JPS58107165A - Transparent tobacco aromatic oil and obtaining same from tobacco extract and use thereof - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is free of polyphenols, resins and waxes and has a reduced nicotine content of 5 to 50 inches (relative to the tobacco from which the tobacco aroma oil is obtained). and to a novel product which is a clear tobacco aroma oil with a tobacco aroma characteristic of the raw tobacco used. Furthermore, the present invention relates to a method for separating transparent tobacco aroma oil from tobacco extracts and its use.

When manufacturing tobacco products, aromas are added to tobacco (
(perpetration) plays a heavy role. Part or all of tobacco aroma oil, which is unique to certain tobaccos, is extracted from highly aromatic tobacco or tobacco waste.
Attempts to isolate it for addition to other less aromatic tobaccos from the same source have previously been unsuccessful. This is because it has proven impossible to isolate anhydrous (clear) tobacco aroma oil that is free of resins and waxes and has a reduced nicotine content.

German Patent Application No. 2.128.779 describes the eluotropic 5eri
es) with one or more solvents located between trichlorethylene and ethyl acetate and from the resulting extract 110 to 1 sot
A method for isolating aroma substances from tobacco and converting aroma precursors is described, characterized in that the aroma precursors are activated by a heat treatment of: The aromatic product obtained by this method is a wax-like resinous substance,
It contains all the waxes and resins of the starting product as well as the polyphenols and (6) and almost all the nicotine.

German Patent Application No. 2.142.205 discloses that in a method for selectively extracting nicotine from tobacco one by one while preserving the aroma, in the first step dry gas is extracted from the dried tobacco at a temperature above the critical point. (e.g. C02) and then temporarily placed in a separate vessel B until the nicotine precipitated in the vessel is extracted from the tobacco in vessel A in a second stage using moist CO2. A method is described, characterized in that the storage is carried out in In the third stage, the aroma substances present in container B are dissolved, for example by Co2 above the critical point, and returned to container A, where they are deposited on the tobacco.

The above methods are expensive and inefficient in obtaining and utilizing tobacco aroma. This is because the product obtained in the first stage is not a clear liquid tobacco aroma oil that can be separated from the resins and waxes, but almost all the undesirable waxes and (7) of the starting product. This is because it is a paste-like material containing resins and undesirable polyphenols.

Moreover, these waxy and resinous substances prevent uniform distribution and aroma transfer in the re-aromatization of the tobacco to be treated. Among other things, polyphenols have the disadvantage of impairing the aroma of smoke.

German Patent Application No. 2,844,781 discloses that by using a two-component solvent such as mol. Methods for extracting substances and, in particular, for processing tobacco are described. The purpose of this two-phase mixture is, for example, to avoid adducts formed in organic solvent extraction and changes in the treated material. When operating under supracritical pressure conditions using only CO2, pressures of 150 bar or more are required to achieve adequate extraction. By the method according to German Patent Application No. 2.844.781, (8) the above-mentioned disadvantages are avoided by adding, for example, a certain amount of alcoholic solvent as a homologous agent for the C02 used for the extraction. I can do it.

This method, like the method according to German Patent Application No. 2,142.205, contains only a small amount of aromatic substances but contains all the wax and resin fractions of the tobacco used for extraction as well as undesired polyphenols. Only a paste-like substance is produced as an intermediate product.

None of the known methods makes it possible to obtain tobacco extracts or tobacco aromas that have a tobacco aroma characteristic of the particular raw tobacco used.

One object of the present invention is that the starting product contains qualitatively and quantitatively almost all aroma substances, is free of resins, waxes and polyphenols, and that the nicotine content is low in the starting product. The object is to obtain a clear and anhydrous tobacco aroma oil which is significantly reduced in comparison.

(9) This object is solved by the method defined in the claims.

