Manufacturing method of tobacco material

Abstract

Provided is a method for producing a tobacco material, the method comprising impregnating a tobacco raw material with a medium having a state selected from the group consisting of gas, liquid and supercritical states, and obtaining a tobacco material having a surface transition rate X of more than 1 as defined below, wherein: the surface transition rate is X＝S / P, where S is the peak area due to GC of a flavor component present on the surface of the tobacco raw material after impregnation, and P is the peak area due to GC of a flavor component present on the surface of the tobacco raw material before impregnation; the tobacco raw material is leaf tobacco, lamina, a center bone, remaining stems, or a core, which is harmonized or disharmonized; and the harmonized raw material has a water content of 5-40 wt%.

Description

[Technical Field]

[0001] The present invention relates to a method for producing tobacco material. [Background technology]

[0002] Research into the aroma components of tobacco leaves has been conducted on a wide variety of tobacco raw materials, including flue-cured, burley, Oriental, and Maryland tobacco, and the characteristic components of each raw material have been reported. To date, over 4,000 components have been reported (Non-Patent Document 1). The components that contribute to the characteristic tobacco leaf aroma can be broadly divided into two groups based on their localization inside or outside tobacco leaf cells. The first group includes components present in the cellular tissue of tobacco leaves. These are aroma compounds primarily composed of pigment-derived decomposition products produced during the maturation or curing process of tobacco leaves, namely, pigment decomposition products such as ionone, megastigmatotrienone, and phytol, as well as monoterpenes and phenols. All of these compounds accumulate inside the cellular tissue of tobacco leaves via metabolic pathways involved in the production of general aroma components, such as the pigment degradation pathway, mevalonate pathway, and shikimic acid pathway.

[0003] The second is the components present on the surface of tobacco leaves. This is commonly called leaf resin, and is composed of relatively high molecular weight organic acids, hydrocarbons, glycosides, and other compounds produced and secreted by hairs and other organelles to protect the tissue from pests and diseases and the growing environment. Its aroma components are characterized by sesquiterpenes, diterpenes, and the terpene glycosides that surround them.

[0004] Various methods for extracting aroma components from tobacco leaves and the like have been proposed. Extraction methods using liquefied carbon dioxide or supercritical carbon dioxide have been proposed, taking advantage of the characteristics of the target components (e.g., Patent Documents 1 and 2). Materials obtained by expanding tobacco leaves with liquefied carbon dioxide have been considered as one of the raw materials for combustion tobacco, but this process is very similar to the extraction process using carbon dioxide described above. Therefore, methods that apply part of this expansion process have been proposed (e.g., Patent Documents 3 and 4). Patent Document 3 discloses an apparatus for producing flavors for expanded tobacco raw materials. The apparatus includes an extraction vessel that contacts the tobacco raw material with supercritical carbon dioxide to dissolve the tobacco components in the carbon dioxide; a separation vessel connected to the extraction vessel that separates and recovers the fat-soluble portions of the tobacco components from the tobacco components dissolved in the carbon dioxide; a circulation path that circulates the supercritical carbon dioxide between the extraction vessel and an absorption vessel containing pure water while purifying it with an activated carbon purification layer, allowing the pure water to absorb the water-soluble portions of the tobacco components; and a recovery vessel that recovers the pure water that has absorbed the water-soluble portions of the tobacco components from the absorption vessel as absorbed water. The fat-soluble portion of the tobacco components and absorbed water are used to produce flavors. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] International Publication No. 2007 / 029264 [Patent Document 2] British Patent No. 2173985 [Patent Document 3] International Publication No. 2007 / 119790 [Non-patent literature]

[0006] [Non-Patent Document 1] Leffingwell et. Al., Leffingwell Reports, Vol.1 (No. 2), February, 2001 [Non-patent document 2] Discoloration and strength deterioration of plant fibers due to thermal degradation, Sen'i Gakkaishi Journal, pp89-95, vol70, no5 (2014) [Non-patent document 3] J.Sui, et.al., Formation of α- and β-Cembranoid Synthetic Genes, Molecules. 23(10): 2511, 2018 [Non-patent document 4] WSSchlotzhauer, et al., Characterization of thermolysis products of cuticular wax compounds of green tobacco leaf, Journal of Analytical and Applied Pyrolysis. Volume 17, Issue 1, December 1989, Pages 25-35 Summary of the Invention [Problem to be solved by the invention]

[0007] In the case of combustible tobacco, the aroma components are distilled and pyrolyzed during the combustion and decomposition of the cellular components. In other words, even if the aroma components of leaf tobacco are localized inside or on the surface of the tobacco leaf cells as described above, they are likely to be transferred to mainstream smoke, and the impact of localization is thought to be very small.

