WO2022137745A1 - Tobacco-component-concentrated liquid, method for manufacturing same, flavor-producing article, and method for manufacturing same - Google Patents

Abstract

Provided is a method for manufacturing an inexpensive tobacco-component-concentrated liquid, the method making it possible to concentrate a flavor component to a high degree of concentration while adequately retaining the flavor component. This method for manufacturing a tobacco-component-concentrated liquid includes a step for concentrating a tobacco-component-containing liquid through a progressive freeze concentration method.

Description

Tobacco component concentrate and its manufacturing method, flavor-producing article and its manufacturing method

The present invention relates to a tobacco component concentrate and a method for producing the same, and a flavor-producing article and a method for producing the same.

Extraction of tobacco components from tobacco raw materials is carried out for the purpose of improving the flavor of the tobacco raw materials and reducing the content of other components in the tobacco raw materials.

For example, in Patent Document 1, the residue after extracting the leaf tobacco material with a low-polarity solvent is further extracted with a high-polarity solvent, and the extract extracted with the low-polarity solvent is applied back to the residue to obtain a tobacco having a good flavor. Methods for obtaining raw materials are disclosed. Further, in Patent Document 2, a tobacco material is extracted with a solvent to provide an extract and a residue, and the extract is treated with a phenol oxidase to reduce the amount of phenolic compound, and then combined with the residue. Disclosed are methods of preparing tobacco products with reduced amounts of phenolic compounds. Further, Patent Document 3 discloses a method of mixing a fraction obtained by steam-distilling leaf tobacco as an essential oil with other materials. Further, Patent Document 4 discloses a method for preparing a distillate by distilling a tobacco raw material under reduced pressure.

International Publication No. 2015/029999 Japanese Patent Publication No. 2002-520005 Special Publication No. 60-045909 Chinese Patent Application Publication No. 104757703

Since the extract, fraction, and distillate obtained by the above method contain an extraction solvent such as water, when it is added to a tobacco product as it is, it is necessary to vaporize and remove the extract solvent. However, the removal operation is energy costly. Therefore, it is conceivable to concentrate the extract or the like in advance before adding the extract or the like to the tobacco product. By carrying out this concentration operation, not only the removal operation becomes unnecessary, but also the volume of the extract or the like can be reduced, so that the transportation cost and the storage cost can be reduced. Further, when the extraction solvent is water, the water content can be reduced by the concentration operation, so that the growth of microorganisms in the liquid can be suppressed and the storage stability is improved.

Examples of the solution concentration method that is widely practiced include an evaporation concentration method, a membrane concentration method, and a freeze-drying method. The evaporation concentration method is a method of vaporizing and removing the solvent in the solution by heating the solution. Since the method can be carried out with a simple device, the device cost can be kept low. However, when it is used for concentrating an extract containing a tobacco component, a component useful for imparting flavor (hereinafter referred to as a flavor component) contained in the tobacco component volatilizes and dissipates or deteriorates due to heating. There is. In addition, a lot of energy is required to remove the solvent.

The membrane concentration method is a method of separating the solvent from the solution by applying pressure to the solution using an RO membrane (reverse osmosis membrane) or the like. Since the method can be carried out at room temperature, thermal denaturation of the components in the solution can be suppressed, and since no phase change is involved in the concentration separation process, energy consumption can be suppressed low. However, it is difficult to concentrate at a high concentration, and since the concentration operation is performed at room temperature, there is a possibility of microbial contamination. In addition, it takes time and money to clean and replace the membrane.

The freeze-drying method is a method of removing the solvent by sublimating the solvent from the frozen raw material. The method is often also used to concentrate liquids. In this method, since the solvent in the raw material is solid over the entire drying period, it is liquid and does not move in the raw material. In addition, since it is dried at a low temperature, it is possible to suppress thermal denaturation and chemical changes of the material. However, this method has many technical problems to be overcome, and the cost is high in terms of energy consumption and capital investment. Therefore, at present, it is practically applied only to some foods such as fruits. The situation is.

The present invention includes a method for producing a low-cost tobacco component concentrate, a tobacco component concentrate obtained by the method, and a method for producing the tobacco component concentrate, which can be concentrated to a high concentration while sufficiently retaining the flavor component. It is an object of the present invention to provide a method for producing a flavor-producing article and a flavor-producing article obtained by the method.

The present invention includes the following embodiments.

[1] A method for producing a tobacco component concentrate, which comprises a step of concentrating a liquid containing a tobacco component by an interface advance freeze concentration method.

[2] Before the step of concentrating the liquid containing the tobacco component by the interface advance freeze concentration method,
The method according to [1], further comprising a step of extracting a tobacco component in a tobacco raw material with a solvent and producing a liquid containing the tobacco component.

[3] The method according to [2], wherein the solvent contains water.

[4] Before the step of concentrating the liquid containing the tobacco component by the interface advance freeze concentration method,
The method according to any one of [1] to [3], further comprising the step of filtering the liquid containing the tobacco component to remove the solid matter.

[5] In the chromatogram obtained by gas chromatography with mass spectrometer (GC / MS) when the tobacco component concentrate is headspaced, the peak of the compound group of RI2000 or less with respect to the total area of the entire peak. The method according to any one of [1] to [4], wherein the ratio of the total area of is 70% or more.

[6] A tobacco component concentrate produced by the method according to any one of [1] to [5].

[7] A step of producing a tobacco component concentrate by the method according to any one of [1] to [5], and
A step of applying the tobacco component concentrate to a base material and drying it to produce a tobacco component-containing base material.
The process of manufacturing a flavor-producing article containing the tobacco component-containing base material, and
A method for producing a flavor-producing article, including.

[8] A flavor-producing article produced by the method according to [7].

[9] The flavor-producing article according to [8], which is a combustion-type flavor suction device or a non-combustion heating-type flavor suction device.