Known methods for extracting tobacco with organic solvents or for extracting tobacco with gases above the critical point, such as CO2, always remove almost all resins and waxes and polyphenols of the raw material. Since we only produce pasty aroma products containing
By primary extraction with an organic solvent or a mixture of these solvents with carbon dioxide and a subsequent secondary extraction with C02, a clear tobacco aroma oil and a solid resin/wax mixture free of aromatic compounds are obtained. It is surprising that a two-phase resin/fragrance oil mixture is produced that can be easily separated.

The present invention will now be explained in more detail.

In the present invention, tobacco refers to fermented tobacco leaves, petioles, stems, powder, and tobacco waste.

Tobacco extract in the sense of the present invention means (10) common organic solvents, in particular benzene, toluene, methanol, ethanol, n-propanol, methylethyl acetate;
Extracts prepared using diethyl ether, acetone, n-propane, n-hexane, cyclohexane, petroleum ether, dichloromethane or trichloromethane or mixtures of these solvents. A primary extract in the sense of the invention is still a CO□ extract, i.e. C as a solvent.
This is an extract prepared using 02.

Adsorbents in the sense of the present invention are all customary adsorbents, in particular activated carbon, alumina, magnesium oxide, sodium aluminum silicate, bleaching earth, bentonite, silica gel, diatomaceous earth, zeolitic molecular sheets and the like.

Tobacco aromatic oil in the sense of the present invention is very transparent at room temperature and is free of resins and waxes as well as polyphenols and is from 5 to 50% (in particular from 10 to 50%) of the tobacco from which the tobacco extract is derived. 40%) (11) A tobacco aromatic oil having a reduced nicotine content and which does not form turbidity or sediment when adding 95% by weight ethanol (containing 95% by weight ethanol). It is a liquid.

The preparation of the tobacco extract used according to the invention comprises:
In particular, the tobacco is extracted into one of the above-mentioned solvents or (in the case of organic solvents) a mixture of solvents.

Preferably one of the abovementioned solvents (preferably CO
2, n-hexane or dichloromethane) 3 to 30
One part by weight of the pre-milled tobacco is extracted using one part by weight. Depending on the efficiency of the extraction equipment present, the -order extraction is
It is applied for at least 10 minutes and at most 10 hours, preferably 1 to 5 hours.

If organic solvents are used, the subsequent extraction is carried out under conditions of atmospheric pressure.

If CO2 is used in the -secondary extraction, the pressure and temperature conditions in the extraction vessel and the separation vessel, as well as the extraction time and the CO2 flow rate (-(12) stage), are specified below in connection with the second extraction. equal.

Undissolved residues from the treatment with these solvents are separated and the solvent-containing extract is concentrated by evaporation until a syrupy solvent-incompatible tobacco extract is obtained. If organic solvents are used, the evaporation is preferably carried out under reduced pressure, particularly preferably at about 15 wHI. If C02 is used, the evaporation is carried out in a separation vessel (in four stages), as already mentioned.
The secondary extraction is carried out under the pressure and temperature conditions described below.

The tobacco-subextract thus obtained contains, inter alia, polyphenols, resins/waxes and nicotine and, as the inventors have found, is especially suitable for the subsequent sub-extraction (using co2'6). Present in a suitable readily obtainable form.

The obtained tobacco sub-extract is then thoroughly mixed with the adsorbent until, according to the invention, there is a homogeneous distribution between the extract and the adsorbent (13). Particularly suitable adsorbents for this process are sodium aluminum silicate, bentonite, magnesium oxide and zeolitic molecular sheets. The mixing ratio of extract to adsorbent can be varied and adjusted to suit the consistency of the extract, the density and particle size of the adsorbent and the desired consistency resulting from the mixing. . Generally 1:0.1 to 1
A mixing ratio of extract to adsorbent of 10 :1 is suitable;
Powdered extracts having a mixing ratio of extract to adsorbent of 0.3 to 1:6 are preferred.

The extract/adsorbent mixture should not fall below a ratio of 1:0.1. This is because the adsorbent used according to the invention provides a transparent, water-free tobacco aroma that can be easily separated from the dissolution of aromatic substances and resins and waxes in the subsequent secondary extraction (in the extraction vessel) using C02. This is because it has a significant effect on oil separation.

