Process for Producing an Aroma-Laden Gas, Aroma-Laden Gas, and Use of the Aroma-Laden Gas
20230112273 · 2023-04-13
Assignee
Inventors
Cpc classification
A23L27/115
HUMAN NECESSITIES
B01D15/40
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A process for producing an aroma-laden gas (10) comprises the following steps: a) providing a liquid phase (5), which contains a solvent and one or several aromatic substances (1, 2, 3); b) guiding through a solid phase extraction column (3) of the liquid phase provided in step (a) by obtaining the solid phase (35) laden with one or several aromatic substances; separating one or several aromatic substances from the laden solid phase by means of at least one gas (2) in a liquid and/or supercritical state; and optionally d) collecting the gas (10), which is laden with one or several aromatic substances (1, 2, 3).
Claims
1.-20. (canceled)
21. A process for producing an aroma-laden gas (10), comprising the following steps: a) providing a liquid phase (5), which contains a solvent and one or several aromatic substances (1, 2, 3); b) guiding the liquid phase (5) provided in step (a) through a solid phase extraction column (3) filled with a solid phase (30) and thereby obtaining a solid phase (35) laden with one or several aromatic substances; and c) separating an aromatic substance or several aromatic substances (1, 2, 3) from the laden solid phase (35) by a gas (2) in a liquid and/or supercritical state, wherein the solid phase (30) filled in the solid phase extraction column (3) is or comprises a nonpolar sorbent, which is based on hydrophobically modified polymer materials and/or silica gels, and wherein a concentration and extraction of the aromatic substance or the several aromatic substances takes place in an ethanol-free manner.
22. The process according to claim 21, wherein after step (c), a step d) collecting an aroma-laden gas (10), which is laden with one or several aromatic substances, is performed.
23. The process according to claim 21, wherein step (c) is performed directly in the solid phase extraction column (3).
24. The process according to claim 21, wherein step (c) is performed in a device (4; 40), which is suitable for this purpose, and wherein the laden solid phase (35) obtained in step (b) is removed from the solid phase extraction column (3) and is transferred into this device (4; 40).
25. The process according to claim 21, wherein the solvent is selected from the group consisting of water, solvents that are miscible with water, and mixtures of water with one or several solvents that are miscible with water.
26. The process according to claim 21, wherein the solid phase (30) filled in the solid phase extraction column (3) is or comprises a nonpolar sorbent, which is based on crosslinked polystyrenes as hydrophobically modified polymer materials.
27. The process according to claim 21, wherein the solid phase is laden completely or partially with one or several aromatic substances (1, 2, 3) in step (b).
28. The process according to claim 21, wherein the gas (2) is carbon dioxide (CO.sub.2).
29. The process according to claim 21, wherein the gas (2) is carbon dioxide (CO.sub.2) in a supercritical state.
30. The process according to claim 21, wherein before or after step (d), a step (d1) separation of an aromatic substance or of several aromatic substances (1, 2, 3) from the gas from the aroma-laden gas (10) by extracting an aromatic substance (1, 2, 3) or a mixture of aromatic substances (123) takes place.
31. The process according to claim 30, wherein a guide-through of the aroma-laden gas (10) through a membrane filter (6) takes place in step (d1), and wherein a filtered-off and aromatic substance-free gas (20) is optionally recycled.
32. The process according to claim 30 with the further step of aromatizing a food, pharmaceutical, oral hygiene or cosmetic product (7), wherein an aromatic substance (1, 2, 3), which is separated from the aroma-laden gas, is brought into contact with the product (7), so that at least one aromatic substance passes at least partially into the product and/or a packaging of the product.
33. The process according to claim 32, wherein the product (7) is a beverage or an oral hygiene liquid product, and wherein the aroma-laden gas (10) is introduced into the liquid product (7).
34. The process according to claim 32, wherein the gas (20) from the aroma-laden gas (10) remains at least partially in the product (7).