According to the present invention, a method for producing a low-cost tobacco component concentrate, a tobacco component concentrate obtained by the method, and a method for producing the tobacco component concentrate, which can be concentrated to a high concentration while sufficiently retaining the flavor components. It is possible to provide a method for producing a flavor-producing article containing, and a flavor-producing article obtained by the method.

It is sectional drawing which shows an example of the freeze-concentrator which can be used in the interface advance freeze-concentration method in this embodiment. It is sectional drawing which shows an example of the combustion type flavor suction apparatus which concerns on this embodiment. An example of the non-combustion heating type flavor suction system according to the present embodiment, (a) a state before inserting the non-combustion heating type flavor suction device into the heating device, and (b) heating the non-combustion heating type flavor suction device. It is a schematic diagram which shows the state which is inserted into an apparatus and is heated. It is a chromatogram obtained by component analysis of the tobacco component concentrates of Example 1 and Comparative Example 1. It is a graph which shows the total peak area in each RI range of the chromatogram of FIG.

[Manufacturing method of tobacco component concentrate]
The method for producing a tobacco component concentrate according to the present embodiment includes a step of concentrating a liquid containing a tobacco component (hereinafter, also referred to as a concentration step) by an interfacial forward freezing concentration method. The "freeze concentration method" is a method of increasing the concentration of a solution by cooling the solution, selectively solidifying the solvent in the solution, and physically separating and removing the solidified solvent. In the above-mentioned "freeze-drying method", since the solution is completely frozen and then only the solvent is sublimated and removed, only the solvent in the solution is selectively solidified and removed by cooling. It is different from "law". In the method according to the present embodiment, the liquid containing the tobacco component is concentrated by the interfacial forward freezing and concentration method, which is one of the freeze and concentration methods. The "interface forward freeze concentration method" is a method of concentrating a solution by forming crystals of a single large solvent solidified product by cooling.

In the method according to the present embodiment, since the concentration operation is performed at a low temperature, it is possible to prevent the flavor component contained in the liquid containing the tobacco component from volatilizing and dissipating or deteriorating. That is, in this method, the flavor component can be concentrated while being sufficiently retained. In addition, since it is concentrated at a low temperature, contamination by microorganisms can be suppressed. Further, since only the solvent is selectively solidified and the solidified solvent is separated and removed, the concentration of the concentrated solution can be sufficiently increased. Further, as compared with, for example, the evaporation concentration method, the latent heat required for the phase change is about 1/7, which saves energy and can suppress the running cost. Among the freeze-concentration methods, the method according to the present embodiment is cheaper than other freeze-concentration methods such as the suspension crystallization method because the liquid containing the tobacco component is concentrated by the interfacial forward freeze-concentration method. Also, the highly viscous liquid can be concentrated.

The method according to the present embodiment is not particularly limited as long as the concentration step is included, but prior to the concentration step, a step of extracting the tobacco component in the tobacco raw material with a solvent to produce a liquid containing the tobacco component (hereinafter referred to as “)”. It is also preferable to further include a tobacco component extract manufacturing process). Further, it is preferable that the method further includes a step of filtering a liquid containing a tobacco component to remove a solid substance (hereinafter, also referred to as a filtration step) before the concentration step. When the method includes both the tobacco component extract manufacturing step and the filtering step, the filtering step can be carried out after the tobacco component extract manufacturing step and before the concentration step. Moreover, the method can further include other steps other than these steps. Hereinafter, each step will be described, but the method according to this embodiment is not limited to the embodiment related to each of these steps.

(Tobacco component extract manufacturing process)
It is preferable that the method according to the present embodiment further includes a step of extracting the tobacco component in the tobacco raw material with a solvent and producing a liquid containing the tobacco component before the concentration step. That is, the liquid containing the tobacco component is preferably a tobacco component extract obtained by extracting the tobacco component in the tobacco raw material with a solvent. By this step, a liquid containing a tobacco component (tobacco component extract) can be easily produced.

Various types of tobacco contained in tobacco raw materials can be used. For example, yellow varieties, Burley varieties, Orient varieties, native varieties, other Nicotiana-Tabacam varieties, and Nicotiana rustica varieties can be mentioned. These varieties can be used alone or blended to obtain the desired flavor. Details of the tobacco varieties are disclosed in "Tobacco Encyclopedia, Tobacco Academic Studies Center, 2009.3.31".

The shape of the tobacco raw material is preferably a shape suitable for extracting tobacco components, and may be, for example, a crushed tobacco product. As for the size of the tobacco raw material, for example, when the shape of the tobacco raw material is a crushed tobacco product, the average particle size can be 10 μm or less.

The solvent used for extraction is not particularly limited, and examples thereof include water, ethanol, chloroform, ethyl acetate and the like. These solvents may be used alone or in combination of two or more. Among these, water is preferable as the solvent from the viewpoint of easy control of freeze concentration.

The mass ratio of the tobacco raw material to the total mass of the solvent and the tobacco raw material at the time of extraction is preferably 5 to 20% by mass, more preferably 8 to 15% by mass from the viewpoint of efficient extraction. The extraction temperature depends on the extraction solvent, but can be, for example, 20 to 60 ° C. The extraction time depends on the extraction solvent and the extraction temperature, but can be, for example, 1 to 3 hours. Extraction can be carried out, for example, by introducing a tobacco raw material and an extraction solvent into an extraction device and stirring them.

The "liquid containing a tobacco component" in the method according to the present embodiment is not limited to the tobacco component extract, and may be, for example, a distillate obtained by distilling a tobacco raw material, a squeezed liquid of a tobacco raw material, or the like. ..

(Filtration process)
The method according to the present embodiment preferably further includes a step of filtering a liquid containing a tobacco component to remove solid matter before the concentration step. By carrying out the filtration step, solid substances contained in the liquid containing tobacco components such as proteins and suspended solids can be removed. As a result, it is possible to suppress the incorporation of the flavor component into the solidified solvent in the cooling process in the subsequent concentration step, and as a result, the concentration of the flavor component in the concentrate can be further improved.

