EP0081231A2 - Process for the production of aromatic substances from a tobacco extract - Google Patents
Process for the production of aromatic substances from a tobacco extract Download PDFInfo
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- EP0081231A2 EP0081231A2 EP82111300A EP82111300A EP0081231A2 EP 0081231 A2 EP0081231 A2 EP 0081231A2 EP 82111300 A EP82111300 A EP 82111300A EP 82111300 A EP82111300 A EP 82111300A EP 0081231 A2 EP0081231 A2 EP 0081231A2
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- tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
Definitions
- the invention relates to a new product, a clear tobacco aroma oil, free of polyphenols, resins and waxes, with a reduced (reduced) nicotine content of 5 to 50% relative (based on the tobacco from which the tobacco aroma oil originates) and with which the typical tobacco smell used in each case.
- the invention relates to a method for separating clear tobacco aroma oil from tobacco extract and its use according to the claims.
- the flavoring of tobacco plays a special role in the manufacture of tobacco products. Attempts to partially or wholly obtain the tobacco aroma oil typical of the respective tobacco from aroma-strong tobacco or tobacco waste in order to add it to other, low-aroma tobacco of the same provenance have so far failed because an absolute (clear) tobacco aroma oil free of resins and waxes with reduced nicotine content.
- DE-OS 21 28 779 describes a process for the production of flavorings and the. Conversion of aroma precursors from tobacco, by extracting the tobacco with one or more solvents which are in the eluotropic range between trichlorethylene and ethyl acetate and activating the aroma precursors from the extract obtained by heat treatment between 110 and 180 °.
- the aroma products obtained by this process represent a wax-like, resinous mass which contains all waxes and resins as well as polyphenols and almost all nicotine of the starting product.
- DE-OS 21 42 205 describes a process for the selective, aroma-preserving extraction of nicotine from tobacco, - in the first stage of which the aroma is extracted from the dry tobacco by treatment with dry, supercritical gases (for example CO 2 ), which is then temporarily removed from the Separation container B remains until the tobacco in container A has been removed from the nicotine by a second process stage with the help of moist CO 2 , which is then separated out in container D.
- the flavoring substances in container B are dissolved with, for example, supercritical CO 2 , returned to container A and deposited there on the tobacco.
- This process is expensive in terms of tobacco aroma extraction and exploitation and is inefficient because the product obtained in the first stage is not a clear liquid tobacco aroma oil that can be separated from resins and waxes, but is a paste that contains almost all undesirable waxes and resins of the starting product and undesirable ones Includes polyphenols.
- these wax and resinous substances prevent the even distribution and aroma transfer when rearomatizing a tobacco to be loaded.
- One of the disadvantages of the polyphenols is that they impair the smoky taste.
- DE-OS 28 44 781 describes a method for the extractive treatment of plant and animal material, i.a.
- the object of the present invention is to obtain a clear, absolute tobacco aroma oil which contains almost all the aroma substances of the starting product qualitatively and quantitatively, is free from resins, waxes and polyphenols and whose nicotine content - compared to the starting product - is greatly reduced.
- tobacco is fermented tobacco leaves, stems, stems or dust, and tobacco waste.
- tobacco primary extract is an ethyl acetate with customary organic solvents, in particular benzene, toluene, methanol, ethanol, n-propanol, methyln-propane, diethyl ether, acetone, n-propane, n-hexane, cyclohexane, petroleum ether, dichloromethane or Trichloromethane, or extract made with mixtures of these solvents.
- a primary extract according to the present invention further provides a C0 2 extract, that is, with the aid of CO 2 produced as a solvent extract.
- Adsorbents for the purposes of the present invention are all common adsorbents, in particular activated carbon, aluminum oxide, magnesium oxide, sodium aluminum silicate, bleaching earth, bentonite, silica gel, diatomaceous earth, zeolitic molecular sieves etc.
- Tobacco aroma oil in the sense of the present invention is an absolutely clear, tobacco aromatic, oily liquid at normal temperature - free of resins and waxes, free of polyphenols, with a reduced nicotine content of 5 to 50% relative (in particular 10 to 40% relative) based on the tobacco from which the tobacco extract originates - which shows no clouding or precipitation when 95% by weight ethanol is added.
- the preparation of the tobacco primary extract used according to the invention consists in particular in extracting the tobacco in one of the abovementioned solvents or (in the case of organic solvents) in a solvent mixture.
- 1 part by weight of pre-shredded tobacco is preferably extracted with about 3 to 30 parts by weight of one of the solvents mentioned (preferably CO 2 , n-hexane or dichloromethane).
- the primary extraction takes place for at least 10 minutes and at most 10 hours, preferably for 1 to 5 hours.
- the primary extraction takes place under normal pressure conditions. If organic solvents are used, the primary extraction takes place under normal pressure conditions. If CO 2 is used in the primary extraction, the pressure and temperature conditions in the extraction container and separating container, as well as the extraction time and CO 2 flow rate are identical to those specified below in connection with the (single-stage) secondary extraction (see page 10, Lines 5 to 19, page 11, lines 12 to 32).
- the evaporation is preferably carried out under reduced pressure, particularly preferably at about 15 torr. If C0 2 is used, the evaporation takes place in the separating container, as already explained above, under the pressure and temperature conditions as specified below for the (single-stage) secondary extraction.
- a tobacco primary extract obtained in this way contains, among other things. Polyphenols, resins / waxes, nicotine and, as the inventor has determined, is in an easily accessible form which is particularly suitable for the subsequent secondary extraction (with CO 2 ),
- the tobacco primary extract obtained is now according to the invention. mixed intensively with an adsorbent until there is an even distribution between extract and adsorbent.
- Particularly preferred adsorbents are: sodium aluminum silicate, bentonite, magnesium oxide or zeolitic molecular sieves.
- the mixing ratio of extract: adsorbent is variable and can be adjusted depending on the consistency of the extract, the density and particle size of the adsorbent and the desired consistency of the mixed product. In general, a mixture ratio of extract: adsorbent between 1: 0.1 to 1:10 is sufficient; preference is given to a powdery extract mixture with an extract: adsorbent mixing ratio of 1: 0.3 to 1: 6.
- the extract / adsorbent mixture should not fall below the ratio 1: 0.1, because the adsorbent used according to the invention, the dissolving of the flavoring substances in the subsequent secondary extraction with CO 2 (in the extraction container) and the separation in the separating container as clear absolute, easily separable from resins and waxes Tobacco aroma oil significantly influenced.
- a mixture ratio of more than 1:10 also gives a good detachment and separation of the tobacco aroma oil, although a larger pressure vessel volume has to be accepted.
- the mixture of primary extract and adsorbent is' in a first pressure vessel (extraction vessel), preferably high pressure vessel, with CO 2 under certain pressure and Treated temperature conditions until all the aromas are present in the second pressure vessel (separator vessel) downstream of the extraction vessel as an oily liquid that can easily be separated from resins and waxes.
- extraction vessel preferably high pressure vessel
- second pressure vessel separator vessel
- This secondary extraction with C0 2 by the method of the invention is achieved by supercritically using the C0 2 used for extracting the extract / adsorbent mixture with respect to pressure and temperature (> 73 bar and> 31.3 ° C) or with respect to Keeps pressure and temperature subcritical ( ⁇ 73 bar and ⁇ 31.3 ° C) or supercritical with regard to pressure (> 73 bar) and subcritical with regard to temperature ( ⁇ 31.3 ° C).
- pressures from 85 to 250 bar and temperatures from + 35 ° C to + 90 ° C are preferred.
- pressures from 25 to 70 bar and temperatures from + 5 ° C to + 25 ° C are preferred.
- pressures from 85 to 200 bar and temperatures from + 10 ° C to + 30 ° C are preferred.
- an additional CO 2 extraction step can be carried out at a lower level between the claimed primary extraction and the claimed secondary extraction Temperatures are interposed.
- the extract obtained in the primary extraction and mixed with the adsorbent is treated beforehand at CO 2 extraction temperatures from -25 ° C. to + 5 ° C.
- nicotine and other secondary alkaloids are almost exclusively dissolved out of the primary extract / adsorbent mixture and in the separation container eliminated.
- the nicotine obtained is removed from the separation container before the subsequent secondary extraction (aroma extraction) with CO 2 begins.
- the separation conditions in the expansion tank are decisive for the quality and quantity of the product obtained according to the invention.
- the relaxation pressures and relaxation temperatures are expediently in the subcritical range of C0 2 (subcritical pressure / subcritical temperature). Pressures of 45 to 65 bar and temperatures of 15 to 30 ° C are preferred; pressures of about 50 to 55 bar and temperatures of 20 to 25 ° C. are particularly preferred.
- the separation in the expansion tank is preferably carried out with simultaneous pressure and temperature lowering than the pressure and temperature conditions prevailing in the extraction tank .;
- the amount of CO 2 flowing through the extraction container and the duration of the flow are also decisive for the procedure according to the invention.
- Treatment times totaling 0.5 to 8 hours, preferably 1 to 5 hours, particularly preferably 2 to 4 hours are expedient;
- a total amount of CO 2 is expedient from 0.3 to 35 kg / hour, preferably 3 to 30 kg / hour, particularly preferably 5 to 15 kg / hour, based on 1 kg of untreated tobacco.
- a special characteristic of the tobacco aromatic oil obtained according to the invention is also that it has the tobacco smell typical of the starting tobacco used in each case. This characteristic clearly distinguishes it from all tobacco extracts known to date, because none of the conventional tobacco extracts made it possible to produce the typical smell of the respective starting tobacco. Based on this characteristic feature of the tobacco extract obtained according to the invention, it can be assumed that its material composition is completely new compared to the prior art.
- the tobacco flavor is separated and obtained as a clear and absolute oil, and this. with measures that are easy to carry out and a particularly efficient result. No indication of the prior art could be found either for this process as such or for the product obtained.
- the tobacco constituents which are obtained by primary extraction according to the procedure according to the invention, behave in a mixture with a powdery adsorbent and subsequent secondary extraction (with C0 2 ) with respect to their viscosity, their solubility and separation ratios very different from the same Ingredients that are only subjected to primary extraction (including CO 2 primary extraction), e.g. from tobacco leaves.
- Aroma oils obtained in a conventional manner were only produced by steam distillation on a laboratory scale.
- the oils obtained were of numerous foreign smells, e.g. Accompanied by chamomile, caraway, peppermint, valerian and amyl alcohol, which are probably caused by artifacts.
- the yield of such tobacco oils was about 0.1 to 0.2%.