35. The process according to claim 32, wherein the gas (20) escapes or is removed from the product (7) prior to the product (7) being used as intended.
36. The process according to claim 32, wherein at least two aroma-laden gases, which differ in number, relative shares, concentration and/or type of the aromatic substances, are brought into contact with the product.
37. An aroma-laden gas (10) or aroma-laden solid phase (35), produced according to the process according to claim 21 at a temperature of maximally 40° C., wherein compared to a liquid phase (5) containing a solvent and one or several aromatic substances (1, 2, 3), it has essentially the same composition of and preferably also the same relative shares of aromatic substances (1, 2, 3), wherein the liquid phase (5) is selected from the group consisting of beverages, fruit juices, coffees, milk and milk products, teas, beers, condensate, rinsing water, a secondary stream and/or side stream and/or waste stream from processing of animal or plant starting materials, or from the production of food, a bypass stream from the processing of fruits, or from the production of beverages, and mixtures thereof, and, compared to a liquid phase (5) based on at least one below-mentioned fruit or based on at least one below-mentioned starting material, respectively, the aroma-lade gas (10) or the aroma-laden solid phase (35) contains at least one of the below-mentioned respective aromas (1, 2, 3) in the same relative shares as the liquid phase: Strawberry: ethyl butyrate, methyl butyrate, ethyl methyl butyrate-2, methyl capronate, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, methyl cinnamate, 3Z-hexenol, gamma-decalactone, Raspberry: alpha- and beta-ionone, 2E-hexenal, delta-decalactone, 3Z-hexenol, linalool, geraniol Apple: 2E-hexenol, 3Z-hexenol, 2E-hexenal, hexanal, ethyl butyrate, ethyl-2-methyl butyrate, beta-damascenone, Orange: ethyl butyrate, methyl butyrate, ethyl-2-methyl butyrate, octanal, hexanal, linalool, acetaldehyde, Grapefruit: nootkatone, ethyl butyrate, myrcene, linalool, p-menthenthiol-1,8, Lemon: citral, geraniol, beta-pinene, Cherry: benzaldehyde, 2E-hexenol, 2E-hexenal, hexanal, beta-damascenone, Peach: gamma-decalactone, delta-decalactone, 6-amyl-alpha-pyron, 2E-hexenol, beta-damascenone, linalool oxide, Banana: 3-methyl butyl butyrate, 3-methyl butyl acetate, hexanal, eugenol Pear: hexyl acetate, 3-methyl butyl acetate, 2E-hexenyl acetate ethyl-2E,4Z-decadienoate, Coffee: beta-damascenone, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, furfurylthiol-2, 4-vinylguaiacol, 3-hydroxy-4,5-dimethylfuran-2(5H)-on, isomeric isopropyl methoxy pyrazines, isomeric ethyl dimethyl pyrazines, Tea: 3Z-Hexenol, indole, methyl jasmonat,3-methyl-2,4-nonandion, jasmine lactone, beta-damascenone, methyl salicylate, Onion: dipropyl disulfide, dipropyl trisulfide, methyl propyl disulfide, Meat: 2E,4Z,7Z-tridecatrienal, 2E,5Z-undecadienal, 2E,4Z-decadienal, Rice: 2-acetyl-1-pyrrolin, octanal, nonanal, Milk: 1-octen-3-on, diacetyl delta-decalactone, delta-dodecalactone, decanoic acid, Tomato: 3Z-hexenol, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, beta-damascenone, dimethyl sulfide Mint: L-menthol, menthone, L-carvone, Beer: isoamyl acetate, 2-phenyl ethanol, ethyl butyrate, octanoic acid, Wine: wine lactone, 2-phenyl ethanol, linalool, linalool oxide. Passionfruit: ethyl hexanoate, linalool, gamma-decalactone, hexyl butyrate, hexyl hexanoate, 3Z-hexenyl butyrate, 3Z-hexenyl hexanoate Mango: dimethyl sulfide, alpha-pinene, ethyl butyrate, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, gamma-octalactone, gamma-decalactone, 3Z-hexenol Pineapple: methy-2-methyl butyrate, ethyl-2-methyl butyrate, ethyl hexanoate, methyl-(3-methylthio)propionate, ethyl-(3-methylthio)propionate, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, Honey: phenyl acetic acid, phenyl acetaldehyde, beta-damascenone Caramel: 3-hydroxy-4,5-dimethylfuran-2(5H)-on, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, 2-hydroxy-3-methyl-2-cyclopenten-1-on, Oat: 2-acetyl-1-pyrroline, (E,E,Z)-2,4,6-nonatrienal, vanillin, Malt: 2-methylbutanal, 3-methylbutanal, 2-acetyl-1-pyrrolin, vanillin, 3-hydroxy-4,5-dimethylfuran-2(5H)-on, isomeric isopropyl methoxypyrazines, isomeric ethyl dimethyl pyrazines, wherein further amounts of mercaptans (thioalcohols) and mono-, di-, tri-sulfides (thioethers), which are relevant from a sensory aspect, can be included in addition to the mentioned aromatic substance components.