[0008] On the other hand, in non-combustible tobacco, compared to conventional combustible tobacco, intracellular movement is restricted by structures such as cell walls, resulting in the volatilization of surface-localized components, primarily leaf resins. Therefore, in non-combustible tobacco, heating temperature is crucial for releasing aroma compounds present inside cells. It is believed necessary to heat to above 200°C, the thermal denaturation temperature of cell wall components (Non-Patent Document 2). For example, ionones (Non-Patent Document 1), which are decomposition products of carotenes contained in plastids, are present intracellularly, and their release is inhibited at low temperatures. However, at the thermal denaturation temperature, they rapidly volatilize along with the thermal denaturation of cell wall components, making their delivery difficult to control. In contrast, cembratrienediol (CBT), a leaf resin component (Non-Patent Document 3), has a low vapor pressure, and therefore is expected to be delivered in proportion to the amount of heat applied, compared to the aroma compounds present within the cells. In other words, in non-combustible tobacco, the release of aroma compounds is restricted depending on the location of the compounds, making it difficult to release aroma compounds as easily as in combustible tobacco. In view of the above circumstances, an object of the present invention is to provide a tobacco material from which aroma components are easily released. [Means for solving the problem]

[0009] The inventors have focused on the fact that during the expansion process of tobacco leaves, aroma components present within tobacco leaf cells migrate from within the cells to outside the cells when the carbon dioxide is vaporized and removed after the impregnation with gaseous carbon dioxide, and that these aroma components may mix with non-volatile substances such as leaf surface resins that are already present outside the cells at the cell surface, thereby dissolving or retaining the intracellular aroma components, and have completed the present invention. That is, the above-mentioned problems are solved by the present invention as follows. Aspect 1 Impregnating a tobacco material with a medium in a state selected from the group consisting of a gas, a liquid, and a supercritical state; obtaining a tobacco material having a surface migration rate X greater than 1, as defined below; Surface migration rate X=S / P S: Peak area of ​​flavor components present on the surface of the tobacco material after impregnation, measured by GC P: Peak area by GC of flavor components present on the surface of the tobacco material before impregnation The tobacco raw material is blended or unblended tobacco leaves, lamina, midrib, stem residue, or shreds; The moisture content of the blended raw materials is 5 to 40% by weight. Method for producing tobacco material. Aspect 2 2. The method of claim 1, wherein the tobacco material is a conditioned material, and the conditioned material comprises storing the material at 22°C and 60% humidity for at least 24 hours. Aspect 3 3. The method according to claim 2, wherein the storage time is 30 hours or less. Aspect 4 A manufacturing method according to any one of aspects 1 to 3, wherein the impregnation comprises permeating the medium into the entire tobacco material. Aspect 5 A method according to any one of Aspects 1 to 4, wherein the solvent used for the impregnation is liquid carbon dioxide. Aspect 6 A manufacturing method according to aspect 5, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 2 MPa or more. Aspect 7 7. The method of claim 6, wherein the pressure is 3 MPa or more. Aspect 8 8. The method of claim 7, wherein the pressure is 5 MPa or more. Aspect 9 A method according to any one of aspects 5 to 8, wherein the pressure is less than 100 MPa. Aspect 10 A method for producing a tobacco material according to any one of aspects 5 to 9, wherein the temperature of the atmosphere surrounding the tobacco raw material during the impregnation is -10 to 35°C. Aspect 11 A method for producing a tobacco material according to any one of aspects 1 to 4, wherein the medium used for the impregnation is supercritical carbon dioxide. Aspect 12 A method for producing a tobacco material according to aspect 11, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 100 MPa or more. Aspect 13 A method for producing a tobacco material according to aspects 11 and 12, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 200 MPa or higher. Aspect 14 Aspects 14. The method for producing a tobacco material according to any one of aspects 11 to 13, wherein the atmospheric pressure around the tobacco raw material during the impregnation is 300 MPa or less. Aspect 15 A method for producing a tobacco material according to any one of aspects 11 to 14, wherein the temperature of the atmosphere surrounding the tobacco raw material during the impregnation is greater than 35°C and equal to or less than 70°C. Aspect 16 Aspect 16. The manufacturing method according to any one of aspects 1 to 15, further comprising a step of wet-pulverizing the tobacco material after the impregnation. Aspect 17 A tobacco material obtained by the method according to any one of aspects 1 to 16. Aspect 18 Aspect 18. The tobacco material according to aspect 17, wherein the tobacco material is in a form selected from the group consisting of tobacco sheets, shredded tobacco, shredded midribs, and combinations thereof. Aspect 19 Aspect 19. The tobacco material according to aspect 18, wherein the tobacco shreds or midrib shreds have a width of 0.5 to 2.0 mm and a length of 3 to 10 mm. Aspect 20 20. The tobacco material according to any one of aspects 17 to 19, wherein the tobacco material comprises 5 to 50 wt % of the aerosol-forming base material, based on the total weight of the tobacco material. [Effects of the Invention]