- the tobacco aroma oil obtained according to the invention which has the typical and pure smell of the starting tobacco used in each case, stands in clear distinction from this. This is how it smells, for example the Havana tobacco flavored oil obtained from Havana tobacco, the Kentucky tobacco flavored oil obtained from Kentucky tobacco. In a similar way, aromatic oils obtained from Virginia, Orient or Burley tobacco show the very typical and pure smell of the respective tobacco variety. Because of this particular characteristic, which is clearly different from the prior art, it should be noted that the tobacco aromatic oil obtained according to the invention is completely new in its material composition compared to the products of the prior art.
- the tobacco aromatic oil obtained in the manner according to the invention is free from foreign odors, free from polyphenols, resins and waxes, has a reduced nicotine content which is only 5 to 50% relative to the tobacco leaves used, and is obtained in yields of 0.8 to 2%. Get 5% (absolute oil).
- the yield in the aromatization of tobacco i 50 ppm of the product obtained according to the invention, for example from Havana tobacco, already shows the same yield and intensity in the aroma as about 250 ppm of an aroma product from Havana tobacco obtained by known methods of steam distillation.
- the invention further relates to the use of the tobacco aromatic oil obtained according to the invention for flavoring
- Tobacco, or tobacco products this flavoring being able to be carried out either directly by tobacco or by aromatizing porous carrier material or tobacco adhesive material.
- the tobacco aromatic oil according to the invention is not only suitable for flavoring weak-flavored tobacco or reconstituted tobacco by means of sauces ("casing"), but is also particularly suitable as a "top flavor".
- porous carrier materials that are in contact with tobacco or tobacco products.
- porous support materials can e.g. in the form of pieces of paper or clay, dummies, inner packaging material (e.g. for boxes, bags, etc.).
- a further embodiment of flavoring using the tobacco aromatic oil according to the invention is also the addition to adhesive material for tobacco products.
- adhesives as are commonly used for tobacco products, e.g. Adhesives for cigar covers, cigarette paper, etc.
- the tobacco aroma oil obtained according to the invention can be used to decisively influence any fluctuations that occur during production (quality differences or other differences in the smoky taste) of the tobacco.
- the amount of tobacco aromatic oil used to flavor tobacco or tobacco products can vary depending on the nature of the tobacco and the desired flavoring.
- aroma oil obtained according to the invention from, for example, Havana tobacco, 25 to 100, particularly preferably 40 to 60 mg of tobacco aroma oil per are preferably used for loading kg of tobacco, ie 25 to 100 ppm, preferably 40 to 60 ppm.
- Liquid CO 2 is removed from the tank 1 in the subcritical pressure and temperature state.
- the heat exchanger 2 sets the CO 2 to the desired subcritical or supercritical temperature and the desired supercritical or subcritical pressure is achieved with the aid of the high pressure pump 3.
- the CO 2 enters the extraction container 4, where the extraction of the mixture of primary extract and adsorbent takes place.
- the extraction container 4 is filled and emptied with product discontinuously by opening and closing. the head opening after each extraction.
- the pressure prevailing in the extraction container is determined with the pressure sensor 14.
- the separation of the tobacco ingredients dissolved in the C0 2 is initiated by the pressure control valve 8 and supported by lowering the temperature in the heat exchanger 9.
- the extracted tobacco components separate into a clear tobacco aroma oil and a waxy, resinous nicotine product, which are either removed continuously through the valve 17 or after the extraction has ended by opening the tank 10.
- opening the valve 5 also causes the extraction side of the Device relieved of pressure.
- the C0 2 emerging from the expansion tank 10 during the extraction is recirculated via line 11.
- the device can be controlled by hand or by means of the electrical control unit 12, the inputs of which are the temperature measured with a temperature sensor 13 in the extraction container 4, the pressure measured with pressure transducers 14 and 15, and the CO 2 streams emerging from the pressure containers 4 and 10 as well as the flow rate measured with the flow meter 7.
- the pressure control valve 8 and also the cooling capacity in the heat exchanger 9 are set as a function of these measured values.
- Havana tobacco 1000 g Havana tobacco (water content 6.5%, nicotine content 1.27%) are crushed in a knife mill and exhaustively extracted in 10 liters of dichloromethane - and the solvent is evaporated off at a vacuum of 15 torr.
- the mixture was treated for 120 minutes in a closed ochrikextratechnischs understandinger H at a pressure of 230 and a temperature of 65 ° C with CO 2.
- the pressure on the relaxation side was 50 bar and the temperature was 24 ° C.
- the flow rate of CO 2 is 6 kg / hour.
- the yield of clear, absolute tobacco aroma oil was 2.25% of the tobacco used.
- the nicotine content was 19.92%, which is 35% relative to the nicotine present in the tobacco.
- the yield of the resin / wax deposit was 1.76%, the nicotine content 43% absolute, which is 60% relative to the nicotine present in the tobacco.
- the tobacco aroma oil obtained was free from resins and waxes and showed no precipitation and no clouding when 95% by weight ethanol was added.
- Treatment duration 3 hours.
- Flow rate CO 2 8 kg / hour.
- this mixture is subjected to a secondary extraction with CO 2 .
- the tobacco aromatic oil obtained was free from resins, waxes and polyphenols and had the smell typical of Kentucky tobacco. No turbidity occurred when 95% by weight ethanol was added.
- the yield of clear tobacco aroma oil was 1.55% of the tobacco used, the nicotine content was 9.55% absolute, which is 5.2% relative to the nicotine present in the tobacco.
- the tobacco aroma oil obtained was free of resins and waxes, pointing to the addition of 95 G ew .-% - ethanol no precipitate and no turbidity.
- the pressure on the relaxation side was 50 bar, the temperature + 20 ° C.
- the flow rate of CO 2 is 10 kg / hour.
- the yield of clear tobacco aroma oil was 1.2% of the tobacco used, the nicotine content was 23.2% absolute, which is 19.17% relative to the nicotine present in the tobacco.
- the resin / wax deposit had a nicotine content of 57.2% absolute, which is 31.5% relative to the nicotine present in the tobacco.
- the tobacco aroma oil obtained was free from resins and waxes and showed no precipitation and no clouding when 95% by weight ethanol was added.
Abstract
Die Erfindung betrifft ein Verfahren zur Gewinnung von Aromastoffen aus einem mit Lösungsmitteln erhältlichen Tabakextrakt (Primärextrakt), durch Vermischen dieses Tabakextraktes mit einem Adsorptionsmittel, Behandeln des erhaltenen Gemisches in einem Druckextraktionsbehälter mit CO2 unter Extraktionsbedingungen (Sekundärextraktion) und Gewinnung eines klaren Tabak-Aromaöls in einem nachgeschalteten Abscheidebehälter.The invention relates to a process for obtaining aroma substances from a tobacco extract (primary extract) obtainable with solvents, by mixing this tobacco extract with an adsorbent, treating the mixture obtained in a pressure extraction container with CO 2 under extraction conditions (secondary extraction) and obtaining a clear tobacco aroma oil a downstream separator tank.
Ferner ist Gegenstand der Erfindung ein neues Tabak- Aromaöl, frei von Harzen, Wachsen und Polyphenolen, mit einem erheblich reduzierten Nikotinanteil.The invention also relates to a new tobacco aromatic oil, free of resins, waxes and polyphenols, with a significantly reduced nicotine content.
Außerdem ist Gegenstand der Erfindung die Verwendung des erhältlichen Tabak-Aromaöls zum Aromatisieren von Tabak oder Tabakerzeugnissen. The invention also relates to the use of the available tobacco aromatic oil for flavoring tobacco or tobacco products.
Description
Die Erfindung betrifft als neues Produkt ein klares Tabak- Aromaöl, frei von Polyphenolen, Harzen und Wachsen,mit einem reduzierten (verminderten) Nikotingehalt von 5 bis 50% relativ (bezogen auf den Tabak, dem das Tabak-Aromaöl entstammt) und mit dem für den jeweils eingesetzten Ausgangstabak typischen Tabakgeruch. Darüberhinaus betrifft die Erfindung ein Verfahren zur Abtrennung von klarem Tabak- Aromaöl aus Tabakextrakt und dessen Verwendung gemäß den Patentansprüchen.The invention relates to a new product, a clear tobacco aroma oil, free of polyphenols, resins and waxes, with a reduced (reduced) nicotine content of 5 to 50% relative (based on the tobacco from which the tobacco aroma oil originates) and with which the typical tobacco smell used in each case. In addition, the invention relates to a method for separating clear tobacco aroma oil from tobacco extract and its use according to the claims.
Bei der Herstellung von Tabakwaren spielt die Aromatisierung des Tabaks eine besondere Rolle. Versuche, aus aromastarken Tabaken oder Tabakabfällen das für den jeweiligen Tabak typische Tabak-Aromaöl teilweise oder ganz zu gewinnen, um es anderen, aromaschwachen Tabaken gleicher Provenienz zuzusetzen, scheiterten bisher daran, daß es nicht gelang, ein absolutes (klares) Tabak-Aromaöl, frei von Harzen und Wachsen mit reduziertem Nikotingehalt, zu gewinnen.The flavoring of tobacco plays a special role in the manufacture of tobacco products. Attempts to partially or wholly obtain the tobacco aroma oil typical of the respective tobacco from aroma-strong tobacco or tobacco waste in order to add it to other, low-aroma tobacco of the same provenance have so far failed because an absolute (clear) tobacco aroma oil free of resins and waxes with reduced nicotine content.
Die DE-OS 21 28 779 beschreibt ein Verfahren zur Gewinnung von Aromastoffen und die. Umwandlung der Aroma-Precursoren aus Tabak, indem der Tabak mit einem oder mehreren Lösungsmitteln, die in der eluotropen Reihe zwischen Trichloräthylen und Äthylacetat liegen, extrahiert wird und aus dem gewonnenen Extrakt durch eine Wärmebehandlung zwischen 110 und 180° die Aroma-Precursoren aktiviert werden. Die nach diesem Verfahren gewonnenen Aroma-Produkte stellen eine wachsartige, harzige Masse dar, die alle Wachse und Harze sowie Polyphenole und nahezu das gesamte Nikotin des Ausgangsproduktes enthalten.DE-OS 21 28 779 describes a process for the production of flavorings and the. Conversion of aroma precursors from tobacco, by extracting the tobacco with one or more solvents which are in the eluotropic range between trichlorethylene and ethyl acetate and activating the aroma precursors from the extract obtained by heat treatment between 110 and 180 °. The aroma products obtained by this process represent a wax-like, resinous mass which contains all waxes and resins as well as polyphenols and almost all nicotine of the starting product.