Filtration of the liquid containing the tobacco component can be performed using, for example, a filter medium such as a filter cloth or a membrane filter. The opening of the filter medium is not particularly limited, but may be, for example, 0.1 μm to 800 μm when the purpose is mainly to remove fine powder of tobacco raw material and other suspended solids. Further, when the purpose is mainly to remove proteins, the opening of the filter medium can be, for example, 2 nm to 100 nm. Filtration may be performed using two or more types of filter media having different openings.

(Concentration process)
The method according to the present embodiment includes a step of concentrating a liquid containing a tobacco component by an interfacial forward freeze concentration method. As a general freeze-concentration method, a suspension crystallization method can be mentioned. The suspension crystallization method is a method of concentrating a solution by forming a large number of fine crystals of a solvent solidified product by cooling. However, since the device cost is high, the application is limited to large-scale continuous production, and the residence time is long, the method according to the present embodiment uses the interface forward freeze concentration method, which is one of the freeze concentration methods. Concentrate the liquid containing the tobacco component. The interfacial forward freeze concentration method is a method of concentrating a solution by forming crystals of a single large solvent solidified product by cooling. In this method, the device used is simple and versatile, and the cost can be reduced. Further, in the suspension crystallization method, the viscosity of the solution to be concentrated is up to about 200 cP, but in the interface forward freeze concentration method, sufficient concentration can be performed even if the viscosity is 200 cP or more.

FIG. 1 shows an example of a freeze-concentrator that can be used in the interface-advanced freeze-concentration method in the present embodiment. The freeze-concentrator 1 shown in FIG. 1 is provided with a stirring blade 4 inside, and the refrigerant 2 circulates on the outer periphery thereof. By introducing the liquid 3 containing the tobacco component into the freeze-concentrator 1 and setting the refrigerant 2 to a predetermined temperature while stirring with the stirring blade 4, the liquid 3 containing the tobacco component can be cooled to a predetermined temperature. .. When a predetermined time has elapsed from the start of cooling, a layer of the solidified solvent 5 is formed on the inner surface of the freeze-concentrator 1, so that the liquid 3 containing the tobacco component can be concentrated. In the freeze-concentrator 1, the inflow of the flavor component into the solidified solvent 5 can be suppressed by cooling the liquid 3 containing the tobacco component while stirring. Further, by controlling the temperature of the refrigerant 2 and controlling the temperature of the liquid 3 containing the tobacco component to a predetermined temperature, freeze concentration can be performed in a short time. The freeze-concentrator that can be used in this embodiment is not limited to the batch-type freeze-concentrator 1 shown in FIG. 1, and may be, for example, a distribution-type freeze-concentrator.

The set temperature of the refrigerant 2 depends on the type of the solvent contained in the liquid 3 containing the tobacco component, but when the solvent is water, for example, it is preferably −15 to 0 ° C., preferably -10.0 to -3. More preferably, it is at 0.0 ° C. At the set temperature, the temperature of the liquid 3 containing the tobacco component is in the range of −3.0 to 0 ° C. When the temperature is within the above range, the inflow of the flavor component into the solidified solvent 5 (ice) can be further suppressed, and the concentration operation can be performed in a short time.

The stirring speed by the stirring blade 4 is preferably 70 to 250 rpm, more preferably 100 to 180 rpm. When the stirring speed is within the above range, the inflow of the flavor component into the solidified solvent 5 can be further suppressed.

When freeze-concentrating is performed using a batch-type freeze-concentrator as shown in FIG. 1, the freeze-concentrate operation may be performed a plurality of times. For example, the liquid 3 containing the tobacco component is introduced into the freeze-concentrator 1 shown in FIG. 1, cooled, and after a predetermined time has elapsed, the liquid 3 containing the concentrated tobacco component is taken out and the freeze-concentrator 1 is used. The solidified solvent 5 formed on the inner surface is recovered. Then, the liquid 3 containing the concentrated tobacco component is introduced into the freeze-concentrator 1 again, cooled, and the concentration operation is performed again. The operation may be repeated twice or more, or may be repeated three or more times. By repeating this operation, the concentration rate ((mass of the liquid containing the tobacco component after concentration / mass of the liquid containing the tobacco component before concentration) * 100)) can be sufficiently increased. The concentration rate in this concentration step can be appropriately set according to a desired purpose, but can be, for example, 5 to 20%, preferably 7 to 15%.

In particular, in the method according to the present embodiment, the flavor component is sufficiently retained in the tobacco component concentrate even if the concentration step is carried out. Specifically, when the tobacco component concentrate obtained by the method according to the present embodiment is headspace-analyzed, the sum of all peaks is obtained in a chromatogram obtained by gas chromatography with a mass spectrometer (GC / MS). The ratio of the total area of the peaks of the compound group of RI2000 or less (the ratio of the compound group having 20 or less carbon atoms) to the area is preferably 70% or more, more preferably 80% or more, and 90% or more. Is more preferable, and 95% or more is particularly preferable. The upper limit of the range of the ratio is not particularly limited, but can be, for example, 99.9% or less. Further, in the chromatogram, the ratio of the total area of the peaks of the compound group of RI1000 to 2000 (the ratio of the compound group having 10 to 20 carbon atoms) is preferably 55% or more, and preferably 65% or more. More preferably, it is more preferably 70% or more. The upper limit of the range of the ratio is not particularly limited, but can be, for example, 90% or less. Further, in the chromatogram, the ratio of the total area of the peaks of the compound group of RI1000 or less (the ratio of the compound group having 10 or less carbon atoms) is preferably 20% or more, more preferably 25% or more. .. The upper limit of the range of the ratio is not particularly limited, but can be, for example, 50% or less. The analysis conditions of gas chromatography with mass spectrometer (GC / MS) are as follows.