[0010] The present invention can provide a tobacco material that is easy to release aroma components from. [Brief explanation of the drawings]

[0011] [Figure 1] FIG. 1 shows an embodiment of a non-combustion heating tobacco flavor inhalation article. [Figure 2] FIG. 1 shows an embodiment of a non-combustion heating tobacco flavor inhalation system. [Figure 3] Gas chromatogram DETAILED DESCRIPTION OF THE INVENTION

[0012] The present invention will be described in detail below. In the present invention, "X to Y" includes the extreme values ​​X and Y. 1. Manufacturing method The manufacturing method of the present invention includes a step of impregnating a tobacco raw material with a medium in a state selected from the group consisting of a gas, a liquid, and a supercritical state, and includes a step of obtaining a material having a surface migration ratio X, as defined below, of greater than 1. Surface migration rate X=S / P S: Peak area of ​​aroma components present on the surface of the tobacco material after impregnation, measured by GC P: Peak area by GC of aroma components present on the surface of tobacco material before impregnation

[0013] (1) Medium The medium is not limited as long as it can extract aroma components from the tobacco raw material, and carbon dioxide, water, or an organic solvent can be used. Examples of organic solvents include aprotic solvents such as pentane, hexane, benzene, diethyl ether, and ethyl acetate. Of these, carbon dioxide is preferably used as the medium from the viewpoint of being able to utilize the expansion treatment of tobacco leaves.

[0014] These media may be in a gaseous, liquid, or supercritical state, but are preferably in a liquid or supercritical state from the viewpoint of ease of handling. In particular, from the viewpoint of being able to utilize the tobacco leaf expansion treatment as described above, it is preferable to use carbon dioxide in a liquid or supercritical state as the media.

[0015] (2) Tobacco raw materials The tobacco raw material is not limited as long as it is derived from a Nicotiana plant, but tobacco leaves, lamina, midrib, stem residue, or shreds are preferred from the standpoint of availability and other factors. Tobacco leaves are a collective term for harvested tobacco leaves before they undergo aging. One form of aging includes curing. Lamina are tobacco leaves that have been deboned, and the removed part is the midrib. Stem residue is the stem that remains in the field after tobacco harvest. Shreds are aged tobacco leaves or midrib, etc., that have been shredded to a specified size. In particular, midrib shreds to a specified size are also called midrib shreds. These may be subjected to a harmonizing process. Harmonizing refers to adjusting the condition to maintain a constant moisture content. For example, harmonizing can be performed by storing lamina at 22°C and 60% humidity for 24 hours or more. There is no upper limit to the storage time, but a storage time of 30 hours or less is preferred. If the raw material has a high moisture content, the raw material swells, making it easier for the medium to diffuse into the cells and for aroma components present inside the cells to migrate to the outside. On the other hand, if the moisture content of the raw material is high, it will be necessary to dry it after treatment. From these points of view, the moisture content of the raw material after conditioning is preferably 5 to 40 wt %, more preferably 10 to 30 wt %.