Die DE-OS 21 42 205 beschreibt ein Verfahren zur selektiven, aromaerhaltenden Extraktion von Nikotin aus Tabak,-indem in der ersten Stufe dem trockenen Tabak durch Behandlung mit trockenen, überkritischen Gasen (z.B. CO2)das Aroma entzogen wird, das dann vorübergehend im Abscheidebehälter B verbleibt, bis dem Tabak im Behälter A durch eine zweite Verfahrensstufe mit Hilfe feuchter C02 das Nikotin entzogen wurde, das dann im Behälter D abgeschieden wird. In einer dritten Verfahrensstufe werden die im Behälter B befindlichen Aromastoffe mit z.B. überkritischer C02 gelöst, wieder in den Behälter A zurückgeführt und dort auf dem Tabak abgeschieden.DE-OS 21 42 205 describes a process for the selective, aroma-preserving extraction of nicotine from tobacco, - in the first stage of which the aroma is extracted from the dry tobacco by treatment with dry, supercritical gases (for example CO 2 ), which is then temporarily removed from the Separation container B remains until the tobacco in container A has been removed from the nicotine by a second process stage with the help of moist CO 2 , which is then separated out in container D. In a third process step, the flavoring substances in container B are dissolved with, for example, supercritical CO 2 , returned to container A and deposited there on the tobacco.
Dieses Verfahren ist bezüglich der Tabakaromagewinnung und Ausnutzung kostspielig und von geringer Effizienz, weil das in der ersten Stufe gewonnene Produkt kein von Harzen und Wachsen abtrennbares, klares flüssiges Tabakaromaöl darstellt, sondern eine Paste ist, die nahezu alle unerwünschten Wachse und Harze des Ausgangsproduktes sowie unerwünschte Polyphenole einschließt. Außerdem verhindern diese wachs- und harzartigen Stoffe die gleichmäßige Verteilung und Aromaübertragung bei der Rearomatisierung eines zu beaufschlagenden Tabaks. Die Polyphenole haben unter anderem den Nachteil, daß sie den Rauchgeschmack beeinträchtigen.This process is expensive in terms of tobacco aroma extraction and exploitation and is inefficient because the product obtained in the first stage is not a clear liquid tobacco aroma oil that can be separated from resins and waxes, but is a paste that contains almost all undesirable waxes and resins of the starting product and undesirable ones Includes polyphenols. In addition, these wax and resinous substances prevent the even distribution and aroma transfer when rearomatizing a tobacco to be loaded. One of the disadvantages of the polyphenols is that they impair the smoky taste.
Die DE-OS 28 44 781 beschreibt ein Verfahren zur extraktiven Behandlung von pflanzlichem und tierischem Material, u.a.DE-OS 28 44 781 describes a method for the extractive treatment of plant and animal material, i.a.
auch die Bearbeitung von Tabak unter Verwendung eines aus zwei Komponenten bestehenden Lösungsmittels, wie z.B. 93 Molprozent C02 + 7 Molprozent Ethanol oder 94 Molprozent C02 + 6 Molprozent Butan. Mit dem Zweiphasengemisch soll erreicht werden, daß z.B. die bei der organischen Lösungsmittelextraktion gebildeten Addukte und Veränderungen im bearbeiteten Material vermieden werden. Das Arbeiten mit CO2 allein unter überkritischen Druckbedingungen soll, um zu ausreichenden Extraktionsgraden zu kommen - Drucke von über 150 bar erfordern. Nach dem Verfahren der DE-OS 28 44 781 sollen diese Nachteile vermieden werden, wenn dem zur Extraktion eingesetzten CO2 gewisse Mengen z.B. alkoholische Lösungsmittel als Schleppmittel hinzugefügt werden.also the processing of tobacco using a solvent consisting of two components, such as 93 mol percent C0 2 + 7 mol percent ethanol or 94 mol percent C0 2 + 6 mol percent butane. The aim of the two-phase mixture is to avoid, for example, the adducts formed in the organic solvent extraction and changes in the processed material. Working with CO 2 alone under supercritical pressure conditions is said to require sufficient degrees of extraction - pressures of over 150 bar. According to the process of DE-OS 28 44 781, these disadvantages are to be avoided if certain amounts, for example alcoholic solvents, are added as entrainer to the CO 2 used for the extraction.
Nach diesem Verfahren wird - ebenso wie nach dem Verfahren der DE-OS 21 42 205 - als Zwischenprodukt nur eine pastenförmige, wenig Aromastoffe enthaltende Substanz mit allen Wachs-und Harzanteilen sowie unerwünschten Polyphenolen des zur Extraktion verwendeten Tabaks gewonnen.According to this process - just like the process of DE-OS 21 42 205 - only a paste-like substance containing little flavoring substances with all wax and resin contents as well as undesirable polyphenols of the tobacco used for the extraction is obtained as an intermediate product.
Gemäß keinem der bekannten Verfahren war die Erzielung eines Tabakextrakts bzw. Tabak-Aromas möglich, das den für den jeweils eingesetzten Ausgangstabak typischen Tabakgeruch besitzt.None of the known methods made it possible to obtain a tobacco extract or tobacco aroma which has the tobacco smell typical of the starting tobacco used in each case.
Aufgabe der vorliegenden Erfindung ist es, ein klares, absolutes Tabak-Aromaöl zu gewinnen, das qualitativ und quantitativ nahezu alle Aromastoffe des Ausgangsproduktes enthält, frei von Harzen, Wachsen und Polyphenolen ist und dessen Nikotingehalt - verglichen mit dem Ausgangsprodukt - stark reduziert ist.The object of the present invention is to obtain a clear, absolute tobacco aroma oil which contains almost all the aroma substances of the starting product qualitatively and quantitatively, is free from resins, waxes and polyphenols and whose nicotine content - compared to the starting product - is greatly reduced.
Diese Aufgabe wird durch das Verfahren gemäß den Patentansprüchen gelöst.This object is achieved by the method according to the patent claims.
Da nach den bekannten Verfahren der Extraktion des Tabaks mit organischen Lösungsmitteln oder der Extraktion des Tabaks mit überkritischen Gasen, wie z.B. CO2, stets nur ein pastenförmiges Aromaprodukt mit nahezu allen Harzen und Wachsen sowie Polyphenolen des Ausgangsmaterials gewonnen wurde, ist es überraschend, daß durch eine Primärextraktion mit organischen Lösungsmitteln oder Mischungen dieser Lösungsmittel untereinander oder mit Kohlendioxid und durch eine nachgeschaltete Sekundärextraktion mit C02 ein zweiphasiges Harz-/Aromaölgemisch gewonnen wird, das leicht in ein klares Tabak-Aromaöl und ein festes Harz/Wachsgemisch ohne Aromaträger aufgetrennt werden kann.Since, according to the known methods of extracting the tobacco with organic solvents or extracting the tobacco with supercritical gases, such as CO 2 , only a paste-like aroma product with almost all resins and waxes and polyphenols of the starting material was obtained, it is surprising that by a primary extraction with organic solvents or mixtures of these solvents with each other or with carbon dioxide and a secondary extraction with C0 2 a two-phase resin / aroma oil mixture is obtained, which can be easily separated into a clear tobacco aroma oil and a solid resin / wax mixture without aroma carrier.
Nachstehend wird die Erfindung im einzelnen erläutert.The invention is explained in detail below.
Tabak im Sinne der vorliegenden Erfindung sind fermentierte Tabak-Blätter, -Stengel, -Stiele oder -Staub sowie Tabakabfälle.For the purposes of the present invention, tobacco is fermented tobacco leaves, stems, stems or dust, and tobacco waste.
Tabak-Primärextrakt im Sinne der vorliegenden Erfindung ist ein mit üblichen organischen Lösungsmitteln, insbesondere Benzol, Toluol, Methanol, Ethanol, n-Propanol, Methyln-Propan äthylacetat, Diäthyläther, Aceton, n-Propan n-Hexan, Cyclohexan, Petroläther, Dichlormethan oder Trichlormethan, oder mit Mischungen dieser Lösungsmittel hergestellter Extrakt. Ein Primär-Extrakt im Sinne der vorliegenden Erfindung ist ferner auch ein C02-Extrakt, d.h. mit Hilfe von CO2 als Lösungsmittel hergestellter Extrakt.For the purposes of the present invention, tobacco primary extract is an ethyl acetate with customary organic solvents, in particular benzene, toluene, methanol, ethanol, n-propanol, methyln-propane, diethyl ether, acetone, n-propane, n-hexane, cyclohexane, petroleum ether, dichloromethane or Trichloromethane, or extract made with mixtures of these solvents. A primary extract according to the present invention further provides a C0 2 extract, that is, with the aid of CO 2 produced as a solvent extract.
Adsorptionsmittel im Sinne der vorliegenden Erfindung sind alle gebräuchlichen Adsorbentien, insbesondere Aktivkohle, Aluminiumoxid, Magnesiumoxid, Natrium-Aluminiumsilikat, Bleicherde, Bentonit, Kieselgel, Kieselgur, zeolithische Molekularsiebe etc.Adsorbents for the purposes of the present invention are all common adsorbents, in particular activated carbon, aluminum oxide, magnesium oxide, sodium aluminum silicate, bleaching earth, bentonite, silica gel, diatomaceous earth, zeolitic molecular sieves etc.
Tabak-Aromaöl im Sinne der vorliegenden Erfindung ist eine bei Normaltemperatur absolut klare, tabakaromatische, ölige Flüssigkeit - frei von Harzen und Wachsen, frei von Polyphenolen, mit einem reduzierten Nikotinanteil auf 5 bis 50% relativ (insbesondere 10 bis 40% relativ) bezogen auf den Tabak, dem der Tabakextrakt entstammt - die bei Zugabe von 95 Gew.-%-igem Ethanol keine Trübungen oder Ausfällungen zeigt.Tobacco aroma oil in the sense of the present invention is an absolutely clear, tobacco aromatic, oily liquid at normal temperature - free of resins and waxes, free of polyphenols, with a reduced nicotine content of 5 to 50% relative (in particular 10 to 40% relative) based on the tobacco from which the tobacco extract originates - which shows no clouding or precipitation when 95% by weight ethanol is added.
Die Herstellung des erfindungsgemäß eingesetzten Tabak-Primärextrakts besteht im einzelnen darin, den Tabak in einem der vorgenannten Lösungsmittel oder (im Falle organischer Lösungsmittel) in einem Lösungsmittelgemisch zu extrahieren.The preparation of the tobacco primary extract used according to the invention consists in particular in extracting the tobacco in one of the abovementioned solvents or (in the case of organic solvents) in a solvent mixture.
