2014147411A1 (en) * 2013-03-22 2014-09-25 The University Of Nottingham Novel agents and uses and methods for the preparation thereof
WO2020257764A1 (en) * 2019-06-21 2020-12-24 John I Haas, Inc Aqueous hop products and processes for imparting flavor and aroma to beverages

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3891781A (en) * 1972-09-08 1975-06-24 Haarmann & Reimer Gmbh Process for the extraction of hops
US4490405A (en) * 1981-02-03 1984-12-25 Horst & Klotz Hopfenveredelung Gmbh Single step extraction of bitter principle and tannins from hops
WO2014147411A1 (en) * 2013-03-22 2014-09-25 The University Of Nottingham Novel agents and uses and methods for the preparation thereof
WO2020257764A1 (en) * 2019-06-21 2020-12-24 John I Haas, Inc Aqueous hop products and processes for imparting flavor and aroma to beverages

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