[0016] (3) Impregnation process Impregnation refers to the process of permeating the medium into the tobacco material. While it is sufficient for the medium to permeate at least a portion of the tobacco material, it is preferable for the medium to permeate the entire tobacco material. The pressure and temperature during impregnation are adjusted to bring the medium into the desired state. For example, when liquid carbon dioxide is used, the atmospheric pressure of the tobacco material (e.g., the pressure inside the container) is preferably 2 MPa or more, more preferably 3 MPa or more, and even more preferably 5 MPa or more (all gauge pressures). The upper limit of the pressure is not limited, but can be, for example, less than 100 MPa. The temperature at this time can be -10 to 35°C. Furthermore, when supercritical carbon dioxide is used, the pressure is preferably 100 MPa or more, more preferably 200 MPa or more (all gauge pressures). The upper limit of the pressure is not limited, but can be, for example, 300 MPa or less. The atmospheric temperature of the tobacco material at this time (e.g., the product temperature or the temperature inside the container) can be greater than 35°C and up to 70°C.

[0017] The impregnation process causes aroma components present inside the cells of the tobacco raw material to migrate outside the cells and further to the surface of the tobacco raw material. While the reason for this is not limited, it is believed that contact between the medium impregnated within the tobacco raw material and the cells creates a concentration gradient of aroma components inside and outside the cells, causing the aroma components present inside the tobacco raw material to migrate toward the medium. Furthermore, when carbon dioxide is used, in addition to the above, the impregnated carbon dioxide cools the water in the tobacco leaves, forming ice within the cells and partially destroying aroma-storing organelles such as oil vesicles and vacuoles, thereby facilitating the migration of aroma components present inside the tobacco raw material toward the medium. To facilitate this migration, it is preferable for the medium to penetrate (impregnate) into the interior of the tobacco raw material. However, if the aroma components are completely dissolved or dispersed in the medium, it becomes difficult for the aroma components to remain on the surface of the tobacco raw material when the medium is removed. Therefore, the present invention combines efficient solvent penetration into the cells of the raw material to dissolve the desired aroma components in the solvent with gentle solvent removal to retain the aroma components present inside the cells on the surface of the tobacco raw material.

[0018] By impregnation, the surface migration ratio X, defined below, is adjusted to be greater than 1. Surface migration rate X=S / P S: Peak area of ​​aroma components present on the surface of the tobacco material after impregnation, measured by GC P: Peak area by GC of aroma components present on the surface of tobacco material before impregnation The surface migration ratio X is preferably 1.2 or more, more preferably 1.5 or more, and even more preferably 2 or more.

[0019] S is determined by collecting aroma compounds present on the surface of processed tobacco material and analyzing them using gas chromatography (GC). Specifically, the tobacco material is contacted with an aprotic solvent such as ethyl acetate to extract the aroma compounds present on the surface. The aprotic solvent is then removed and the extract is weighed. GC is then used to determine the peak area of ​​the aroma compounds. P is determined in the same manner as S using the tobacco material before processing.

[0020] S and P are more preferably defined as follows: S: Peak area by GC of aroma components extracted from the tobacco material after impregnation under the following conditions P: Peak area by GC of aroma components extracted from tobacco raw material before impregnation under the following conditions [conditions] 1) Weigh out 5 g of the impregnated tobacco material. 2) 100 ml of an aprotic solvent is placed in a container (preferably a 200 ml beaker), and the sample is placed therein. 3) After adding the ingredients, shake the container and extract for 30 seconds (think of it as washing the surface of the ingredients). 4) The extract is filtered to obtain a filtrate (preferably in a 200 ml Erlenmeyer flask). 5) The extract obtained in step 4) is filtered, preferably using filter paper. 6) Add a desiccant to the filtered extract and dehydrate overnight. 7) The drying agent is filtered off, and the filtrate is concentrated under reduced pressure to obtain a dry product. It is preferable to use filter paper for this process. This is dissolved in the aprotic solvent to form a 4% solution, which is then analyzed by GC / MS to obtain the S value. 8) Perform steps 1) to 7) on the tobacco raw material before impregnation to obtain the P value.