Bevorzugt wird dabei 1 Gewichtsteil vorzerkleinerter Tabak mit etwa 3 bis 30 Gewichtsteilen eines der genannten Lösungsmittel (vorzugsweise CO2, n-Hexan oder Dichlormethan) extrahiert. Je nach der Effizienz der vorhandenen Extraktionsvorrichtungen erfolgt die Primärextraktion während mindestens 10 Minuten und höchstens 10 Stunden, vorzugsweise während 1.bis 5 Stunden.1 part by weight of pre-shredded tobacco is preferably extracted with about 3 to 30 parts by weight of one of the solvents mentioned (preferably CO 2 , n-hexane or dichloromethane). Depending on the efficiency of the extraction devices available, the primary extraction takes place for at least 10 minutes and at most 10 hours, preferably for 1 to 5 hours.
Im Falle des Einsatzes organischer Lösungsmittel erfolgt die Primärextraktion unter normalen Druckbedingungen. Im Falle des Einsatzes von CO2 bei der Primärextraktion sind die Druck-und Temperaturbedingungen im Extraktionsbehälter und Abscheidebehälter, sowie Extraktionszeit und CO2-Stronimenge mit denjenigen identisch, die nachstehend im Zusammenhang mit der (einstufigen) Sekundärextraktion angegeben sind (vgl. Seite 10, Zeile 5 bis 19, Seite 11, Zeile 12 bis 32).If organic solvents are used, the primary extraction takes place under normal pressure conditions. If CO 2 is used in the primary extraction, the pressure and temperature conditions in the extraction container and separating container, as well as the extraction time and CO 2 flow rate are identical to those specified below in connection with the (single-stage) secondary extraction (see
Der bei der Behandlung mit diesen Lösungsmitteln ungelöste Rückstand wird abgetrennt und der Lösungsmittel enthaltende Extrakt durch Verdampfen eingeengt, bis ein sirupartiger lösungsmittelfreier Tabakextrakt gewonnen wird. Das Verdampfen erfolgt im Falle des Einsatzes organischer Lösungsmittel vorzugsweise bei Unterdruck, besonders bevorzugt bei etwa 15 Torr. Im Falle des Einsatzes von C02 erfolgt das Verdampfen im Abscheidebehälter, wie bereits vorstehend ausgeführt, unter den Druck-und Temperaturbedingungen, wie sie nachstehend für die (einstufige) Sekundärextraktion angegeben sind.The undissolved residue in the treatment with these solvents is separated off and the solvent-containing extract is evaporated down until a syrup-like, solvent-free tobacco extract is obtained. If organic solvents are used, the evaporation is preferably carried out under reduced pressure, particularly preferably at about 15 torr. If C0 2 is used, the evaporation takes place in the separating container, as already explained above, under the pressure and temperature conditions as specified below for the (single-stage) secondary extraction.
Ein in dieser Weise gewonnener Tabak-Primärextrakt enthält u.a.. Polyphenole, Harze/Wachse, Nikotin und liegt, wie der Erfinder festgestellt hat, in einer für die nachfolgende Sekundärextraktion (mit CO2) besonders geeigneten, leicht zugänglichen Form vor,A tobacco primary extract obtained in this way contains, among other things. Polyphenols, resins / waxes, nicotine and, as the inventor has determined, is in an easily accessible form which is particularly suitable for the subsequent secondary extraction (with CO 2 ),
Der erhaltene Tabak-Primärextrakt wird nun erfindungsgemäB . mit einem Adsorptionsmittel intensiv vermischt, bis eine gleichmäßige Verteilung zwischen Extrakt und Adsorptionsmittel vorliegt. Dabei sind besonders bevorzugte Adsorptionsmittel: Natrium-Aluminiumsilikat, Bentonit, Magnesiumoxid oder zeolithische Molekularsiebe. Das Mischungsverhältnis Extrakt:Adsorptionsmittel ist variabel und kann in Abhängigkeit von der Konsistenz des Extraktes, der Dichte und Teilchengröße des Adsorptionsmittels sowie der gewünschten Konsistenz des Mischproduktes eingestellt werden. Im allgemeinen ist ein Mischungsverhältnis Extrakt:Adsorptionsmittel zwischen 1:0,1 bis 1:10 ausreichend; bevorzugt wird ein pulverförmiges Extraktgemisch mit einem Mischungsverhältnis Extrakt:Adsorptionsmittel von 1:0,3 bis 1:6.The tobacco primary extract obtained is now according to the invention. mixed intensively with an adsorbent until there is an even distribution between extract and adsorbent. Particularly preferred adsorbents are: sodium aluminum silicate, bentonite, magnesium oxide or zeolitic molecular sieves. The mixing ratio of extract: adsorbent is variable and can be adjusted depending on the consistency of the extract, the density and particle size of the adsorbent and the desired consistency of the mixed product. In general, a mixture ratio of extract: adsorbent between 1: 0.1 to 1:10 is sufficient; preference is given to a powdery extract mixture with an extract: adsorbent mixing ratio of 1: 0.3 to 1: 6.
Das ExtraktjAdsorptionsmittel-Gemisch soll das Verhältnis 1:0,1 nicht unterschreiten, weil das erfindungsgemäß eingesetzte Adsorptionsmittel das Lösen der Aromastoffe bei der folgenden Sekundärextraktion mit CO2 (im Extraktionsbehälter) und die Abscheidung im Abscheidebehälter als leicht von Harzen und Wachsen abtrennbares, klares absolutes Tabak-Aromaöl maßgeblich beeinflußt.The extract / adsorbent mixture should not fall below the ratio 1: 0.1, because the adsorbent used according to the invention, the dissolving of the flavoring substances in the subsequent secondary extraction with CO 2 (in the extraction container) and the separation in the separating container as clear absolute, easily separable from resins and waxes Tobacco aroma oil significantly influenced.
Ein Mischungsverhältnis von mehr als 1:10 gibt ebenfalls noch eine gute Ablösung und Abscheidung des Tabak-Aromaöls, wobei allerdings ein größeres Druckbehältervolumen in Kauf zu nehmen ist.A mixture ratio of more than 1:10 also gives a good detachment and separation of the tobacco aroma oil, although a larger pressure vessel volume has to be accepted.
Das Gemisch aus Primärextrakt und Adsorptionsmittel wird erfindungsgemäß in ' einem ersten Druckbehälter (Extraktionsbehälter) , vorzugsweise Hochdruckbehälter, mit CO2 unter bestimmten Druck- und Temperaturbedingungen solange behandelt, bis alle Aromastoffe in dem dem Extraktionsgefäß nachgeschalteten zweiten Druckbehälter (Abscheidebehälter) als leicht von Harzen und Wachsen auftrennbare, ölige Flüssigkeit vorliegen.According to the invention, the mixture of primary extract and adsorbent is' in a first pressure vessel (extraction vessel), preferably high pressure vessel, with CO 2 under certain pressure and Treated temperature conditions until all the aromas are present in the second pressure vessel (separator vessel) downstream of the extraction vessel as an oily liquid that can easily be separated from resins and waxes.
Diese Sekundärextraktion mit C02 nach dem Verfahren der Erfindung wird erreicht, indem man die zur Extraktion des Extrakt/ Adsorptionsmittel-Gemisches verwendete C02 in Bezug auf Druck und Temperatur überkritisch (> 73 bar und > 31,3°C) oder in bezug auf Druck und Temperatur unterkritisch (< 73 bar und < 31,3°C) oder in bezug auf Druck überkritisch ( > 73 bar) und in bezug auf Temperatur unterkritisch (< 31,3°C) hält.This secondary extraction with C0 2 by the method of the invention is achieved by supercritically using the C0 2 used for extracting the extract / adsorbent mixture with respect to pressure and temperature (> 73 bar and> 31.3 ° C) or with respect to Keeps pressure and temperature subcritical (<73 bar and <31.3 ° C) or supercritical with regard to pressure (> 73 bar) and subcritical with regard to temperature (<31.3 ° C).
Bei überkritischer Arbeitsweise hinsichtlich Druck und Temperatur werden vorzugsweise Drucke von 85 bis 250 bar und Temperaturen von +35°C bis +90°C gewählt. Beim Arbeiten im unterkritischen Druck- und unterkritischen Temperaturbereiche sind Drucke von 25 bis 70 bar und Temperaturen von +5°C bis +25°C bevorzugt. Beim Arbeiten im überkritischen Druck- und unterkritischen Temperaturbereich sind Drucke von 85 bis 200 bar und Temperaturen von +10°C bis +30°C bevorzugt.When working with supercritical pressure and temperature, pressures from 85 to 250 bar and temperatures from + 35 ° C to + 90 ° C are preferred. When working in the subcritical pressure and subcritical temperature ranges, pressures from 25 to 70 bar and temperatures from + 5 ° C to + 25 ° C are preferred. When working in the supercritical pressure and subcritical temperature range, pressures from 85 to 200 bar and temperatures from + 10 ° C to + 30 ° C are preferred.
Falls ein besonders niedriger Nikotinanteil im Endprodukt (Sekundärextrakt) erwünscht ist (z.B. von 5 bis 10% relativ, bezogen auf den Tabak, der zur Primärextraktion verwendet wurde), kann zwischen der anspruchsgemäßen Primärextraktion und der anspruchsgemäßen Sekundärextraktion ein zusätzlicher CO2-Extraktionsschritt bei niedrigen Temperaturen zwischengeschaltet werden. Zu diesem Zweck wird der bei der Primärextraktion erhaltene und mit dem Adsorptionsmittel vermischte Extrakt vorab bei C02-Extraktionstemperaturen von -25°C bis +5°C und C02-Extraktionsdrucken von etwa 20 bis 25 bar behandelt; bei diesem zwischengeschalteten C02-Extraktionsschritt erfolgt die Entspannung im Abscheidebehälter bei unterkritischen Druck- und Temperaturbedingungen, wobei eine Abscheidung (des Nikotins) im Abscheidebehälter bei Temperaturen von etwa +15°C bis +30°C und bei Drucken von etwa 2 bis 15 bar bevorzugt ist. Dabei genügt eine Extraktionszeit von 0,5 bis 2 Stunden, bevorzugt etwa . 1 Stunde sowie eine CO2-Strommenge von 5 bis 50 kg/Stunde, bevorzugt 10 bis 30 kg/Stunde. Überraschenderweise werden bei diesem zwischengeschalteten C02-Extraktionsschritt fast ausschließlich Nikotin und andere Nebenalkaloide (nicht aber andere an sich C02-lösliche Bestandteile, wie z.B. Aromastoffe, Harze, Wachse, Polyphenole etc.) aus dem Primärextrakt/Adsorptionsmittel-Gemisch herausgelöst und im Abscheidebehälter ausgeschieden. Das erhaltene Nikotin wird dem Abscheidebehälter entnommen, bevor die anschließende Sekundärextraktion (Aromaextraktion) mit CO2 beginnt.If a particularly low nicotine content in the end product (secondary extract) is desired (e.g. from 5 to 10% relative, based on the tobacco that was used for the primary extraction), an additional CO 2 extraction step can be carried out at a lower level between the claimed primary extraction and the claimed secondary extraction Temperatures are interposed. For this purpose, the extract obtained in the primary extraction and mixed with the adsorbent is treated beforehand at CO 2 extraction temperatures from -25 ° C. to + 5 ° C. and CO 2 extraction pressures from approximately 20 to 25 bar; in this intermediate C0 2 extraction step, the pressure in the separating tank is released under subcritical pressure and temperature conditions, with a separation (of nicotine) in the separating tank at temperatures of about + 15 ° C to + 30 ° C and at pressures of about 2 to 15 bar is preferred. It is enough an extraction time of 0.5 to 2 hours, preferably about. 1 hour and a CO 2 flow rate of 5 to 50 kg / hour, preferably 10 to 30 kg / hour. Surprisingly, in this intermediate C0 2 extraction step, nicotine and other secondary alkaloids (but not other per se C0 2 -soluble constituents, such as flavorings, resins, waxes, polyphenols etc.) are almost exclusively dissolved out of the primary extract / adsorbent mixture and in the separation container eliminated. The nicotine obtained is removed from the separation container before the subsequent secondary extraction (aroma extraction) with CO 2 begins.