<Analysis conditions>
・ Gas chromatography with mass spectrometer (GC / MS)
Equipment: Agilent Technologies 7890B / 5977B GC / MSD
-GC condition column: HP-5MS UI (manufactured by Agilent Technologies)
Inner diameter 0.25 mm x length 30 m, film thickness 0.25 μm
Injection volume: 1 μl
Injection mode: split (10: 1)
Injection port temperature: 270 ° C
Septam purge flow rate: 5 ml / min Carrier gas: Helium (He)
Column flow rate: 1 ml / min (constant flow rate mode)
Oven temperature: 40 ° C (3 minutes) -4 ° C / min-280 ° C (20 minutes)
Transfer line temperature: 280 ° C
-MS conditions Solvent waiting time: 4 minutes Ionization method: Electron impact ionization method (EI method), 70 eV
Ion source temperature: 230 ° C
Quadrupole temperature: 150 ° C
Measurement mode: Scan MS scan range: m / z 26-450
Threshold: 50
Sampling rate: 2

The peak of the compound group of RI2000 or less in the chromatogram mainly corresponds to the flavor component, and when the ratio is within the above range, the tobacco component concentrate contains a sufficient amount of the flavor component. Note that RI indicates a retention index, and is specifically calculated by the method described later.

[Tobacco component concentrate]
The tobacco component concentrate according to the present embodiment is produced by the method for producing a tobacco component concentrate according to the present embodiment. Since the tobacco component concentrate is produced by the method according to the present embodiment, it can have a high content of flavor components and a low solvent concentration (high concentration rate).

For example, when the raw material for tobacco is yellow sulcatone, as described above, regarding the content of flavor components, in the chromatogram obtained by analysis by the above-mentioned analysis method, the compound group of RI1000 or less with respect to the total area of the entire peak. The ratio of the total area of the peaks (the ratio of the total area of the peaks of the compound group having 10 or less carbon atoms) is preferably 20% or more, and in this case, the tobacco component concentrate is, for example, 6-METHYL-5. It contains a lot of compounds such as HEPTEN-2-ONE. Further, the ratio of the total area of the peaks of the compound group having RI2000 or less (the ratio of the total area of the peaks of the compound group having 20 or less carbon atoms) is preferably 70% or more. When the content of the compound group of RI2000 or less (the compound group having 20 or less carbon atoms) is high, the amount and balance of the flavor component are good.

Regarding the solvent concentration, for example, when the solvent is water, the content ratio of water in the tobacco component concentrate is preferably 20 to 90% by mass, more preferably 40 to 80% by mass. The water content is a value measured by Karl Fischer titration.

[Manufacturing method of flavor-producing articles]
The method for producing a flavor-producing article according to the present embodiment includes a step of producing a tobacco component concentrate by the method according to the present embodiment (hereinafter referred to as a tobacco component concentrate manufacturing step) and a tobacco component concentrate as a base material. A step of producing a tobacco component-containing base material (hereinafter referred to as a tobacco component-containing base material manufacturing step) and a step of manufacturing a flavor-producing article containing the tobacco component-containing base material (hereinafter referred to as flavor). It is referred to as a product manufacturing process) and. In the method according to the present embodiment, the tobacco component concentrate is produced by the method according to the present embodiment, and the flavor-producing article is produced using the tobacco component concentrate. Therefore, flavor generation containing a predetermined amount of the flavor component is produced at low cost. Goods can be manufactured. The method according to the present embodiment is not particularly limited as long as it includes a tobacco component concentrate manufacturing step, a tobacco component-containing base material manufacturing step, and a flavor-producing article manufacturing step, and may further include steps other than these steps. ..

(Tobacco component-containing base material manufacturing process)
The method according to the present embodiment includes a step of applying the tobacco component concentrate produced by the method according to the present embodiment to a substrate and drying to produce a tobacco component-containing substrate. The base material is not particularly limited, and examples thereof include residues, pulp, and the like after extracting the tobacco component in the tobacco raw material with a solvent in the tobacco component extract manufacturing step. The tobacco component concentrate can be applied to the substrate by, for example, coating. The drying conditions after the tobacco component concentrate is applied to the substrate are not particularly limited. For example, in the case of hot air drying, the product can be dried at 35 to 100 ° C. until the finished water content reaches a desired value. It is also possible to remove water using far infrared rays, mid infrared rays, and near infrared rays. Drying using infrared rays can suppress vaporization and denaturation due to heat, and can retain tobacco components predominantly, as compared with hot air drying. Further, drying using infrared rays has an advantage that the components can be selectively vaporized.

When the flavor-producing article is a non-combustion heating type flavor suction device, an aerosol-generating base material that generates aerosol smoke by heating may be further applied to the base material. The type of the aerosol-forming substrate is not particularly limited, and extracts from various natural products and / or their constituents can be selected depending on the intended use. Specific examples of the aerosol-forming substrate include, but are limited to, polyhydric alcohols such as glycerin, propylene glycol, sorbitol, xylitol, and erythritol, triacetin, 1,3-butanediol, and mixtures thereof. Not done. In addition to the tobacco component concentrate and the aerosol-producing base material, fragrances and the like may be further added to the base material.

(Flavor-producing article manufacturing process)
The method according to the present embodiment includes a step of producing a flavor-producing article containing a tobacco component-containing base material produced by the above method. As the flavor producing article, for example, a combustion type flavor suction device, a non-combustion heating type flavor suction device, or the like can be used as described later. The tobacco component-containing substrate can be contained, for example, in the tobacco-containing segment of the device. The flavor-producing article can be produced by a known method.

[Flavor-producing goods]
The flavor-producing article according to the present embodiment is manufactured by the method for producing a flavor-producing article according to the present embodiment. Since the flavor-producing article is produced by the method for producing a flavor-producing article according to the present embodiment, a desired amount of flavor component can be contained and the cost is low. Examples of the flavor producing article include a combustion type flavor suction device, a non-combustion heating type flavor suction device, and the like.