[0021] In a more preferred embodiment, the extraction is carried out in two stages, specifically as follows. [conditions] 1) Weigh out 5 g of the impregnated tobacco material. 2) 100 ml of an aprotic solvent is placed in a container (preferably a 200 ml beaker), and half of the sample is placed therein. 3) After adding the ingredients, gently shake the container and extract for 30 seconds (like washing the surface of the ingredients). 4-1) Filter the extract and collect the filtrate in another container (preferably a 200 ml Erlenmeyer flask). 4-2) Add the remaining ingredients to the filtrate and extract for 30 seconds in the same manner as in 3). 5) The extract obtained in step 4) is filtered, preferably using filter paper. 6) Add a desiccant to the filtered extract and dehydrate overnight. 7) The anhydrous sodium sulfate is filtered off, and the filtrate is concentrated under reduced pressure to obtain a dry product. It is preferable to use filter paper for this process. This is dissolved in the aprotic solvent to form a 4% solution, which is then analyzed by GC / MS to obtain the S value. 8) Perform steps 1) to 7) on the tobacco raw material before impregnation to obtain the P value.

[0022] The aprotic solvent may be an ester solvent such as ethyl acetate. The amount of the desiccant may be about 1 to 5 g, more preferably 2 to 4 g. Anhydrous inorganic salts such as anhydrous sodium sulfate may be used as the desiccant.

[0023] Aroma components subject to the surface migration rate X include terpene aroma components derived from the mevalonic acid pathway, such as monoterpenes and sesquiterpenes, such as limonene, geraniol, and farnesol; phenolic aroma components derived from the shikimic acid pathway or lignin, such as eugenol, anethole, and vanillin; fatty acid or linear unsaturated hydrocarbons, such as palmitic acid, myristic acid, oleic acid, and solanesol; aroma components derived from amino acids, such as indole and skatole; alkaloids, such as nicotine, specific to tobacco; and pigment degradation products, such as ionone, damascenone, and megastigmatrienone, derived from carotenoid pigments specific to dried leaves. All of these are accumulated or dried and fixed inside cells. Secretory aroma components include sesquiterpenes, such as cembratrienediol (CBT) and abienol, and diterpenes. Although CBT and other substances exist outside cells, they are retained near the surface by the intracellular components. Among these, the following are particularly important components for which the surface migration rate X is to be determined:

[0024] [Table A]

[0025] It is preferable that at least one of these has a surface migration rate X exceeding 1. In one embodiment, the impregnation time is 10 minutes or more or 15 minutes or more.

[0026] After impregnation, the impregnation process is completed by separating the treated tobacco material from the medium. The method of separation is not limited, but the medium can be removed by evaporation. For example, when using carbon dioxide in a liquid or supercritical state, the carbon dioxide can be removed by releasing the reaction system and returning the pressure to normal pressure. In this way, the tobacco material can be isolated. The time for releasing the pressure is not limited, but can be, for example, 0.1 to 100 minutes.

[0027] When the impregnation process is carried out under normal pressure using water or an organic solvent, the water and organic solvent can be separated from the tobacco material by, for example, evaporating them. Furthermore, it is not necessary to separate the treated tobacco material from the medium after impregnation. In this case, the tobacco material can be obtained as a mixture of the treated tobacco material and the medium.

[0028] (4) Crushing process The separated tobacco material can be pulverized to the desired size using known methods. Alternatively, the tobacco material obtained as a mixture can be subjected to pulverization. When liquid or supercritical carbon dioxide is used as the medium, the tobacco material is a mixture of the processed tobacco raw material and dry ice, and since the tobacco raw material is in a frozen state, it can be freeze-pulverized as is. Alternatively, when a medium that is liquid at normal pressure (water or an organic solvent) is used, the tobacco material is obtained as a mixture of the processed tobacco raw material and the liquid. In this case, it can also be subjected to wet pulverization. In one aspect, the D90 of the pulverized tobacco material is preferably 30 μm or less.

[0029] 2. Tobacco materials In the tobacco material obtained by the production method of the present invention (hereinafter referred to as "the tobacco material of the present invention"), aroma components that are originally present inside the cells are present outside the cells, or aroma components originally present outside the cells are trapped by components that have migrated from the inside of the cells, and are present in greater amounts on the surface. In other words, the tobacco material of the present invention is characterized by a surface migration rate X of greater than 1. Therefore, when used as a flavor inhalation article, the aroma components are easily released, providing the user with a pleasant smoking flavor. Flavor inhalation articles will be described later.