Bei dem erfindungsgemäßen Verfahren gemäß dem Patentanspruch, insbesondere bei der Sekundärextraktion, sind die Abscheidungs- bedingungen im Entspannungsbehälter (Abscheidebehälter) für die Qualität und Quantität des erfindungsgemäß gewonnenen Produkts maßgeblich. Die Entspannungsdrucke und Entspannungstemperaturen liegen zweckmäßigerweise im unterkritischen Bereich der C02 (unterkritischer Druck/unterkritische Temperatur). Dabei sind Drucke von 45 bis 65 bar und Temperaturen von 15 bis 30°C bevorzugt; besonders bevorzugt sind Drucke von etwa 50 bis 55 bar und Temperaturen von 20 bis 25°C. Die Abscheidung im Entspannungsbehälter wird vorzugsweise bei gleichzeitiger Druck- und Temperaturabsenkung gegenüber den im Extraktionsbehälter herrschenden Druck- und Temperaturbedingungen vorgenommen.;In the method according to the invention, in particular in secondary extraction, the separation conditions in the expansion tank (separation tank) are decisive for the quality and quantity of the product obtained according to the invention. The relaxation pressures and relaxation temperatures are expediently in the subcritical range of C0 2 (subcritical pressure / subcritical temperature). Pressures of 45 to 65 bar and temperatures of 15 to 30 ° C are preferred; pressures of about 50 to 55 bar and temperatures of 20 to 25 ° C. are particularly preferred. The separation in the expansion tank is preferably carried out with simultaneous pressure and temperature lowering than the pressure and temperature conditions prevailing in the extraction tank .;
Auch die Menge der den Extraktionsbehälter durchströmenden CO2 und die Dauer der Durchströmung sind für die erfindungsgemäße Verfahrensweise maßgeblich. Zweckmäßig sind Behandlungszeiten von insgesamt 0,5 bis 8 Stunden, bevorzugt 1 bis 5 Stunden, besonders bevorzugt 2 bis 4 Stunden; zweckmäßig ist eine CO2-Strommenge von insgesamt 0,3 bis 35 kg/Stunde, bevorzugt 3 bis 30 kg/Stunde, besonders bevorzugt 5 bis 15 kg/Stunde, bezogen auf 1 kg unbehandelten Tabak. Wie bereits oben ausgeführt wurde (vgl. Seite 8, Zeile 20 bis 25), gelten die vorstehend für dieThe amount of CO 2 flowing through the extraction container and the duration of the flow are also decisive for the procedure according to the invention. Treatment times totaling 0.5 to 8 hours, preferably 1 to 5 hours, particularly preferably 2 to 4 hours are expedient; A total amount of CO 2 is expedient from 0.3 to 35 kg / hour, preferably 3 to 30 kg / hour, particularly preferably 5 to 15 kg / hour, based on 1 kg of untreated tobacco. As already explained above (see page 8, lines 20 to 25), the above apply to the
(einstufige) Sekundärextraktion angegebenen Bedingungen der C02-Extraktion, wie Druck- und Temperatur im Extraktionsbehälter, Druck und Temperatur im Abscheidebehälter, Extraktionszeit und C02-Strommenge auch für die Primärextraktion, wenn bei ihr als Lösungsmittel CO2 eingesetzt wird. Eine nochmalige Aufzählung dieser Parameter, speziell für den Fall der Primärextraktion, erübrigt sich daher.(Single-stage) secondary extraction specified conditions of the C0 2 extraction, such as pressure and temperature in the extraction container, pressure and temperature in the separating container, extraction time and C0 2 flow rate also for the primary extraction if CO 2 is used as the solvent. It is therefore not necessary to list these parameters again, especially in the case of primary extraction.
Bei dem erfindungsgemäßen Verfahren erhält man nach Beendigung der Sekundärextraktion bei der Entnahme aus dem Entspannungsbehälter ein Feststoff/Ölgemisch, das bereits in 2 Phasen vorliegt. Durch einfache Filtration kann dieses Gemisch in ein klares, absolutes Tabak-Aromaöl frei von Polyphenolen mit stark reduziertem Nikotinanteil und ein festes Harz/Wachsgemisch mit relativ hohem Nikotinanteil getrennt werden.In the process according to the invention, after the secondary extraction has ended, a solid / oil mixture which is already present in two phases is obtained upon removal from the expansion tank. By simple filtration, this mixture can be separated into a clear, absolute tobacco aroma oil free of polyphenols with a greatly reduced nicotine content and a solid resin / wax mixture with a relatively high nicotine content.
Ein besonderes Charakteristikum des erfindungsgemäß gewonnenen Tabak-Aromaöls besteht außerdem darin, daß es den für den jeweils eingesetzten Ausgangstabak typischen Tabakgeruch aufweist. Es unterscheidet sich mit dieser Eigenschaft eindeutig von allen bisher bekannt gewordenen Tabakextrakten, denn mit keinem der herkömmlichen Tabakextrakte war es möglich, den typischen Geruch des jeweiligen Ausgangstabaks herzustellen. Aufgrund dieses charakteristischen Merkmals des erfindungsgemäß gewonnenen Tabakextrakts ist davon auszugehen, daß er in seiner stofflichen Zusammensetzung gegenüber dem Stand der Technik völlig neuartig ist.A special characteristic of the tobacco aromatic oil obtained according to the invention is also that it has the tobacco smell typical of the starting tobacco used in each case. This characteristic clearly distinguishes it from all tobacco extracts known to date, because none of the conventional tobacco extracts made it possible to produce the typical smell of the respective starting tobacco. Based on this characteristic feature of the tobacco extract obtained according to the invention, it can be assumed that its material composition is completely new compared to the prior art.
Mit der vorliegenden Erfindung wird erstmals, ausgehend von einem Produkt (Tabakprimärextrakt), das nebeneinander Aromastoffe, Polyphenole, Nikotin, Harze, Wachse und andere Stoffe enthält, eine Abtrennung und Gewinnung des Tabakaromas als klares und absolutes öl erzielt, und dies. mit einfach durchzuführenden Maßnahmen und besonders effizientem Resultat. Weder für dieses Verfahren als solches noch für das erhaltene Produkt ließ sich dem Stand der Technik ein Hinweis entnehmen.With the present invention, for the first time, starting from a product (tobacco primary extract) which contains flavors, polyphenols, nicotine, resins, waxes and other substances, the tobacco flavor is separated and obtained as a clear and absolute oil, and this. with measures that are easy to carry out and a particularly efficient result. No indication of the prior art could be found either for this process as such or for the product obtained.
Bemerkenswert und überraschend an dem erfindungsgemäß gewonnenen Produkt ist, daß nach beendeter Sekundärextraktion aus dem Entspannungsbehälter eine leicht abtrennbare, klare Schicht von Tabak-Aromaöl mit stark reduziertem Nikotinanteil, frei von Polyphenolen, Harzen und Wachsen und eine harzigwachsartige Schicht entnommen werden kann, die einen wesentlichen Anteil des Nikotins des Primärextrakts einschließt.It is remarkable and surprising about the product obtained according to the invention that after the secondary extraction has ended, an easily separable, clear layer of tobacco aromatic oil with a greatly reduced nicotine content, free of polyphenols, resins and waxes and a resinous wax-like layer can be removed, which is an essential one Proportion of nicotine in the primary extract.
Es war überraschend, daß die Tabakinhaltsstoffe, die nach der erfindungsgemäßen Verfahrensweise durch Primärextraktion gewonnen werden, sich in der Mischung mit einem pulverförmigen Adsorptionsmittel und anschließender'Sekundärextraktion (mit C02) hinsichtlich ihrer Viskosität, ihrer Löslichkeits- und Abscheideverhältnisse ganz anders verhalten als die gleichen Inhaltsstoffe, die nur der Primärextraktion (auch der C02-Primärextraktion), z.B. aus Tabakblättern, unterworfen werden.It was surprising that the tobacco constituents, which are obtained by primary extraction according to the procedure according to the invention, behave in a mixture with a powdery adsorbent and subsequent secondary extraction (with C0 2 ) with respect to their viscosity, their solubility and separation ratios very different from the same Ingredients that are only subjected to primary extraction (including CO 2 primary extraction), e.g. from tobacco leaves.
Auch im Falle der erfindungsgemäß gegebenenfalls zwischengeschalteten besonders effizienten Nikotin-Extraktion (gegebenenfalls zwischengeschalteter CO2-Extraktionsschritt) wird dies sehr deutlich: Nach der geltenden Lehre werden Nikotin und Polyphenole nur in Anwesenheit von Feuchtigkeit, z.B. aus Tabakblättern, mit Hilfe von C02 extrahiert. Bei der erfindungsgemäßen Verfahrensweise wird jedoch .in keiner Verfahrensstufe Feuchtigkeit zugesetzt oder benutzt, und trotzdem wird aus dem erfindungsgemäß hergestellten Primärextrakt fast das gesamte Nikotin gelöst und im Abscheidebehälter niedergeschlagen. Diese neue Erkenntnis resultiert auch in der erfindungsgemäßen Verfahrensvariante, (sofern gewünscht) nahezu reines Nikotin selektiv aus dem Primärextrakt/Adsorptionsmittel-Gemisch durch (trockene) C02-Extraktion bei Temperaturen von -25°C bis +5°C zu extrahieren.This is also very clear in the case of the particularly efficient nicotine extraction which may be interposed according to the invention (if appropriate an interposed CO 2 extraction step): according to the current teaching, nicotine and polyphenols are only extracted in the presence of moisture, for example from tobacco leaves, using C0 2 . In the procedure according to the invention, however, moisture is not added or used in any process step, and nevertheless almost all of the nicotine is dissolved from the primary extract prepared according to the invention and deposited in the separating container. This new finding also results in the process variant according to the invention of selectively extracting (if desired) almost pure nicotine from the primary extract / adsorbent mixture by (dry) CO 2 extraction at temperatures from -25 ° C. to + 5 ° C.