(14) Mixing ratios greater than 1:10 still result in better dissolution and separation of tobacco aroma oil, but a larger pressure vessel volume must be accommodated -6° between primary extract and adsorbent. According to the invention, in a first pressure vessel (extraction vessel), preferably a high-pressure vessel, the mixture is
02 as an oily liquid that can be easily separated from the resin and wax in a second pressure vessel (separation vessel) followed by the above extraction vessel under constant pressure and temperature conditions. Process until it exists.

This secondary extraction with C02 according to the method of the invention is the C0 used to extract the extract/adsorbent mixture.
2 above the critical point with respect to pressure and temperature (〉73 bar and ) 31.3 T:) or to the critical point F with respect to pressure and temperature (〈73 bar and <31';
3t') or above the critical point with respect to pressure (>73 bar) and below the critical point with respect to temperature (<31.3 t
″) is achieved by (15).

When operating under conditions above the critical point regarding pressure and temperature, a pressure of 85 to 250 bar and +35
A temperature of +qoc is preferably selected. When operating in subcritical pressure and subcritical temperature ranges, a pressure of 25 to 70 bar and +5υ
A temperature of +25'C is preferred. When operating in the supercritical pressure and subcritical temperature range, pressures of 85 to 200 bar and temperatures of +10'C to +30υ are preferred.

If a particularly low nicotine content is desired in the final product (secondary extract) (e.g. 5 to 10% with respect to the tobacco used for the second extraction), an additional Co2 extraction step at low temperature can be claimed. It can be inserted between the primary extraction defined in the range and the secondary extraction defined in the range. For this purpose, the extract obtained in the primary extraction and mixed with the adsorbent is treated, inter alia, at an extraction temperature of <-2 sr to +5 υ and a Co2 extraction pressure of about 20 to 25 bar: In the inserted Co2 extraction step, the separation vessel is depressurized at subcritical pressure and temperature conditions, with the separation vessel at a temperature of about +15 t' to +30 υ and a pressure of about 2 to 15 bar. ) of nicotine is preferred for separation.

extraction time of 0.5 to 2 hours, preferably about 1 hour;
and 5 to 50 kg/hr, preferably 10
A CO□ flow rate of between 30 and 30 kg/hr is sufficient for this process. Surprisingly, this intervening CO2 extraction step almost exclusively removes nicotine and other secondary alkaloids (but e.g. aromas, resins, waxes, etc.) from the extract/adsorbent mixture. (excluding other components which are themselves Co2 soluble, such as polyphenols etc.) are bathed out and precipitated in a separation vessel. The nicotine obtained is removed from the separation vessel before the next secondary extraction (aromatic extraction) with CO□ begins.

(17) In the process according to the invention as defined in the claims, especially in the secondary extraction, the separation conditions in the expansion vessel (separation vessel) are determined by the quality of the product isolated according to the invention. and critical to quantity. The expansion pressure and the expansion temperature are advantageously in the range below the critical point of CO□ (subcritical pressure/subcritical temperature). 45
A pressure of about 50 to 55 bar and a temperature of about 15 to 30 bar are preferred;
Temperatures between 0 and 25'C are particularly preferred. Separation within the expansion vessel is preferably carried out with a simultaneous pressure and temperature reduction with respect to the pressure and temperature conditions within the extraction vessel.

The amount of CO2 flowing through the extraction vessel and the length of the flow-through treatment are also important for the method according to the invention. 0.
A total treatment time of 5 to 8 hours, preferably 5 to 5 hours and particularly preferably 2 to 4 hours is advantageous, and a total treatment time of 0.3 to 3 hours per kg of untreated tobacco is preferred.
Stg/h, (18) preferably 3 to 50 to 4/h and particularly preferably 5 to 15 kg/h total C02 flow rate is advantageous.