[0030] The tobacco material of the present invention can be used in various forms, such as tobacco sheets, shreds, cigarette papers, polysaccharide sheets, etc. These forms are explained below. (1) Tobacco sheets A tobacco sheet is a sheet obtained by molding a composition containing tobacco raw materials. A tobacco sheet can be prepared from a composition containing tobacco leaves and lamina, which are the tobacco materials of the present invention. In the present invention, "sheet" refers to a material having a pair of approximately parallel main and side surfaces. A tobacco sheet can be molded by known methods such as papermaking, casting, and rolling. Details of various tobacco sheets molded by these methods are disclosed in "Encyclopedia of Tobacco," Tobacco Research Center, March 31, 2009.

[0031] For example, in the papermaking method, a paper-made sheet can be produced by extracting water-soluble components from the tobacco leaves or lamina, separating them into an aqueous extract and a residue, making a mixture of the fibrous residue and pulp into paper, and adding a concentrated solution of the aqueous extract to the made sheet. In the casting method, a cast sheet can be produced by mixing water, pulp, a binder, and the tobacco leaves or lamina to form a mixture, and casting the mixture. In the rolling method, a sheet can be produced by mixing water, pulp, a binder, and ground tobacco leaves or lamina to form a mixture, and feeding the mixture into multiple rolling rollers to roll the mixture.

[0032] Furthermore, as described in International Publication No. 2014 / 104078, a nonwoven tobacco sheet can be obtained by mixing the ground tobacco leaves or lamina with a binder to form a mixture, sandwiching the mixture between nonwoven fabrics, and molding the laminate into a certain shape by heat welding.

[0033] The tobacco sheet may contain an aerosol-generating substrate. The type of aerosol-generating substrate is not particularly limited, and extracts from various natural products or their components can be selected depending on the application. Specific examples of aerosol-generating substrates include polyhydric alcohols such as glycerin, propylene glycol, sorbitol, xylitol, and erythritol, triacetin, 1,3-butanediol, and mixtures thereof. The content of the aerosol-generating substrate can be adjusted to various amounts depending on the form in which it is used in the tobacco product. For example, when the tobacco sheet contains an aerosol-generating substrate, the content thereof is typically 5% by weight or more, preferably 10% by weight or more, and more preferably 15% by weight or more, and typically 50% by weight or less, preferably 40% by weight or less, and more preferably 25% by weight or less, based on the total weight of the tobacco sheet, from the perspective of achieving a good flavor.

[0034] (2) time The tobacco leaves or lamina can be shredded to produce tobacco shreds, and the midrib can be shredded to produce midrib shreds. The size of the shredded tobacco is not limited, and examples include shredded tobacco with a width of 0.5 to 2.0 mm and a length of 3 to 10 mm. Shredded tobacco of this size is preferred in the embodiment of filling a filler, which will be described later. Another example of shredded tobacco is strand-type shredded tobacco, which is obtained by shredding processed tobacco leaves to a width of 0.5 to 2.0 mm and a length longer than the aforementioned tobacco shredded tobacco, preferably about the same length as cigarette paper.

[0035] The perilla may contain the aerosol-forming base material. When the perilla contains the aerosol-forming base material, the content thereof is usually 5% by weight or more, preferably 10% by weight or more, and more preferably 15% by weight or more, relative to the weight of the perilla, from the viewpoints of generating a sufficient amount of aerosol and obtaining a good flavor, and is usually 50% by weight or less, preferably 40% by weight or less, and more preferably 25% by weight or less.

[0036] 4. Tobacco-flavored inhalers In the present invention, a "flavor inhalation article" refers to an article with which a user inhales flavor. Among flavor inhalation articles, those containing tobacco or components derived from tobacco are called "tobacco flavor inhalation articles." Tobacco flavor inhalation articles are broadly classified into "combustion-type tobacco flavor inhalation articles" (also simply referred to as "smoking articles") that generate flavor through combustion, and "non-combustion-type tobacco flavor inhalation articles" that generate flavor without combustion. Non-combustion-type tobacco flavor inhalation articles are further broadly classified into "non-combustion-heating-type tobacco flavor inhalation articles" that generate flavor through heating, and "non-combustion-non-heating-type tobacco flavor inhalation articles" that generate flavor without heating. The tobacco flavoring agent of the present invention is suitable for combustion-type tobacco flavor inhalation articles or non-combustion-heating-type tobacco flavor inhalation articles.