Eine weitere Überraschung beruht auf der Ergiebigkeit und der Reinheit des Geruchs des erfindungsgemäß hergestellten Produkts sowie auf dessen den Rauchgeschmack verbessernden Effekt.Another surprise is based on the productivity and the purity of the smell of the product produced according to the invention and on its smoke-improving effect.
Über das Aromaöl speziell des Tabaks ist bisher wenig bekannt geworden. In herkömmlicher Weise gewonnene Aromaöle wurden lediglich durch Wasserdampfdestillation im Labormaßstab hergestellt. Die erhaltenen öle waren von zahlreichen Fremdgerüchen, wie z.B. Kamille, Kümmel, Pfefferminz, Baldrian und Amylalkohol begleitet, die wahrscheinlich durch Artefakt-Bildungen hervorgerufen werden. Die Ausbeute derartiger Tabaköle betrug etwa 0,1 bis 0,2%.Little is known about the aromatic oil, especially tobacco. Aroma oils obtained in a conventional manner were only produced by steam distillation on a laboratory scale. The oils obtained were of numerous foreign smells, e.g. Accompanied by chamomile, caraway, peppermint, valerian and amyl alcohol, which are probably caused by artifacts. The yield of such tobacco oils was about 0.1 to 0.2%.
Wie bereits-oben ausgeführt, steht in klarem Unterschied hierzu das erfindungsgemäß gewonnene Tabak-Aromaöl, das den typischen und reinen Geruch des jeweils eingesetzten Ausgangstabaks aufweist. So riecht z.B. das aus Havanna-Tabak gewonnene Aromaöl nach Havannatabak, aus Kentucky-Tabak gewonnenes Aromaöl nach Kentucky-Tabak. In ähnlicher Weise zeigen aus Virginia-, Orient- oder Burley-Tabak gewonnene Aromaöle den ganz typischen und reinen Geruch der jeweiligen.Tabaksorte. Aufgrund dieses besonderen, vom Stand der Technik eindeutig unterschiedlichen Charakteristikums ist festzuhalten, daß das erfindungsgemäß gewonnene Tabak-Aromaöl in seiner stofflichen Zusammensetzung gegenüber den Produkten des Stands der Technik ganz neuartig ist.As already explained above, the tobacco aroma oil obtained according to the invention, which has the typical and pure smell of the starting tobacco used in each case, stands in clear distinction from this. This is how it smells, for example the Havana tobacco flavored oil obtained from Havana tobacco, the Kentucky tobacco flavored oil obtained from Kentucky tobacco. In a similar way, aromatic oils obtained from Virginia, Orient or Burley tobacco show the very typical and pure smell of the respective tobacco variety. Because of this particular characteristic, which is clearly different from the prior art, it should be noted that the tobacco aromatic oil obtained according to the invention is completely new in its material composition compared to the products of the prior art.
Das auf die erfindungsgemäße Weise gewonnene Tabak-Aromaöl ist frei von Fremdgerüchen, frei von Polyphenolen, Harzen und Wachsen, hat einen reduzierten Nikotinanteil, der nur 5 bis 50% relativ der verwendeten Tabakblätter beträgt, und wird in Ausbeuten von 0,8 bis 2,5% (absolutes öl) erhalten.The tobacco aromatic oil obtained in the manner according to the invention is free from foreign odors, free from polyphenols, resins and waxes, has a reduced nicotine content which is only 5 to 50% relative to the tobacco leaves used, and is obtained in yields of 0.8 to 2%. Get 5% (absolute oil).
Hinsichtlich der Ergiebigkeit bei der Aromatisierung von Tabakizeigen bereits 50 ppm des erfindungsgemäß gewonnenen Produkts z.B. aus Havanna-Tabak die gleiche Ergiebigkeit und Intensität im Aroma wie etwa 250 ppm eines nach bekannten Methoden der Wasserdampfdestillation gewonnenen Aroma-Produktes aus Havanna-Tabak.With regard to the yield in the aromatization of tobacco i , 50 ppm of the product obtained according to the invention, for example from Havana tobacco, already shows the same yield and intensity in the aroma as about 250 ppm of an aroma product from Havana tobacco obtained by known methods of steam distillation.
Gegenstand der Erfindung ist ferner die Verwendung des erfindungsgemäß gewonnenen Tabak-Aromaöls zum Aromatisieren vonThe invention further relates to the use of the tobacco aromatic oil obtained according to the invention for flavoring
Tabak, oder Tabakerzeugnissen wobei diese Aromatisierung sowohl durch Beaufschlagen unmittelbar von Tabak erfolgen kann, als auch durch Aromatisieren von porösem Trägermaterial oder von Tabak-Klebematerial.Tobacco, or tobacco products, this flavoring being able to be carried out either directly by tobacco or by aromatizing porous carrier material or tobacco adhesive material.
Im Fall des unmittelbaren Beaufschlagens von Tabak eignet sich das erfindungsgemäße Tabak-Aromaöl nicht nur zum Aromatisieren aromaschwacher Tabake oder rekonstituierten Tabaks mittels Soßen ("Casing") sondern es ist auch besonders als "Top Flavor" geeignet.In the case of direct exposure to tobacco, the tobacco aromatic oil according to the invention is not only suitable for flavoring weak-flavored tobacco or reconstituted tobacco by means of sauces ("casing"), but is also particularly suitable as a "top flavor".
Eine weitere Art des Aromatisierens besteht darin, daß das Tabak-Aromaöl auf poröse Trägermaterialien, die in Berührung mit Tabak oder Tabakerzeugnissen stehen, aufgetragen wird. Solche poröse Trägermaterialien können z.B. in Form von Papier- oder Tonstücken, Attrappen, innerem Verpackungsmaterial (beispielsweise bei Schachteln, Beuteln etc.) vorliegen.Another type of flavoring is that the tobacco aromatic oil is applied to porous carrier materials that are in contact with tobacco or tobacco products. Such porous support materials can e.g. in the form of pieces of paper or clay, dummies, inner packaging material (e.g. for boxes, bags, etc.).
Als weitere Ausführungsform des Aromatisierens unter Einsatz des erfindungsgemäßen Tabak-Aromaöls ist auch die Zugabe zu Klebematerial für Tabakerzeugnisse zu nennen. Beispiele dafür sind Klebemittel, wie sie üblicherweise für Tabakerzeugnisse verwendet werden, z.B. Klebstoffe für Zigarrendeckblätter, Zigarettenpapier, etc.A further embodiment of flavoring using the tobacco aromatic oil according to the invention is also the addition to adhesive material for tobacco products. Examples of these are adhesives as are commonly used for tobacco products, e.g. Adhesives for cigar covers, cigarette paper, etc.
Mittels des erfindungsgemäß gewonnenen Tabak-Aromaöls lassen sich etwaige, bei der Produktion auftretende Schwankungen (Qualitätsunterschiede oder sonstige Unterschiede im Rauchgeschmack) des Tabaks entscheidend beeinflussen.The tobacco aroma oil obtained according to the invention can be used to decisively influence any fluctuations that occur during production (quality differences or other differences in the smoky taste) of the tobacco.
Die zum Aromatisieren von Tabak oder Tabakerzeugnissen eingesetzte Menge an Tabak-Aromaöl kann je nach Beschaffenheit des Tabaks und der angestrebten Aromatisierung schwanken. Im Falle von aus z.B. Havanna-Tabak erfindungsgemäß gewonnenem Aromaöl verwendet man zum Beaufschlagen bevorzugt 25 bis 100, besonders bevorzugt 40 bis 60 mg Tabak-Aromaöl pro kg Tabak, d.h. 25 bis 100 ppm, bevorzugt 40 bis 60 ppm.The amount of tobacco aromatic oil used to flavor tobacco or tobacco products can vary depending on the nature of the tobacco and the desired flavoring. In the case of aroma oil obtained according to the invention from, for example, Havana tobacco, 25 to 100, particularly preferably 40 to 60 mg of tobacco aroma oil per are preferably used for loading kg of tobacco, ie 25 to 100 ppm, preferably 40 to 60 ppm.
Die mit dem erfindungsgemäßen Produkt. erzielbare hohe Ergiebigkeit und Intensität wird besonders dadurch gefördert, daß ein harz-, polyphenol- und wachsfreies Tabak-Aromaöl vorliegt. Auch diese besondere Beschaffenheit des Tabak-Aromaöls stellt ein gegenüber dem Stand der Technik besonders charakteristisches und neuartiges Merkmal dar.The with the product according to the invention. Achievable high productivity and intensity is particularly promoted by the fact that a tobacco aroma oil free of resin, polyphenol and wax is present. This particular quality of the tobacco aroma oil also represents a particularly characteristic and novel feature compared to the prior art.