(Combustion type flavor suction device)
FIG. 2 shows an example of the combustion type flavor suction device according to the present embodiment. As shown in FIG. 2, the combustion type flavor suction device 6 includes a tobacco-containing segment 7 and a filter segment 8 provided adjacent to the tobacco-containing segment 7. The tobacco-containing segment 7 includes a tobacco filling 9 containing a tobacco component-containing base material to which the tobacco component concentrate according to the present embodiment is applied, and a rolling paper 10 wrapped around the tobacco filling 9. The filter segment 8 is not particularly limited as long as it has a function as a general filter. For example, a tow made of synthetic fibers (also simply referred to as “tow”) or a material such as paper is processed into a columnar shape. Things can be used. The tobacco-containing segment 7 and the filter segment 8 are connected by a chip paper member 11 wound on the tobacco-containing segment 7 and the filter segment 8. The chip paper member 11 may have a vent hole in a part of the outer periphery thereof. The number of ventilation holes may be one or a plurality, and for example, 10 to 40 ventilation holes may be formed. When the number of ventilation holes is plurality, the ventilation holes can be arranged in an annular shape in a line on the outer peripheral portion of the chip paper member 11, for example. The plurality of ventilation holes can be arranged at substantially constant intervals. By providing the ventilation holes, air is taken into the filter segment 8 from the ventilation holes at the time of suction. By diluting the mainstream smoke with the outside air from the ventilation holes, it is possible to design a product with a desired tar value.

The user can enjoy the flavor of tobacco by igniting the tip of the tobacco-containing segment 7 and sucking the mouthpiece of the filter segment 8 in the mouth. The number of filter segments 8 is not limited to one, and for example, a plurality of filter segments having different functions may be connected and arranged.

(Non-combustion heating type flavor suction device)
The non-combustion heating type flavor suction device according to the present embodiment can include, for example, a tobacco-containing segment, a tubular cooling segment having perforations on the periphery, a center hole segment, and a filter segment. The non-combustion heating type flavor suction device according to the present embodiment may have other segments other than the tobacco-containing segment, the cooling segment, the center hole segment and the filter segment.

The axial length of the non-combustion heating type flavor suction device according to the present embodiment is not particularly limited, but is preferably 40 mm or more and 90 mm or less, more preferably 50 mm or more and 75 mm or less, and more preferably 50 mm or more. It is more preferably 60 mm or less. Further, the peripheral length of the non-combustion heating type flavor suction device is preferably 16 mm or more and 25 mm or less, more preferably 20 mm or more and 24 mm or less, and further preferably 21 mm or more and 23 mm or less. For example, the length of the tobacco-containing segment is 20 mm, the length of the cooling segment is 20 mm, the length of the center hole segment is 8 mm, and the length of the filter segment is 7 mm. The length of the filter segment can be selected within the range of 4 mm or more and 10 mm or less. The ventilation resistance of the filter segment at that time is selected so as to be 15 mmH ₂ O / seg or more and 60 mmH ₂ O / seg or less per segment. The lengths of these individual segments can be appropriately changed according to manufacturing aptitude, required quality, and the like. Furthermore, even if only the filter segment is arranged on the downstream side of the cooling segment without using the center hole segment, it can function as a non-combustion heating type flavor suction device.

<Tobacco-containing segment>
The tobacco-containing segment can include a tobacco filling containing a tobacco component-containing substrate to which the tobacco component concentrate according to the present embodiment is applied, and a rolling paper wrapped around the tobacco filling. The method of filling the tobacco filling in the wrapping paper (hereinafter, also referred to as a wrapper) is not particularly limited, but for example, the tobacco filling may be wrapped in a wrapper, or the tubular wrapper may be filled with the tobacco filling. When the shape of the tobacco component-containing substrate has a longitudinal direction such as a rectangular shape, the tobacco component-containing substrate may be filled so that the longitudinal direction is an unspecified direction in the wrapper, and the tobacco-containing substrate may be contained. The segments may be aligned and filled in the axial direction or in a direction perpendicular to the axial direction. When the tobacco-containing segment is heated, the tobacco component (flavor component), aerosol-forming base material and water contained in the tobacco filling are vaporized, and these are transferred to the mouthpiece segment by suction.

<Cooling segment>
The cooling segment may be configured by a tubular member. The tubular member may be, for example, a paper tube obtained by processing thick paper into a cylindrical shape.

The total surface area of the cooling segment can be 300 mm ² / mm or more and 1000 mm ² / mm or less. This surface area is the surface area per length (mm) in the cooling segment ventilation direction. The total surface area of the cooling segment is preferably 400 mm ² / mm or more, more preferably 450 mm ² / mm or more, while preferably 600 mm ² / mm or less, preferably 550 mm ² / mm or less. Is more preferable.

It is desirable that the cooling segment has a large total surface area with a large internal structure. Thus, in a preferred embodiment, the cooling segment may be wrinkled to form a channel and then formed by a sheet of pleated, gathered, and folded thin material. Folding or folds within a given volume of the element increases the total surface area of the cooling segment.

In some embodiments, the thickness of the constituent material of the cooling segment can be 5 μm or more and 500 μm or less, for example, 10 μm or more and 250 μm or less.

The aerosol cooling element can be formed from a material having a specific surface area of 10 mm ² / mg or more and 100 mm ² / mg or less. In one embodiment, the specific surface area of the constituent material can be about 35 mm ² / mg. The specific surface area can be determined in consideration of materials having a known width and thickness. For example, the material can be polylactic acid with an average thickness of 50 μm and a variation of ± 2 μm. If the material also has a known width, for example between 200 mm and above, 250 mm and below, the specific surface area and density can be calculated.