[0037] (1) Combustible tobacco-flavored inhalation products The combustion-type tobacco flavor inhalation article may have a known structure. For example, the combustion-type tobacco flavor inhalation article may include a tobacco rod portion and a filter. The tobacco rod portion is filled with the tobacco material of the present invention, preferably in the form of shreds.

[0038] (2) Non-combustion heated tobacco flavor inhalation products FIG. 1 shows one embodiment of a non-combustion heating tobacco flavor inhalation article. As shown in the figure, the non-combustion heating tobacco flavor inhalation article 20 includes a tobacco rod portion 20A, a cylindrical cooling portion 20B having perforations on its circumference, and a filter portion 20C. The non-combustion heating tobacco flavor inhalation article 20 may include other components. The axial length of the non-combustion heating tobacco flavor inhalation article 20 is not limited, but is preferably 40 to 90 mm, more preferably 50 to 75 mm, and even more preferably 50 to 60 mm. The circumferential length of the non-combustion heating tobacco flavor inhalation article 20 is preferably 16 to 25 mm, more preferably 20 to 24 mm, and even more preferably 21 to 23 mm. For example, the tobacco rod portion 20A may be 20 mm long, the cooling portion 20B may be 20 mm long, and the filter portion 20C may be 7 mm long. The lengths of these individual components may be appropriately changed depending on manufacturing suitability, required quality, and the like. Although FIG. 1 shows an embodiment in which the first segment 25 is arranged, it is also possible to arrange only the second segment 26 downstream of the cooling section 20B without the first segment 25 being arranged.

[0039] 1) Tobacco rod part 20A The tobacco rod portion 20A can use the tobacco material of the present invention in the form of shredded tobacco or a tobacco sheet as the tobacco filler 21. The method for filling the tobacco filler 21 into the cigarette paper 22 is not particularly limited; for example, the tobacco filler 21 may be wrapped in the cigarette paper 22, or the tobacco filler 21 may be filled into a tubular cigarette paper 22. When the tobacco has a longitudinal direction, such as a rectangular shape, the tobacco may be filled so that the longitudinal direction is in an unspecified direction within the cigarette paper 22, or may be aligned in the axial direction of the tobacco rod portion 20A or in a direction perpendicular to the axial direction. Furthermore, the cigarette paper 22 can also be cigarette paper containing the tobacco flavoring agent of the present invention described above. When the tobacco rod portion 20A is heated, the tobacco components, aerosol-generating substrate, and water contained in the tobacco filler 21 vaporize and are available for inhalation.

[0040] 2) Cooling section 20B The cooling section 20B is preferably configured as a tubular member. The tubular member may be, for example, a cardboard tube 23 formed by processing cardboard into a cylindrical shape. The cooling section 20B may also be formed from a sheet of thin material that is wrinkled and then pleated, gathered, or folded to form channels. Examples of such materials include sheet materials selected from the group consisting of polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate, polylactic acid, cellulose acetate, and aluminum foil. The total surface area of ​​the cooling section 20B is appropriately adjusted taking into account cooling efficiency, and may be, for example, 300 to 1000 mm2 / mm2. The cooling section 20B is preferably provided with perforations 24. The presence of the perforations 24 allows outside air to be introduced into the cooling section 20B during puffing. This allows the tobacco rod section 20 The vaporized aerosol components generated by heating A come into contact with the outside air, and as their temperature drops, they are liquefied, forming an aerosol. The diameter (distance across) of perforations 24 is not particularly limited, but may be, for example, 0.5 to 1.5 mm. The number of perforations 24 is not particularly limited, and may be one or two or more. For example, a plurality of perforations 24 may be provided on the circumference of cooling section 20B.

[0041] The cooling section 20B may be rod-shaped with an axial length of, for example, 7 to 28 mm. For example, the axial length of the cooling section 20B may be 18 mm. The cooling section 20B may have a substantially circular axial cross section with a diameter of 5 to 10 mm. For example, the diameter of the cooling section may be approximately 7 mm.