As already mentioned above, the pressure and temperature in the extraction vessel,
0 as indicated above for the (1-stage) secondary extraction, such as pressure and temperature in the separation vessel, extraction time and Co2 flow rate.
The conditions for the 02 extraction are also valid for the -order extraction if CO□ is used as solvent in the -order extraction.Therefore, there is no need to specifically enumerate these parameters again in the case of the primary extraction.

In the process according to the invention, upon removal from the expansion vessel after the end of the secondary extraction, a solid/oil mixture is obtained which is already present as two phases. By simple F:iM, this mixture can be separated into a clear and anhydrous tobacco aroma oil containing no polyphenols and with a significantly reduced nicotine content, and a solid resin/wax mixture with a relatively high nicotine content.

Another special feature of the tobacco aroma oil isolated according to the invention (19) is that it has a tobacco aroma characteristic of the particular raw tobacco from which it is used. This property clearly distinguishes it from other tobacco extracts that exist. This is because it has not been possible to prepare the unique aroma of a specific raw material tobacco using any conventional tobacco extract. Due to this feature of the tobacco extract isolated according to the invention, its material composition is considered to be completely novel compared to the known technology.

Starting from a product (secondary tobacco extract) containing at the same time aroma substances, polyphenols, nicotine, resins, waxes 2 and other substances, the present invention provides for the first time a transparent anhydrous oil - this tobacco aromatic product. Separation and retrieval are achieved in a simple manner and with particularly effective results. Neither the process itself nor the products obtained have been described or suggested in the prior art.

In the product obtained according to the invention, (20) an easily separable tobacco aroma oil with a significantly reduced nicotine content and free of polyphenols, resins and waxes after the secondary extraction has ended; It is remarkable and surprising that the clear layer of 100% and the resin/wax layer containing most of the nicotine of the primary extract is removed from the expansion vessel.

The tobacco components isolated by the primary extraction in the process according to the invention, in a mixture with a powdered adsorbent and in the subsequent secondary extraction (with C02), with respect to their viscosity and solubility and separation properties, e.g. It was surprising that it behaved quite differently than the same component subjected only to extraction (CO□-subextraction).

This fact is very evident in the case of the particularly effective nicotine extraction optionally inserted according to the invention (possibly an intermediate extraction step). Thus, according to previous knowledge, nicotine and polyphenols can only be extracted using CO2 from, for example, tobacco (21) leaves only in the presence of moisture. However, in the process according to the invention, despite not adding or using water in any step, almost all of the nicotine is eluted from the primary extract prepared according to the invention and in the separation vessel. precipitates. This new finding shows that still (if desired) almost pure nicotine can be extracted from the extract/adsorbent mixture at temperatures between -25'C and +5J (
Drying) brings about an alternative method according to the invention in which it is selectively extracted by CO2 extraction.

What is even more surprising is the yield and purity of the product prepared according to the invention as well as its effectiveness in improving its flavor.

Particularly little was known about the aromatic oil of tobacco. Aromatic oils isolated by conventional methods have only been prepared on a laboratory scale by steam distillation. The resulting oil was accompanied by a number of external odors, such as chamomile, fennel, pepper, valerian and amyl(22) alcohol, probably caused by the formation of the processed product. The yield of this type of tobacco oil was about 0.1 to 0.2 inches.

As already mentioned, there are distinct differences between these tobacco oils and the tobacco aroma oils which have the pure aroma characteristic of the particular source tobacco isolated and used according to the invention. Thus, for example, an aromatic oil isolated from Havana tobacco has a Havana tobacco aroma, while an aromatic oil obtained from Kentucky tobacco has a Kentucky tobacco aroma. Similarly, aromatic oils isolated from Virginia, Turkish or Burley tobacco each have a pure aroma characteristic of that particular type of tobacco. Owing to this special feature, which clearly differs from the prior art, it can be said that the tobacco aroma oil 1 isolated according to the invention is completely new in its substance composition compared to the products according to the prior art. .