38. The aroma-laden gas (10) produced according to the process according to claim 21, wherein the gas is carbon dioxide, and wherein the aroma-laden gas is produced at a temperature of 40° C. or less.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
[0129] In a flowchart,
[0130] The aroma-laden gas 10 from step c) can optionally be subjected to a step d), in which a collecting of the gas 10, which is laden with one or several romantic substances, is performed.
[0131] The aroma-laden gas can furthermore be subjected to a step d1), in which an at least partial separation of an aromatic substance or of several, in particular of all, aromatic substances 1, 2, 3 from the gas by extracting an aromatic substance or a mixture of aromatic substances takes place. Either a gas 10, which is enriched with aromatic substance or aromatic substances, or an essentially gas-free aroma or an essentially gas-free mixture of aromatic substances, respectively, is thus created.
[0132] The embodiments illustrated in
[0133] Step b) is illustrated in
[0134] The solid phase 30 is provided in a solid phase extraction column 3. The liquid 5 is guided through it.
[0135] After flowing through the solid phase extraction column 3, the liquid leaves the column 3. The liquid 50 is thereby depleted of aromatic substances, compared to the liquid 5, which flows into the column 3. In particular, the liquid 50 is essentially free from aromatic substances.
[0136] On principle, step c) is illustrated in
[0137] According to the illustration in
[0138] According to the illustration in
[0139] A container 8, into which the aroma-laden gas 10 is introduced and remains there, is provided, for example, for this purpose. The container 8 can be uncoupled from the feeding of aroma-laden gas in particular after reaching the desired fill amount, and can be stored, for example, in a closed manner until the aroma-laden gas 10 is used to aromatize a product.
[0140] In a further development, the aroma-laden gas can pass through a separating means 6, in which an aromatic substance or several, in particular all, aromatic substances are separated from the gas from the aroma-laden gas by extracting an aromatic substance or a mixture of aromatic substances in a step d1). An example for an embodiment of this type of step d1) is illustrated in
[0141] In the embodiment shown in
[0142] In an arrangement according to
[0143] In an embodiment, the guide-through of an aroma-laden liquid phase 5 through the solid phase extraction column 3 can take place first in an arrangement according to
[0144] The basic diagram of a preferred embodiment of the process is illustrated in
[0145] In the shown embodiment, the aroma-laden gas 10 formed thereby is transferred into a container 8 and is guided via a separating means 6. In the shown embodiment, aromatic substances are held back by the separating means, in particular in the container 8. After passing through the separating means 6, an aroma-depleted gas 20 leaves the separating means. It can be reused as gas 2, which is used to strip aromatic substances from the laden solid phase 35. Depending on conditions of the specific application, the gas 20 can be purified and/or temperature-controlled and/or compressed or relaxed, respectively, prior to being reused as gas 2. A dashed line is delineated in
[0146] In the context of the invention, it is also possible to use a separating means, which holds back the gas and which allows the aromatic substances to pass. The further use of the aromatic substances and of the gas are maintained thereby.