The tubular member and the mouthpiece lining paper, which will be described later, are provided with perforations that penetrate both of them. The presence of perforations introduces outside air into the cooling segment during suction. As a result, the aerosol vaporization component generated by heating the tobacco-containing segment comes into contact with the outside air, and the temperature drops, so that the aerosol is liquefied to form an aerosol. The diameter of the perforation (delivery length) is not particularly limited, but may be, for example, 0.5 mm or more and 1.5 mm or less. The number of perforations is not particularly limited and may be one or two or more. For example, a plurality of perforations may be provided on the circumference of the cooling segment.

The amount of outside air introduced from the drilling is preferably 85% by volume or less, more preferably 80% by volume or less, based on the total volume of the gas sucked by the user. When the ratio of the amount of outside air is 85% by volume or less, the reduction of flavor due to dilution by the outside air can be sufficiently suppressed. In other words, this is also called the ventilation ratio. From the viewpoint of cooling performance, the lower limit of the ventilation ratio range is preferably 55% by volume or more, more preferably 60% by volume or more.

The resistance that the cooling segment gives to the air passing through the tobacco-containing segment is preferably small. Preferably, the cooling segment has substantially no effect on the suction resistance of the non-combustion heated flavor suction device. Resistance to suction (RTD) is the pressure required to push air through the entire length of an object under a flow rate test of 17.5 ml / sec at 22 ° C. and 101 kPa (760 tolls). RTD is generally expressed in _mmH2O units and is measured according to ISO 6565: 2011. Therefore, it is preferable that the amount of pressure drop from the upstream end of the cooling segment to the downstream end of the cooling segment is small. To achieve this, it is preferred that the vertical porosity is greater than 50% and the airflow path through the cooling segment is relatively unconstrained. The longitudinal porosity of the cooling segment can be determined by the ratio of the cross-sectional area of the material forming the cooling segment to the internal cross-sectional area of the cooling segment.

In some embodiments, the resulting aerosol may drop by 10 ° C or more as it is sucked into the user through the cooling segment. In another aspect, the temperature may drop by 15 ° C. or higher, and in yet another aspect, the temperature may drop by 20 ° C. or higher.

The cooling segment may be composed of a sheet material selected from the group comprising metal foil, polymer sheets, and substantially non-perforated paper or thick paper. In one embodiment, the cooling segment can include a sheet material selected from the group consisting of polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate, polylactic acid, cellulose acetate, and aluminum foil. The constituent material of the cooling segment may be made from a biodegradable material, such as non-perforated paper, a biodegradable polymer such as polylactic acid, or a starch-based copolymer.

It is preferable that the air flow passing through the cooling segment does not substantially deviate between adjacent segments. In other words, the airflow through the cooling segment is preferably along the longitudinal segment with virtually no radial deviation. In some embodiments, the cooling segment is formed from a material with low porosity or substantially no pores, except for longitudinal extending channels. Materials used to define or form longitudinal extending channels, such as wrinkled or gathered sheets, have low porosity or virtually no pores.

As mentioned above, the cooling segment may include a sheet of suitable constituent material wrinkled, pleated, gathered or folded. The cross-sectional profile of such an element may indicate a randomly oriented channel. The cooling segment can be formed by other means. For example, the cooling segment can be formed from a bundle of longitudinally extending tubes. Cooling segments can be formed by extrusion, molding, laminating, injection, or shredding of suitable materials.

The cooling segment can be formed, for example, by wrapping, gathering, or folding a sheet material with rolling paper. In some embodiments, the cooling segment can include a sheet of wrinkled material gathered in a rod shape and tied with a wrapper, for example, a roll of filter paper.

The cooling segment can be formed into a rod shape having an axial length of, for example, 7 mm or more and 28 mm or less. For example, the axial length of the cooling segment can be 18 mm.

In some embodiments, the cooling segment is substantially circular in its axial cross-sectional shape and can have a diameter of 5 mm or more and 10 mm or less. For example, the diameter of the cooling segment can be about 7 mm.

<Center hall segment>
The center hole segment is composed of a packed bed having one or more hollow portions and an inner plug wrapper (inner rolling paper) covering the packed bed. For example, the center hole segment is composed of a second packed bed having a hollow portion and a second inner plug wrapper covering the second packed bed. The center hole segment has a function of increasing the strength of the mouthpiece segment. The second packed bed is, for example, filled with cellulose acetate fiber at a high density, and a plasticizer containing triacetin is added in an amount of 6% by mass or more and 20% by mass or less with respect to the mass of cellulose acetate to cure the inner diameter of φ1.0 mm or more. , The rod can be φ5.0 mm or less. Since the packed bed of the second packed bed has a high packed density of fibers, air and aerosol flow only in the hollow portion at the time of suction, and hardly flow in the second packed bed. Since the second packed bed inside the center hole segment is a fiber packed bed, the feeling of touch from the outside during use is less likely to cause discomfort to the user. It should be noted that the center hole segment may not have a second inner plug wrapper and its shape may be maintained by thermoforming.

<Filter segment>
The structure of the filter segment is not particularly limited, but may be composed of a single or a plurality of packed layers. The outside of the packed bed may be wrapped with one or more sheets of rolling paper. The aeration resistance per segment of the filter segment can be appropriately changed depending on the amount of the filler filled in the filter segment, the material and the like. For example, if the filler is cellulose acetate fibers, increasing the amount of cellulose acetate fibers filled in the filter segment can increase aeration resistance. When the filler is cellulose acetate fiber, the packing density of the cellulose acetate fiber can be 0.13 to 0.18 g / cm ³ . The ventilation resistance is a value measured by a ventilation resistance measuring device (trade name: SODIMAX, manufactured by SODIM).

The peripheral length of the filter segment is not particularly limited, but is preferably 16 to 25 mm, more preferably 20 to 24 mm, and even more preferably 21 to 23 mm. The axial length of the filter segment can be selected from 4 to 10 mm, and the ventilation resistance thereof is selected to be 15 to 60 mmH ₂ O / seg. The axial length of the filter segment is preferably 5 to 9 mm, more preferably 6 to 8 mm. The shape of the cross section of the filter segment is not particularly limited, but may be, for example, a circle, an ellipse, a polygon, or the like. In addition, destructive capsules containing fragrances, fragrance beads, and fragrances may be directly added to the filter segment.