Tobacco isolated by the method according to the invention (23) The aromatic oil is free of extraneous aromas, free of polyphenols, resins and waxes and has a reduced nicotine content of 5 to 50 grams with respect to the tobacco leaf used. content and yield of 0.8 to 2.5% (anhydrous oil)
It can be obtained with

Regarding the effects of tobacco poisoning, according to the invention, the product isolated from Havana tobacco, for example, contains at 50 ppm the same aroma as the aroma product isolated from Havana tobacco by the already known steam distillation (2507) pm. It has the effect and strength of

A further object of the invention is the use of the tobacco aromatic oil obtained according to the invention in the preparation of tobacco or tobacco products, in which case the preparation not only involves the application of IK to the tobacco, but also the porous This can be done by poisoning the carrier material or tobacco adhesive.

When applied directly to tobacco, the tobacco aroma oil according to the invention is suitable for use as a "top flavor" as well as for the deterioration of weakly aromatic or recycled tobacco (24) by means of the sauce (casing). Are suitable.

Another method of infliction consists in applying tabap aroma oil onto a porous carrier material that is fused with tobacco or tobacco products. Such porous carrier materials include, for example:
Present in the form of pieces of paper or clay, dummies, internal packaging materials (eg cardboard boxes, bags and the like).

As another embodiment of the harm caused by the use of tobacco aroma oils according to the invention, mention should also be made of their addition to adhesives for tobacco production. Examples of such containers are adhesives commonly used in tobacco manufacturing, such as adhesives for cigar outer wraps, double-cut tobacco paper, and other containers.

The tobacco aroma oil obtained according to the invention decisively influences the variations that may or may occur during the production of tobacco (differences in quality or differences in smoke aroma).

The amount of tobacco flavor oil used in the formulation of tobacco or tobacco products will vary depending on the nature of the tobacco and the desired (25) formulation. For example, in the case of the aromatic oil obtained according to the invention from Novana tobacco, tobacco IIc
g, preferably 25 to 1 oomg, particularly preferably 40 to 60 mg, i.e. 25 to 1001:
+pm, preferably 40 to 60 ppm tobacco aroma oil is used.

The excellent effect and intensity obtained with the products according to the invention are increased in particular by the presence of resin-, polyphenol- and wax-free tobacco aroma oils. This special property of this tobacco aroma oil shows special properties and novel characteristics compared to the prior art.

A particularly neglected apparatus for carrying out the secondary extraction according to the invention is described below (see accompanying drawings).

Liquid CO2 is removed from tank 1 at a pressure and temperature below the critical point. The heat exchanger 2 adjusts the temperature of Co2 to a desired critical temperature or above,
A desired pressure above or below the critical level is obtained by the high pressure pump 3. CO2 through the flow meter 16
Extraction (26) A vessel 4 is reached, where the mixture of sub-extract and adsorbent is extracted. The loading and unloading of the product into the extraction vessel 4 takes place intermittently by opening and closing the top opening after each extraction. The pressure within the extraction vessel is determined by a pressure valve 14. The liquid or fluid 002 containing the dissolved tobacco contents is led to a pressure regulating valve 8 (=pressure relief valve) via a butterfly valve 6, and then introduced into a pressure relief container 10 via a heat exchanger 9. be done. C.O.
2. Separation of the tobacco contents completely dissolved in
and is supported by a decrease in temperature in the heat exchanger 9. The extracted tobacco components are separated into a clear tobacco aroma oil and a waxy IM fatty nicotine product in an expansion vessel 10, which can be pumped through a valve 17 either continuously or after the extraction is finished in the vessel. It is removed by opening 10.

At the end of each brew, the brew side of the device is also depressurized by opening valve 5. During extraction, the Co2 leaving the expansion vessel 10 is recycled via conduit 11 (27). Control of the device is carried out manually or by means of an electric control device 12, to which as inputs the temperature in the extraction vessel 4 measured by a thermocouple 13, the pressure measured by pressure gauges 14 and 15. , the flow of CO2 leaving the pressure vessels 4 and 10 and the flow rate measured by the flow meter 7 are used. Depending on these measured values, the cooling in the pressure regulating valve 8 and the heat exchanger 9 is regulated.