[0147] Depending on the type of product 7 and the structure and setup of the product, a product 7 itself can serve as “separating means” 6, as is shown in
[0148] According to the illustration in
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[0150] For this purpose, the adsorber material can be provided in particular in a separate packaging, which allows for a simple handling of the adsorber fill. A receptacle 34 is provided, for example, for this purpose.
[0151] The receptacle 34 is designed to receive 30 and/or 35 and can be detachably positioned in the solid phase extraction column 3 in such a way that at least steps b) and c) can be performed during operation, wherein the receptacle 34 is inserted in the SPE column 3, and the starting liquid 5 or the gas 2, respectively, flows through (aroma-laden) absorber arranged therein.
[0152] In the simplest case, this device can be formed by means of the receptacle 34 itself, as shown in
[0153] The basic diagram of a further preferred embodiment of the process is illustrated in
[0154] In order to facilitate the removal of the aroma-laden solid phase from the SPE column, the sorbent can be accommodated in the SPE column between two frits in a hose made of an inert material, for example of plastic or stainless steel, or in one or several plastic cartridges.
[0155] The removal of the solid phase from the solid phase extraction column and the transfer into a different device is thus made possible in a simple way.
[0156] Such a container, preferably made as hose in a simple way, has in particular at least one connection for introducing gas 2 and a connection for discharging aroma-laden gas 10.
[0157] In a further embodiment, a hose-like container 34 can be inserted into a device (not separately illustrated in
[0158] A container 34 inserted into such a device 4 is illustrated in
[0159] After performing step c), the process is continued according to the above- and below-described options. Aroma-laden gas can also be introduced directly into a produce from a container 34 as “hose”.
[0160] The device 4; 40 serves to receive the receptacle 34 and the connection thereof for performing step c). In its design, the device 4; 40 corresponds, for example on principle, to a solid phase extraction column, and is therefore designed in a pressure-resistant manner for step c).
[0161] In the context of the invention, the receptacle 34 can also be designed in such a way that step c) can be performed directly by using the receptacles 34. The process is carried out without the use of a device 4; 40 in this case.
[0162] Embodiments are illustrated in
[0163] A further option for aromatizing a product with a mixture of aromatic substances 1, 2, and 3 is illustrated in
[0164] The gas 100 and the gas 10 can be introduced into the product so as to overlap in time or one after the other, the aromatization can in particular also be performed at separate locations by means of several, here two, different gases. The gas 100 contains an aroma mixture of the aromas 1 and 2, which were stripped from the correspondingly laden solid phases 351, 352. In this embodiment, the gas 100 is generated by mixing the gases, which are laden with one aromatic substance 1, 2 each. For example, a mixture of the aromatic substances 1 and 2 can be produced first, and the aroma 3 can be extracted separately. The correspondingly laden adsorber material 353 is used in a casing 34 in a connecting device 4.
Exemplary Embodiment 1
[0165] For test purposes, a beer was used as starting solution, which was diluted with water. On principle, any dilutions can be used, for example a dilution by the factor 1:4. In the exemplary embodiment, the beer was diluted with water by the factor 1:20.
[0166] According to step b) of the process, this starting solution was guided through an SPE column. This solid phase extraction column was laden with the adsorber resin LEWATIT® VP OC 1064. This adsorber resin is a crosslinked polystyrene with pore diameters according to manufacturer information of between 5 and 10 nm and a specific surface BET 800 m.sup.2/g.
[0167] An SPE column with a length of approx. 0.5 m and an inner diameter of approx. 20 cm was used. The flow speed during the guide-through of the diluted beer is calculated and set on the basis of the inner diameter of the column and the specification of the adsorber resin. The total amount of the liquid, which is to be guided through, until the absorption capacity of the adsorber resin is depleted, depends on the concentration of the aromatic substances in the starting product. Based on his experience, the person of skill in the art can estimate a possible amount, and then determines the exact maximum capacity by means of tests.