Im folgenden wird eine zur Durchführung der erfindungsgemäßen Sekundärextraktion besonders geeignete Vorrichtung beschrieben (vgl. beigefügte Zeichnung): Flüssiges C02 wird aus dem Tank 1 im unterkritischen Druck-und Temperaturzustand entnommen. Durch den Wärmeaustauscher 2 wird das CO2 auf die gewünschte unterkritische oder überkritische Temperatur eingestellt und mit Hilfe der Hochdruckpumpe 3 der gewünschte überkritische oder unterkritische Druck erzielt. Durch das Durchflußmeßgerät 16 gelangt das C02 in den Extraktionsbehälter 4, wo die Extraktion des Gemisches aus Primärextrakt und Adsorptionsmittel stattfindet. Die Befüllung und Entleerung des Extraktionsbehälters 4 mit Produkt erfolgt diskontinuierlich durch öffnen und Verschlie- . ßen der Kopföffnung nach jeder Extraktion. Der im Extraktionsbehälter herrschende Druck wird mit dem Druckaufnehmer 14 bestimmt. Das flüssige oder fluide CO2, das die gelösten Tabakinhaltsstoffe enthält, wird über das Drosselventil 6 zum Druckregelventil 8 (='Entspannungsventil) geführt und durch den Wärmeaustauscher 9 in den Entspannungsbehälter 10 eingebracht. Die Trennung der in dem C02 gelösten Tabakinhaltsstoffe wird durch das Druckregelventil 8 eingeleitet und durch Senken der Temperatur im Wärmeaustauscher 9 unterstützt. Im Entspannungsbehälter 10 trennen sich die extrahierten Tabakbestandteile in ein klares Tabak-Aromaöl und ein wachsartiges, harziges Nikotinprodukt, die entweder kontinuierlich durch das Ventil 17 oder nach beendeter Extraktion durch öffnen des Behälters 10 entnommen werden. Am Ende jeder Extraktion wird durch Öffnen des Ventils 5 auch die Extraktionsseite der Vorrichtung vom Druck entlastet. Das während der Extraktion aus dem Entspannungsbehälter 10 austretende C02 wird über die Leitung 11 rezirkuliert. Die Steuerung der Vorrichtung kann von Hand oder mittels des elektrischen Steuergerätes 12 erfolgen , dem als Eingänge die mit einem Temperaturfühler 13 im Extraktionsbehälter 4 gemessenen Temperatur, die mit Druckaufnehmer 14 und 15 gemessenen Drucke, die aus den Druckbehältern 4 und 10 austretenden CO2-Ströme sowie die mit dem Durchflußmesser 7 gemessene Durchflußmenge dienen. In Abhängigkeit von diesen Meßwerten wird das Druckregelventil 8 und auch die Kühlleistung im Wärmeaustauscher 9 eingestellt.A device which is particularly suitable for carrying out the secondary extraction according to the invention is described below (see attached drawing): Liquid CO 2 is removed from the
Falls bei der anspruchsgemäßen Primärextraktion C02 als Lösungsmittel eingesetzt wird, kann die geschilderte, in der Zeichnung erläuterte Vorrichtung auch dabei Anwendung finden.If C0 2 is used as solvent in the primary extraction according to the claims, the device described and explained in the drawing can also be used here.
Die folgenden Beispiele erläutern die Erfindung, ohne ihre Anwendung zu beschränken.The following examples illustrate the invention without restricting its application.
Die Bestimmung des Nikotins erfolgte spektralphotometrisch gemäß der aus "Handbuch der Lebensmittelchemie" Bd. VI, (1970), Seiten 321 bis 325, bekannten Methode von H. Kuhn.The nicotine was determined spectrophotometrically in accordance with the method of H. Kuhn known from "Handbuch der Lebensmittelchemie" Vol. VI, (1970), pages 321 to 325.
1000 g Havanna-Tabak (Wassergehalt 6,5%, Nikotingehalt 1,27%) werden in einer Messermühle zerkleinert und in 10 Liter Dichlormethan erschöpfend extrahiert - und das Lösungsmittel bei einem Unterdruck von 15 Torr abgedampft.1000 g Havana tobacco (water content 6.5%, nicotine content 1.27%) are crushed in a knife mill and exhaustively extracted in 10 liters of dichloromethane - and the solvent is evaporated off at a vacuum of 15 torr.
Es wurden 75 g lösungsmittelfreier, dunkler, sirupartiger Dichlormethanextrakt (Primärextrakt) erhalten, der mit 90 g Na-Aluminiumsilikat (Na-Al-Zeolith) in einem Knetapparat intensiv vermischt wurde (Mischungsverhältnis 1: 1, 2) .75 g of solvent-free, dark, syrup-like dichloromethane extract (primary extract) were obtained, which were mixed with 90 g of Na aluminum silicate (Na-Al zeolite) in a kneader was mixed thoroughly (mixing ratio 1: 1, 2).
Das Gemisch wurde 120 Minuten lang in einem geschlossenen Hochdruckextraktionsbehälter bei einem Druck von 230 bar und einer Temperatur von 65°C mit CO2 behandelt. Der Druck auf der Entspannungsseite betrug 50 bar, die Temperatur 24°C.The mixture was treated for 120 minutes in a closed ochdruckextraktionsbehälter H at a pressure of 230 and a temperature of 65 ° C with CO 2. The pressure on the relaxation side was 50 bar and the temperature was 24 ° C.
Die Durchflußmenge an CO2 beträgt 6 kg/Stunde.The flow rate of CO 2 is 6 kg / hour.
Nach Beendigung des Versuches wurden dem Entspannungsbehälter 40,1 g eines Zweiphasengemisches entnommen, das durch einfache Filtration in 22,5 g klares, öliges Tabak-Aromaöl und 17,6 g eines Harz-/Wachsniederschlages aufgetrennt wurde.After the end of the experiment, 40.1 g of a two-phase mixture were removed from the flash tank, which was separated by simple filtration into 22.5 g of clear, oily tobacco aroma oil and 17.6 g of a resin / wax precipitate.
Die Ausbeute an klarem, absolutem Tabak-Aromaöl betrug 2,25% des verwendeten Tabaks. Der Nikotingehalt war 19,92%, das sind 35% relativ von dem im Tabak vorhanden gewesenen Nikotin.The yield of clear, absolute tobacco aroma oil was 2.25% of the tobacco used. The nicotine content was 19.92%, which is 35% relative to the nicotine present in the tobacco.
Die Ausbeute des Harz-/Wachsniederschlages war 1,76%, der Nikotingehalt 43% absolut, das sind 60% relativ des im Tabak vorhanden gewesenen Nikotins.The yield of the resin / wax deposit was 1.76%, the nicotine content 43% absolute, which is 60% relative to the nicotine present in the tobacco.
Das gewonnene Tabak-Aromaöl war frei von Harzen und Wachsen und zeigte bei der Zugabe von 95 Gew.-%-igem Ethanol keinen Niederschlag und keine Trübung.The tobacco aroma oil obtained was free from resins and waxes and showed no precipitation and no clouding when 95% by weight ethanol was added.
1000 g Kentucky-Tabak (Wassergehalt 8,0%, Nikotingehalt 1,7%) werden in einer Schneidemühle zerkleinert und in einer CO2-Hochdruck-Extraktionsanlage (gemäß Zeichnung) mit C02 als Lösungsmittel extrahiert:1000 g of Kentucky tobacco (water content 8.0%, nicotine content 1.7%) are crushed in a cutting mill and extracted in a CO 2 high-pressure extraction system (according to the drawing) with C0 2 as solvent:
Druck im Extraktionsbehälter: 250 bar Temperatur im Extraktionsbehälter: 40°C Druck im Entspannungsbehälter: 55 bar Temperatur im Entspannungsbehälter: 22°CPressure in the extraction container: 250 bar Temperature in the extraction container: 40 ° C Pressure in the expansion tank: 55 bar Temperature in the expansion tank: 22 ° C
Dauer der Behandlung: 3 Stunden. Durchflußmenge CO2: 8 kg/Stunde.Treatment duration: 3 hours. Flow rate CO 2 : 8 kg / hour.
Nach beendeter Extraktion werden 70 g einer braunen, festen Paste (Primärextrakt) dem Entspannungsbehälter entnommen und intensiv mit 140 g Bentonit vermischt.After the extraction is complete, 70 g of a brown, solid paste (primary extract) are removed from the flash tank and mixed intensively with 140 g of bentonite.
Analog den in Beispiel 1 genannten Bedingungen wird dieses Gemisch einer Sekundärextraktion mit CO2 unterworfen.Analogously to the conditions mentioned in Example 1, this mixture is subjected to a secondary extraction with CO 2 .
Nach beendeter Sekundärextraktion wurden dem Entspannungs-, behälter 38 g eines Zweiphasengemisches-entnommen, das durch Druckfiltration (Filterdruck 5 bar) in 29 g eines Harz/ Wachsgemisches und 9 g klares Tabak-Aromaöl aufgetrennt wurde.After the secondary extraction had ended, 38 g of a two-phase mixture were removed from the flash tank, which was separated by pressure filtration (filter
Das gewonnene Tabak-Aromaöl war frei von Harzen, Wachsen und Polyphenolen und hatte den für Kentucky-Tabak typischen Geruch. Bei der Zugabe von 95 Gew.-%-igem Ethanol erfolgte keine Trübung.The tobacco aromatic oil obtained was free from resins, waxes and polyphenols and had the smell typical of Kentucky tobacco. No turbidity occurred when 95% by weight ethanol was added.
1000 g Burley-Tabak (Wassergehalt 7%, Nikotingehalt 2,85%), wurden in einer Messermühle zerkleinert, in 6 Liter n-Hexan erschöpfend extrahiert und das verwendete Lösungsmittel bei einem Unterdruck von 20 Torr restlos abgedampft.1000 g of Burley tobacco (
Es wurden 65 g lösungsmittelfreier, dunkler, sirupartiger Primärextrakt erhalten, der mit 260 g Magnesiumoxid intensiv vermischt wurde (Mischungsverhältnis 1:4).65 g of solvent-free, dark, syrup-like primary extract were obtained, which was mixed intensively with 260 g of magnesium oxide (mixing ratio 1: 4).
Das Gemisch wurde sodann in einem geschlossenen Hochdruck-Extraktionsbehälter einem zwischengeschalteten C02-Extraktionsschritt und erst dann der Sekundärextraktion unterworfen:The mixture was then subjected to an intermediate CO 2 extraction step in a closed high-pressure extraction container and only then subjected to the secondary extraction:
Das gleiche, noch im Extraktionsbehälter befindliche Material wurde durch Druck- und Temperaturerhöhung folgendermaßen weiter behandelt:
Nach Ablauf der Behandlungszeit wurden dem Entspannungsbehälter 29,7 g eines Zweiphasengemisches entnommen, das durch einfache Filtration in 15,5 g klares Tabak-Aromaöl und 14,2 g Harz-/Wachsniederschlag aufgetrennt wurde.At the end of the treatment period, 29.7 g of a two-phase mixture were removed from the flash tank, which was separated into 15.5 g of clear tobacco aroma oil and 14.2 g of resin / wax precipitate by simple filtration.
Die Ausbeute an klarem Tabak-Aromaöl betrug 1,55% vom eingesetzten Tabak, der Nikotingehalt war 9,55% absolut, das sind 5,2% relativ von dem im Tabak vorhanden gewesenen Nikotin. Das gewonnene Tabak-Aromaöl war frei von Harzen und Wachsen und zeigte bei der Zugabe von 95 Gew.-%-igem Ethanol keinen Niederschlag und keine Trübung.The yield of clear tobacco aroma oil was 1.55% of the tobacco used, the nicotine content was 9.55% absolute, which is 5.2% relative to the nicotine present in the tobacco. The tobacco aroma oil obtained was free of resins and waxes, pointing to the addition of 95 G ew .-% - ethanol no precipitate and no turbidity.