If C02 is used as the solvent for the primary extraction, the equipment shown and described in the drawings is also used here.

The following examples illustrate the invention without limiting it.

Nicotine was measured by spectroscopic analysis using Kuhn (H, Ku
hn) method ("Handbook of Food Chemistry" Vol. 6 (1970) No. 621-525 ("H
anabuck der Lebensmittelc
hemie” Bd, VI, (1970) 5ei
321 bis 325)).

(28) Example 1 Havana tobacco 1,000. ! 9 (water content = 6.5 h, nicotine content: 1.27%) is ground in a blade mill and extracted thoroughly in 1 ol of dichloromethane, and the solvent is evaporated under reduced pressure of 15y+mHjF.

75 g of solvent-free dark syrupy dichloromethane extract (sub-extract) is obtained, which is thoroughly mixed with 90 I of sodium aluminum silicate (Na-A4 zeolite) in a kneading machine (mixing ratio: 1:1.
2).

This mixture was extracted using 002 in a closed high-pressure extraction vessel kept at a pressure of 230 bar and a temperature of 65 υ.
Processed for 20 minutes. The pressure on the relief side was 50 bar and the temperature tI' was 124 r.

The flow rate of C02 is 6 kg/hr.

At the end of the experiment, remove the two-phase mixture 40.1 from the expansion vessel.
g was removed and a clear oily tobacco aroma oil 22.5 fi and resin/wax precipitate 1 was removed by simple PJM.
7.69.

(29) The yield of clear anhydrous tobacco aroma oil was 2.25% of the tobacco used. Nicotine content is 19°22
%, which was 35% in terms of nicotine present in tobacco.

The yield of resin/wax precipitate was 1.76% and the nicotine content was 43 T (absolute), or 60 T with respect to the nicotine present in the tobacco.

The resulting tobacco aroma oil was free of resins and waxes, and did not precipitate or become cloudy even when 95% ethanol was added.

Example 2 Centara key tobacco (water content: 8.0%, nicotine content: 1.7%) 1.000p was ground with a cutting mill and extracted using CO2 as a solvent in an Oo2 high pressure extraction device (see drawing). Extract.

Extraction conditions: Pressure in the extraction vessel 250 bar Temperature in the extraction vessel: 40T: Pressure in the expansion vessel = 55 bar (30) Temperature in the expansion vessel: 22mm Processing time:
3 hour CO2 flow rate:
After the end of the 8 to 9/hr extraction, 70 g of a brown hard paste (extract) is removed from the expansion vessel and thoroughly mixed with 140 g of bentonite).

This mixture is subjected to a secondary extraction using Co2 under the same conditions as described in Example 1.

After the completion of the secondary extraction, the two-phase mixture 38 is removed from the expansion vessel.
g was removed and by high pressure filtration (5 bar filtration pressure) 29 g of resin/wax mixture and 9 I of clear tobacco aroma oil were removed.
It was separated into

The resulting tobacco aroma oil was free of resins, waxes and polyphenols, and had the characteristic scent of Kentucky tobacco. Even when ethanol was added at a concentration of 95%, no turbidity occurred.

Example 3 ・"Burley tobacco (water content -4itnear%, nicotine content: 2.85
h) 1,000 g of the powder (31) was ground in a blade mill, thoroughly extracted in n-hexane 61, and the solvent used was evaporated under reduced pressure of 20 gmHjF without leaving any residue.

Dark syrupy primary extract containing no solvent 65
This product was thoroughly mixed with 260 g of magnesium oxide (mixing ratio: 1:4).

This mixture was then subjected to an intermediately connected 002 extraction step in a closed high-pressure extraction vessel and then only to a secondary extraction: 1st stage: Co2 extraction temperature: -17rCO7 extraction pressure Crab 20 bar expansion vessel Temperature inside: +18υ Pressure inside the expansion vessel;
8 barrel processing time = 40
The minute CO2 flow rate is 25 kg/hr.