[0168] The laden solid phase, thus the adsorber resin laden with aromatic substances from the diluted beer, was removed from the SPE column and was temporarily stored in a vacuum bag.
[0169] As step c), the adsorber resin laden with aromatic substances from the beer was subjected to an extraction with supercritical CO2. The composition of the aromatic substance composition in the laden solid phase was eluted with ethanol and was examined. In the context of measuring inaccuracies, the concentration of aromatic substances in the ethanol corresponds to the concentration in the CO.sub.2. The beer had an aroma mixture comprising essentially 2-phenylethyl alcohol, octanoic acid, 3-methyl-1-butanol, 2-methyl-1-butanol, hexanoic acid, 3-methylbutyl-acetate, decanoic acid, isobutanol, octanoic acid ethyl ester and ethyl acetate. The composition of these aromatic substances in the laden solid phase resulted from this as follows:
TABLE-US-00002 Aromatic substance Ppm %% by weight Log P 2-phenylethyl alcohol 1772 0.39048899 1.36 octanoic acid 1232.6 0.27162344 2.9 3-methyl-1-butanol 806.2 0.17765927 1.22 2-methyl-1-butanol 297.1 0.06547081 1.22 hexanoic acid 201.3 0.04435973 1.84 3-methylbutyl acetate 68.9 0.01518323 2.12 decanoic acid 51 0.01123868 3.96 isobutanol 47.2 0.01040129 0.69 octanoic acid ethyl ester 31.5 0.00694154 3.9 ethyl acetate 30.1 0.00663302 0.71
[0170] The aroma-laden gas obtained by means of the extraction with supercritical CO.sub.2 has a typical “smell of beer”.
Exemplary Embodiment 2
[0171] A CO.sub.2 laden with beer aromas according to Exemplary Embodiment 1 was produced. According to step d1) of the process, the aromatic substances were then separated from the CO.sub.2 extract stream via a high-pressure membrane as separating means.
[0172] It was thus possible to separate the aromatic substances from the aroma-laden CO.sub.2 and to enrich them, namely at pressures in the range of between approximately 130 bar to approximately 160 bar, and a temperature in the range of from approximately 60° C. to approximately 14° C., preferably at a temperature of approx. 70° C. when using a membrane made of “Teflon® AF2400”.
Exemplary Embodiment 3
[0173] A CO.sub.2 laden with beer aromas according to Exemplary Embodiment 1 was produced, and the aromatic substances were separated from the CO.sub.2 extract stream via a high-pressure membrane as separating means according to step d1) of the process. The CO.sub.2, which was thus filtered off and which is aromatic substance-free, was then recycled for performing step c) of the solid phase extraction.
[0174] The person of skill in the art can see that the invention is not limited to the above-described examples, but, on the contrary, can be varied in a variety of ways. The features of the individually illustrated examples can in particular also be combined with one another or can be exchanged with one another
LIST OF REFERENCE NUMERALS
[0175] 1, 2, 3 aromatic substance [0176] 123 mixture of aromatic substances [0177] 10; 100 aroma-laden gas [0178] 2 gas, in particular gas in the liquid or supercritical state; CO2 [0179] 20 essentially aromatic substance-free gas; gas after passing through a separating step d1); recovered gas [0180] 3 solid phase extraction column; SPE column [0181] 30 solid phase in the essentially unladen state [0182] 34 receptacle or container for receiving 30 and/or 35 [0183] 35 solid phase laden with aromatic substance or aromatic substances [0184] 4; 40 connecting device for receiving 34 for performing step c) [0185] 5 liquid phase; starting material; condensate, rinsing water, secondary stream, side stream, waste stream, or bypass stream from the processing of fruit or from the production of beverages [0186] 50 liquid depleted of aromatic substances [0187] 6 separating means; filter; membrane; CO2-specific membrane; CO2-specific filter [0188] 7 product [0189] 8 container