1000 g Orient-Tabak (Izmir) (Wassergehalt 7,2%, Nikotingehalt 1,45%) wurden in 8 Liter Petroläther erschöpfend extrahiert und das Lösungsmitteln bei einem Unterdruck von 15 Torr restlos abgedampft.1000 g of oriental tobacco (Izmir) (water content 7.2%, nicotine content 1.45%) were extracted exhaustively in 8 liters of petroleum ether and the solvent was evaporated off completely at a negative pressure of 15 torr.
Es wurden 58 g lösungsmittelfreier, dunkler, sirupartiger Primärextrakt erhalten, der mit 23,2 g Kieselgur intensiv vermischt wurde (Mischungsverhältnis 1:0,4). Das Gemisch wurde 180 Minuten lang bei einem Druck von 180 bar und einer Temperatur von +20°C in einem geschlossenen Hochdruckbehälter mit CO2 behandelt.58 g of solvent-free, dark, syrup-like primary extract were obtained, which was mixed intensively with 23.2 g of diatomaceous earth (mixing ratio 1: 0.4). The mixture was treated with CO 2 in a closed high-pressure container for 180 minutes at a pressure of 180 bar and a temperature of + 20 ° C.
Der Druck auf der Entspannungsseite betrug 50 bar, die Temperatur +20°C. Die Durchflußmenge an CO2 beträgt 10 kg/Stunde.The pressure on the relaxation side was 50 bar, the temperature + 20 ° C. The flow rate of CO 2 is 10 kg / hour.
Nach beendetem Versuch wurden dem Entspannungsbehälter 20 g eines Zweiphasengemisches entnommen, das durch einfache Filtration in 12 g klares, absolutes Tabak-Aromaöl und 8 g Harz/Wachsniederschlag aufgetrennt wurde.After the end of the experiment, 20 g of a two-phase mixture were removed from the flash tank, which was separated into 12 g of clear, absolute tobacco aroma oil and 8 g of resin / wax precipitate by simple filtration.
Die Ausbeute an klarem Tabak-Aromaöl betrug 1,2% vom verwendeten Tabak, der Nikotingehalt war 23,2% absolut, das sind 19,17 % relativ von dem im Tabak vorhanden gewesenen Nikotin.The yield of clear tobacco aroma oil was 1.2% of the tobacco used, the nicotine content was 23.2% absolute, which is 19.17% relative to the nicotine present in the tobacco.
Der Harz/Wachsniederschlag hatte einen Nikotingehalt von 57,2% absolut, das sind 31,5% relativ von dem im Tabak vorhanden gewesenen Nikotin.The resin / wax deposit had a nicotine content of 57.2% absolute, which is 31.5% relative to the nicotine present in the tobacco.
Das gewonnene Tabak-Aromaöl war frei von Harzen und Wachsen und zeigte bei der Zugabe von 95 Gew.-%-igem Ethanol keinen Niederschlag und keine Trübung.The tobacco aroma oil obtained was free from resins and waxes and showed no precipitation and no clouding when 95% by weight ethanol was added.
Die Ergiebigkeit des erfindungsgemäß gewonnenen Tabak-Aromaöls wurde wie folgt belegt:
- Mit Hilfe bekannter Methoden der Wasserdampfdestillation wurden aus dem gleichen Havanna-Tabak -
wie im Beispiel 1 benutzt - 0,14% klares und in 95 Gew.-%-igem Ethanol. sich nicht trübendes Tabak-Aromaöl gewonnen. Der Nikotingehalt des Aromaöls betrug 0%.
- Using known methods of steam distillation, 0.14% clear ethanol and 95% by weight ethanol were used from the same Havana tobacco as used in Example 1. non-cloudy tobacco aroma oil. The nicotine content of the aromatic oil was 0%.
Zur Beurteilung der Ergiebigkeit wurden in einem Versuch (Versuch A) 200 mg, in einem weiteren Versuch (Versuch B) 250 mg dieses Aromaöls in einer ethanolischen Lösung auf je 1 kg zuvor entaromatisierten Tabak aufgesprüht. In einem weiteren Versuch (Versuch C) wurden 50 mg des nach dem erfindungsgemäßen Beispiel 1 gewonnenen Tabak-Aromaöls in einer ethanolischen Lösung ebenfalls auf 1 kg zuvor entaromatisierten Tabak aufgesprüht.To assess the yield, 200 mg of this aromatic oil were sprayed in an experiment (experiment A) and 250 mg in another experiment (experiment B) in an ethanolic solution onto 1 kg of tobacco which had previously been de-aromatized. In a further experiment (Experiment C), 50 mg of the tobacco aromatic oil obtained according to Example 1 according to the invention were also sprayed onto 1 kg of tobacco which had previously been de-aromatized in an ethanol solution.
Der sensorische Vergleich brachte folgendes Ergebnis:The sensory comparison brought the following result:
Dieser fiel durch seine geringe Aroma-Intensität auf und war auch bezüglich seines gesamten Aromas auch im Rauchgeschmack wenig ausdrucksvoll.This stood out due to its low aroma intensity and was also not very expressive in terms of its overall aroma, even in the smoky taste.
Er war etwas ausdrucksvoller im Aroma, begleitet von Fremdgerüchen, es wurde ferner eine nachteilige Brenzschärfe im Rauchgeschmack festgestellt.It was a little more expressive in the aroma, accompanied by foreign smells, and a disadvantageous sharpness in the smoky taste was also found.
Er hatte ein intensives, reines abgerundetes Aroma ohne Fremdgeruch und war im Rauchgeschmack voller Herzhaftigkeit. Tabak C wurde eindeutig bevorzugt und ist am besten für die Aromatisierung geeignet.He had an intense, pure-rounded flavor without foreign odors and was erzhaftigkeit in smoke flavor full H. Tobacco C was clearly preferred and is best suited for flavoring.
Claims (15)
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BR8302980A BR8302980A (en) | 1982-12-07 | 1983-06-06 | PROCESS FOR OBTAINING AROMATIC SUBSTANCES FROM A TOBACCO STRATE, LIGHT TOBACCO AROMATIC OIL AND EMPLOYMENT |
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DE19813148335 DE3148335C2 (en) | 1981-12-07 | 1981-12-07 | Process for obtaining flavorings from tobacco and their use |
DE3148335 | 1981-12-07 | ||
DE3218760 | 1982-05-18 | ||
DE19823218760 DE3218760A1 (en) | 1982-05-18 | 1982-05-18 | Clear tobacco aroma oil, process for its isolation from a tobacco extract and use thereof |
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EP0081231A2 true EP0081231A2 (en) | 1983-06-15 |
EP0081231A3 EP0081231A3 (en) | 1985-06-19 |
EP0081231B1 EP0081231B1 (en) | 1988-09-07 |
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EP82111300A Expired EP0081231B1 (en) | 1981-12-07 | 1982-12-07 | Process for the production of aromatic substances from a tobacco extract |
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EP (1) | EP0081231B1 (en) |
KR (1) | KR880000170B1 (en) |
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DE (1) | DE3278987D1 (en) |
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- 1982-12-07 GB GB08234899A patent/GB2111371B/en not_active Expired
- 1982-12-07 EP EP82111300A patent/EP0081231B1/en not_active Expired
- 1982-12-07 KR KR8205485A patent/KR880000170B1/en active
Patent Citations (5)
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DE2142205A1 (en) * | 1971-08-23 | 1973-03-15 | Hag Ag | Nicotine removal from tobacco by extraction - preceded by temporary removal of aroma substances |
US3847164A (en) * | 1973-10-11 | 1974-11-12 | Kimberly Clark Co | Method of making reconstituted tobacco having reduced nitrates |
DE2844781A1 (en) * | 1978-10-13 | 1980-04-24 | Hag Ag | METHOD FOR EXTRACTIVE PROCESSING OF VEGETABLE AND ANIMAL MATERIALS |
EP0010665A1 (en) * | 1978-10-13 | 1980-05-14 | HAG Aktiengesellschaft | Process for the extractive treatment of vegetal and animal matter |
GB2031707A (en) * | 1978-10-20 | 1980-04-30 | Philip Morris Inc | Treatment of tobacco |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0338831A2 (en) * | 1988-04-21 | 1989-10-25 | R.J. Reynolds Tobacco Company | Process for providing tobacco extracts |
EP0338831A3 (en) * | 1988-04-21 | 1990-05-02 | R.J. Reynolds Tobacco Company | Process for providing tobacco extracts |
EP0669151A1 (en) * | 1994-02-24 | 1995-08-30 | Matsushita Electronics Corporation | Method for extracting organic substance, solvent for use in said method, and method for measuring content of organic substance |
US5714071A (en) * | 1994-02-24 | 1998-02-03 | Matsushita Electronics Corporation | Method for extracting organic substance, solvent for use in said method, and method for measuring content of organic substance |
EP0822247A2 (en) * | 1996-07-29 | 1998-02-04 | Müller Extract Company GmbH | Tobacco aromatic oil substantially free of nicotine and method of preparation |
EP0822247A3 (en) * | 1996-07-29 | 1998-11-25 | Müller Extract Company GmbH | Tobacco aromatic oil substantially free of nicotine and method of preparation |
EP0908185A1 (en) * | 1997-10-13 | 1999-04-14 | Max Zeller Söhne AG | Process for the production of extracts from medicinal plants |
WO1999018984A1 (en) * | 1997-10-13 | 1999-04-22 | Max Zeller Soehne Ag | Method for producing medicinal plant extracts |
EP1980163A1 (en) * | 2007-04-10 | 2008-10-15 | Litesso-Anstalt | Method for treating tobacco leaves and tobacco leaves and their utilisation |
WO2009110775A1 (en) * | 2008-03-05 | 2009-09-11 | Abat Murzagaliyev | Method of medicinal tobacco oil production |
Also Published As
Publication number | Publication date |
---|---|
DE3278987D1 (en) | 1988-10-13 |
EP0081231A3 (en) | 1985-06-19 |
GB2111371A (en) | 1983-07-06 |
DK528082A (en) | 1983-06-08 |
IN158943B (en) | 1987-02-21 |
AU9118582A (en) | 1983-06-16 |
IE822901L (en) | 1983-06-07 |
EP0081231B1 (en) | 1988-09-07 |
AU555181B2 (en) | 1986-09-18 |
US4506682A (en) | 1985-03-26 |
GB2111371B (en) | 1985-09-11 |
KR840002624A (en) | 1984-07-16 |
KR880000170B1 (en) | 1988-03-12 |
IE53724B1 (en) | 1989-01-18 |
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