After the above processing time had elapsed, an almost colorless, odorless oil 25J7'' was removed from the expansion vessel.

The nicotine content of this oil was 94.1% (vs.), which was 82.5% with respect to 2(32) cotine recompressed into tobacco.

Second stage (secondary extraction): The same material still present in the extraction vessel was further processed at increased pressure and temperature as follows: CO2 extraction temperature: CO2 extraction pressure at +15; 60 bar in the expansion vessel Temperature: +20υ pressure crab in expansion vessel
50 barrels 2nd stage processing time: 200
The minute Co2 flow rate was 15 Icg/hr.

After the above treatment time has elapsed, the two-phase mixture 29.7 f
1 is removed and by simple filtration clear tobacco aroma oil 1
5.5.9 and resin/wax precipitate 14.29.

The yield of clear tobacco aroma oil is 1.5% of the tobacco used.
55%, and the nicotine content is 9.55% (absolute value)
, i.e. 5.2 with respect to the nicotine present in the tobacco.
%Met. The isolated tobacco aroma oil was free of resins and waxes, (53) and did not precipitate or become cloudy upon addition of 95 wt % ethanol.

Example 4 Turkish tobacco (Izmir) (water content near 2%, nicotine content: 1.45t) 1.0
00 g was thoroughly extracted in petroleum ether 81 and solvent 1
Evaporate under reduced pressure of 5 mm Hp until no residue remains.

58 g of a dark syrupy extract containing no solvent was obtained, which was thoroughly mixed with 25.29 g of diatomaceous earth (mixing ratio: 1:0.4). This mixture was treated with CO2 for 180 minutes at a pressure of 180 bar and a temperature of +20 bar in a closed high-pressure vessel.

The pressure on the relief side was 50 par, and the temperature was +20υ. The flow rate of 002 is 10 to 9/hr.

At the end of the experiment, 20 g of the two-phase mixture was removed from the expansion vessel, which was separated by simple filtration into 12 g of clear tobacco aroma oil and 81 resin/straw (34) cous precipitate.

The yield of clear tobacco aroma oil is 1.5% of the tobacco used.
2%, and the nicotine content is 23.2% (absolute value), i.e. 3% with respect to the nicotine present in the tobacco.
It is 1.5%.

The isolated tobacco aroma oil was free of resin and wax, and did not precipitate or become cloudy even when 95% ethanol was added.

Example 5 The results of the tobacco aroma oil isolated according to the invention were shown as follows: 0.14% of the clear tobacco aroma oil, which did not become cloudy in ethanol at a concentration of 95% by weight, compared with the known Obtained from the same Havana tobacco used in Example 1 using a steam distillation method. The nicotine content of this aromatic oil was 0.

To evaluate the results, in one experiment (Experiment A), 11 cg of previously deodorized tobacco was sprayed with 200 m9 of the above aromatic oil in an ethanol solution, and in another experiment (Experiment B) ( 35) was similarly sprayed at 250 mg. In another experiment (experiment C), 50 m9 of tobacco aroma oil, isolated according to the invention analogously to Example 1 and dissolved in a solution of ethanol, was sprayed onto 1 kg of pre-deodorized tobacco.

In the sensory test, the following results were obtained: Tobacco from Experiment A: The aroma intensity was noticeably low, and the smoke aroma was not very strong compared to the overall aroma.

Tobacco from Experiment B: This was somewhat strong in aroma, but was accompanied by other aromas, and the smoke had an undesirable burnt sharpness.

Experiment C tobacco: It had a strong, pure, mellow aroma with no other aromas, and had a strong savory flavor in the smoke aroma. Tobacco C is clearly preferred and most suitable as a flavoring agent.