The center hole segment and the filter segment can be connected with an outer plug wrapper (outer roll paper). The outer plug wrapper can be, for example, cylindrical paper. Further, the tobacco-containing segment, the cooling segment, and the connected center hole segment and filter segment can be connected by the mouthpiece lining paper. These connections can be made by, for example, applying glue such as vinyl acetate glue to the inner surface of the mouthpiece lining paper, inserting the above three segments, and winding them. In addition, these segments may be connected in a plurality of times by a plurality of lining papers.

(Non-combustion heating type flavor suction system)
The non-combustion heating type flavor suction system according to the present embodiment may include a non-combustion heating type flavor suction device according to the present embodiment and a heating device for heating the tobacco-containing segment of the non-combustion heating type flavor suction device. can. The non-combustion heating type flavor suction system according to the present embodiment may have other configurations other than the non-combustion heating type flavor suction device and the heating device according to the present embodiment.

FIG. 3 shows an example of the non-combustion heating type flavor suction system according to this embodiment. The non-combustion heating type flavor suction system shown in FIG. 3 includes a non-combustion heating type flavor suction device 12 according to the present embodiment, and a heating device 13 for heating the tobacco-containing segment of the non-combustion heating type flavor suction device 12 from the outside. To prepare for.

FIG. 3A shows a state before the non-combustion heating type flavor suction device 12 is inserted into the heating device 13, and FIG. 3B shows a state in which the non-combustion heating type flavor suction device 12 is inserted into the heating device 13 and heated. Indicates the state to be used. The heating device 13 shown in FIG. 3 includes a body 14, a heater 15, a metal tube 16, a battery unit 17, and a control unit 18. The body 14 has a cylindrical recess 19 at a position on the inner side surface of the recess 19 corresponding to the tobacco-containing segment of the non-combustion heating type flavor suction device 12 inserted into the recess 19, the heater 15 and the metal tube. 16 are arranged. The heater 15 can be a heater by electric resistance, and electric power is supplied from the battery unit 17 according to an instruction from the control unit 18 that controls the temperature, and the heater 15 is heated. The heat generated from the heater 15 is transferred to the tobacco-containing segment of the non-combustion heating type flavor suction device 12 through the metal tube 16 having high thermal conductivity.

In FIG. 3B, since it is schematically shown, there is a gap between the outer circumference of the non-combustion heating type flavor suction device 12 and the inner circumference of the metal tube 16, but in reality, heat is efficiently used. For the purpose of transmission, it is desirable that there is no gap between the outer circumference of the non-combustion heating type flavor suction device 12 and the inner circumference of the metal tube 16. The heating device 13 heats the tobacco-containing segment of the non-combustion heating type flavor suction device 12 from the outside, but may be heated from the inside.

The heating temperature by the heating device is not particularly limited, but is preferably 400 ° C. or lower, more preferably 150 ° C. or higher and 400 ° C. or lower, and further preferably 200 ° C. or higher and 350 ° C. or lower. The heating temperature indicates the temperature of the heater of the heating device.

Hereinafter, the present embodiment will be described in detail by way of examples, but the present embodiment is not limited to these examples. The component analysis of the tobacco component concentrate was performed by the following method.

[Component analysis of tobacco component concentrate]
Headspace analysis of the tobacco component concentrates obtained in each example and comparative example was performed. First, 5 mL of the tobacco component concentrate was heated at 60 ° C. for 1 hour to adsorb the volatile components on the adsorbent. As the adsorbent, Monotrap RCC 18 (trade name) manufactured by GL Sciences Co., Ltd. was used. Extraction was performed by adding 300 μL of a mixed solvent of hexane: acetone = 1: 1 (volume ratio) to the adsorbent. The obtained extract was analyzed by a gas chromatograph with a mass spectrometer (GC / MS). A 7890B manufactured by Agilent was used for the gas chromatograph, a 5977B MSD (trade name) was used for the detector, and an HP-5 ms UI (30 m × 250 μm × 0.25 μm) was used for the column. The carrier gas of the gas chromatograph was helium gas, and the flow rate was 1.0 mL per minute. As the heating conditions, the temperature was raised from 40 ° C. to 280 ° C. at 4 ° C. per minute and maintained at 280 ° C. for 20 minutes.

The chromatogram retention index (RI) obtained by the above analysis was calculated by the following method. The retention index (RI) used was a value calculated using an n-alkane mixture in the range of n-hexane (C6, RI: 600) to n-pentatricontane (C35, RI: 3500) by the linear method. .. The n-alkane mixture used in calculating the retention index (RI) is not limited to this. RI: 0 to 1000 is a group of compounds having 10 or less carbon atoms, RI: 1000 to 1500 is a group of compounds having 10 to 15 carbon atoms, RI: 1500 to 2000 is a group of compounds having 15 to 20 carbon atoms, RI: 2000 to 2500 is a group of compounds having 15 to 20 carbon atoms. Each corresponds to a group of compounds having 20 to 25 carbon atoms.

[Example 1]
(Tobacco component extract manufacturing process)
Tobacco leaf (yellow seed) and water were mixed at a ratio of tobacco leaf: water = 1:10 (mass ratio) and stirred at 50 ° C. for 2 hours to obtain a tobacco component extract.

(Filtration process)
The tobacco component extract was filtered using a filter cloth (nylon dumpling bag, opening: 0.45 mm) to remove fine particles in the tobacco component extract.