(56)

[Brief explanation of the drawing]

The drawing shows an example of a device for carrying out the method according to the invention. In the diagram above, the main parts are shown with reference numbers as follows: 1...Liquid CO2 tank 2...Heat exchanger 3...High pressure pump 4...Extraction vessel 5...Valve 6... Butterfly valve 7... Flow meter 8... Pressure control valve 9... Heat exchanger 10... Expansion vessel 11... Conduit 12... Control device 13... Thermocouple 14, 15...Pressure gauge 16...Flow meter (37) 17...Valve (38)

Claims (1)

[Claims] 1. Tobacco extract obtained using a solvent (-sub-extract)
is mixed with an adsorbent, this mixture is subjected to a secondary extraction with CO2 in a closed pressure vessel (extraction vessel), and easily separated from the resin and wax in a second closed pressure vessel (separation vessel). A method for obtaining tobacco aroma oil from tobacco extract, characterized in that a transparent tobacco aroma oil is isolated having a reduced nicotine content. Benzene as a solvent for preparing the Z-order extract;
Toluene, methanol, ethanol, n-propertool, methyl ethyl acetate, diethyl ether, acetone, furopane, n-hexane, cyclohexane, petroleum ether, dichloromethane, trichloromethane, or (
1) A method according to claim 1, in which a mixture of these solvents or carbon dioxide is used. 3. Magnesium oxide as an adsorbent during secondary extraction,
3. Process according to claim 1, characterized in that activated carbon, aluminum oxide, sodium aluminum silicate, bleaching earth, bentonite, silica gel, diatomaceous earth or zeolitic molecular sieves are used. 4. Process according to any one of claims 1 to 3, characterized by a primary extract:adsorbent mixing ratio of 4.1=0.1 to 1:10. 5. Secondary extraction with 002 in the extraction vessel under conditions of pressure and temperature above the critical point, under conditions of pressure and temperature below the critical point, or under conditions of pressure and temperature above the critical point and temperature below the critical point. The method according to any one of claims 1 to 4, which is carried out in the following. 6. The method according to any one of claims 1 to 5 (2), wherein the separation container is depressurized to a pressure and temperature condition F below the critical point during the secondary extraction with CO2. 7. According to any one of claims 1 to 6, wherein a tobacco aromatic oil is obtained in which the nicotine content of tobacco leaves is reduced by 5 to 50 h (relative to the nicotine content of tobacco leaves before extraction). Method described. 8. In order to reduce the nicotine content in tobacco aroma oil by 5 to 10 V (relative to the nicotine content of tobacco leaves before secondary extraction), the secondary extraction with CO2 is carried out in two steps: a. In the extraction vessel. A first extraction step with CO□ at 125'C+5 at this temperature and a pressure of about 20 to 25 bar, and then increasing the pressure and temperature in the extraction vessel to 25 bar and 5T: 8. A method according to any one of claims 1 to 7, carried out in a second extraction stage in which the extraction stage is increased to . 9. The method according to claim 3 (8), wherein the separation vessel is depressurized under pressure and temperature conditions below the critical point. 10. The method according to any one of claims 1 to 9, wherein the secondary extraction with CO2 is carried out for 0.5 to 8 hours. 11. Claims 1 to 10 characterized in that in the secondary extraction, Co2 is added at a rate of 0.3 to 35 kg/hr per 1 kg of tobacco from which the tobacco extract is obtained.
The method described in any of the paragraphs. 1z The product obtained during the secondary extraction in a separating vessel is separated by filtration into resin and wax on the one hand and into clear tobacco aroma oil on the other hand. Any method described. 16. A transparent tobacco aroma oil, characterized in that it is free of polyphenols, resins and waxes and that the tobacco extract has a nicotine content of 5 to 50 Ti, relative to the original weight of the tobacco obtained therefrom. 14. Compounding tobacco or tobacco products with a clear tobacco aroma oil free of polyphenols, resins and waxes and from which tobacco extracts are obtained (4) having a nicotine content of 5 to 50 T with respect to the original weight of the tobacco. A method of using the transparent tobacco aroma oil as described above. 15. Claim 1, in which the infliction is carried out directly on the tobacco or to the porous carrier or tobacco adhesive
How to use as described in Section 4.