(Concentration process)
The tobacco component extract after the filtration step was concentrated by an interface forward freeze concentration method using a stirring type freeze concentration device (trade name: PFC-M10, manufactured by Meiwa Kogyo Co., Ltd.). Specifically, 10 kg of the tobacco component extract was placed in a 12 L container and concentrated to 7.145 kg under the condition of a brine temperature of -17 ° C while stirring at 120 rpm to obtain a first concentrated solution (concentration rate 71. 45%). At the same time, 2.855 kg of the first ice was collected as an ice portion. Then, 7.145 kg of the first concentrated solution was placed in an 8 L container and concentrated to 3.765 kg under the condition of a brine temperature of -17 ° C. while stirring at 120 rpm to obtain a second concentrated solution (concentration rate 37.65). %). At the same time, 3.38 kg of ice was collected for the second time as an ice portion. Further, 3.765 kg of the second concentrate was placed in a 6 L container and concentrated to 1.605 kg under the condition of a brine temperature of -17 ° C while stirring at 150 rpm to obtain a third concentrate (tobacco component concentrate). (Concentration rate 16.05%). At the same time, 2.16 kg of ice was collected for the third time as an ice portion.

The obtained tobacco component concentrate was analyzed for components by the above method. The chromatogram obtained by component analysis is shown in FIG. Further, in the chromatogram, the total peak area in each RI range is shown in FIG. Table 1 shows the ratio of the total peak area in each RI range.

[Comparative Example 1]
(Tobacco component extract manufacturing process, filtration process)
A tobacco component extract was prepared in the same manner as in Example 1, and a filtration step was carried out.

(Concentration process)
The tobacco component extract after the filtration step was concentrated by the evaporation concentration method. Specifically, 200 g of the tobacco component extract was concentrated under reduced pressure to 32 g while being maintained at 40 ° C. under a reduced pressure of 40 mmHg using a rotary evaporator (manufactured by Nippon Buch). The evaporation temperature at that time was 34 ° C. As a result, a tobacco component concentrate (concentration rate 16%) was obtained.

The obtained tobacco component concentrate was analyzed for components by the above method. The chromatogram obtained by component analysis is shown in FIG. Further, in the chromatogram, the total peak area in each RI range is shown in FIG. Table 1 shows the ratio of the total peak area in each RI range.

As is clear from the chromatogram shown in FIG. 4, when Example 1 and Comparative Example 1 are compared, the component group (carbon number 20) in the range of 2000 or less in RI as compared with Comparative Example 1 in Example 1 It was found that the number of peaks of the following compound group) was large and the intensity of each peak was also large.

As shown in FIG. 5 and Table 1, it was found that, in particular, when RI was in the range of 1000 to 1500, the amount of components in Example 1 was about 3 times larger than that in Comparative Example 1. Examples of the component group within the range of RI include phenolic compounds characterized by various tobacco-specific aromas. Further, it was found that in the range of RI of 1500 to 2000, the amount of components in the range of Example 1 was about twice as large as that of Comparative Example 1. Examples of the component group within the range of RI include carotenoid decomposition products such as megastigma toluenone, which is one of the flavor components of tobacco.

From the above results, by concentrating by the freeze concentration method, the liquid can be sufficiently retained while retaining a larger amount of aroma components contained in the liquid containing the tobacco component such as the tobacco component extract than the conventional evaporation concentration method. It was confirmed that it can be concentrated in tobacco.

[Example 2, Comparative Example 2]
5 g of the tobacco component concentrate prepared in Example 1 and Comparative Example 1 was sprayed and aromatized on 50 g of tobacco base sheet. The obtained perfumed sheet engravings were dried at 35 ° C. for 1 hour in the open air to obtain perfumed sheet engravings. A non-combustion heating type flavor suction device containing the perfumed sheet engraving in the tobacco-containing segment was prepared, and the tobacco-containing segment of the device was heated and sucked from the outside to evaluate the flavor. The non-combustion heating type flavor suction device (Example 2) including the perfumed sheet engraving of Example 1 is more than the non-combustion heating type flavor suction device (Comparative Example 2) including the perfumed sheet engraving of Comparative Example 1. , The original aroma of tobacco was better expressed.

1 Freezing and concentrating device 2 Refrigerator 3 Liquid containing tobacco components 4 Stirring blades 5 Solidified solvent 6 Combustion type flavor suction device 7 Tobacco-containing segment 8 Filter segment 9 Tobacco filling 10 Rolling paper 11 Chip paper member 12 Non-combustion heating type flavor suction device 13 Heating device 14 Body 15 Heater 16 Metal tube 17 Battery unit 18 Control unit 19 Recess

Claims (9)

A method for producing a tobacco component concentrate, which comprises a step of concentrating a solution containing a tobacco component by an interface advance freeze concentration method. Before the step of concentrating the liquid containing the tobacco component by the interface advance freeze concentration method,
The method according to claim 1, further comprising a step of extracting a tobacco component in a tobacco raw material with a solvent and producing a liquid containing the tobacco component. The method according to claim 2, wherein the solvent contains water. Before the step of concentrating the liquid containing the tobacco component by the interface advance freeze concentration method,
The method according to any one of claims 1 to 3, further comprising the step of filtering the liquid containing the tobacco component to remove the solid matter. In the chromatogram obtained by gas chromatography with mass spectrometer (GC / MS) when the tobacco component concentrate was headspaced, the total area of the peaks of the compound group of RI2000 or less with respect to the total area of the entire peak. The method according to any one of claims 1 to 4, wherein the proportion of the gas is 70% or more. Tobacco component concentrate produced by the method according to any one of claims 1 to 5. A step of producing a tobacco component concentrate by the method according to any one of claims 1 to 5.
A step of applying the tobacco component concentrate to a base material and drying it to produce a tobacco component-containing base material.
The process of manufacturing a flavor-producing article containing the tobacco component-containing base material, and
A method for producing a flavor-producing article, including. A flavor-producing article produced by the method according to claim 7. The flavor-producing article according to claim 8, which is a combustion-type flavor suction device or a non-combustion heating-type flavor suction device.

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