[0042] 3) The filter part 20C The configuration of the filter part 20C is not particularly limited, and may be composed of one or more packed layers. The outside of the packed layer may be wrapped with one or more sheets of wrapping paper. The airflow resistance of the filter part 20C can be appropriately changed depending on the amount, material, etc. of the packing filled in the filter part 20C. For example, when the packing is cellulose acetate fiber, the airflow resistance can be increased by increasing the amount of cellulose acetate fiber filled in the filter part 20C. When the packing is cellulose acetate fiber, the packing density of the cellulose acetate fiber is 0.13 to 0.18 g / cm. 3 The airflow resistance is a value measured using an airflow resistance measuring device (product name: SODIMAX, manufactured by SODIM).

[0043] The circumferential length of the filter portion 20C 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 portion 20C (the horizontal direction in FIG. 1) can be selected from 4 to 10 mm, and is selected so that the airflow resistance is 15 to 60 mmH2O / seg. The axial length of the filter portion 20C is preferably 5 to 9 mm, more preferably 6 to 8 mm. The cross-sectional shape of the filter portion 20C is not particularly limited, but may be, for example, circular, elliptical, polygonal, etc. In addition, a flavor-containing breakable capsule, flavor beads, or flavor may be directly added to the filter portion 20C.

[0044] The filter portion 20C may have a center hole portion as the first segment 25. The center hole portion is composed of a first packed layer 25a having one or more hollow portions and an inner plug wrapper (inner wrapping paper) 25b that covers the packed layer. The center hole portion has the function of increasing the strength of the mouthpiece portion. The center hole portion may not have an inner plug wrapper 25b, and its shape may be maintained by thermoforming. The filter portion 20C may have a second segment 26. The second segment 26 is composed of a second packed layer 26a and an inner plug wrapper (inner wrapping paper) 26b that covers the packed layer. First packed layer 25aFor example, the cellulose acetate fiber may be densely packed, and a plasticizer containing triacetin may be added in an amount of 6 to 20% by weight based on the weight of the cellulose acetate, and the plasticizer may be hardened to form a rod having an inner diameter of 5.0 to 1.0 mm. 1 Because the filling layer has a high fiber packing density, when inhaling, air and aerosols flow only through the hollow part, with almost no flow within the second filling layer. Because the second filling layer inside the center hole segment is a fiber-filled layer, the feel from the outside during use is less likely to cause discomfort to the user.

[0045] The first filling layer 25a and the second filling layer 26a are connected by an outer plug wrapper (outer wrapping paper) 27. The outer plug wrapper 27 can be, for example, a cylindrical piece of paper. The tobacco rod portion 20A, the cooling portion 20B, and the connected first filling layer 25a and second filling layer 26a are connected by a mouthpiece lining paper 28. These connections can be made, for example, by applying a glue such as a vinyl acetate glue to the inner surface of the mouthpiece lining paper 28 and wrapping the three components. These components may also be connected in multiple layers using multiple lining papers.

[0046] A combination of a non-combustion heating type tobacco flavor inhalation article and a heating device for generating an aerosol is particularly referred to as a non-combustion heating type tobacco flavor inhalation system. An example of such a system is shown in Fig. 2. In the figure, the non-combustion heating type tobacco flavor inhalation system includes a non-combustion heating type tobacco flavor inhalation article 20 and a heating device 10 that heats a tobacco rod portion 20A from the outside.

[0047] The heating device 10 includes a body 11, a heater 12, a metal tube 13, a battery unit 14, and a control unit 15. The body 11 has a cylindrical recess 16, and the heater 12 and metal tube 13 are disposed in a position corresponding to the tobacco rod portion 20A to be inserted therein. The heater 13 may be an electric resistance heater, and is heated by power supplied from the battery unit 14 in response to instructions from the control unit 15, which controls the temperature. The heat generated by the heater 12 is transferred to the tobacco rod portion 20A through the metal tube 13, which has high thermal conductivity. While the figure shows an embodiment in which the heating device 10 heats the tobacco rod portion 20A from the outside, it may also heat from the inside. The heating temperature of the heating device 10 is not particularly limited, but is preferably 400°C or less, more preferably 150 to 400°C, and even more preferably 200 to 350°C. The heating temperature refers to the temperature of the heater of the heating device 10. [Example]

[0048] The present invention will be described below with reference to examples. In the present invention, unless otherwise specified, the pressure inside the vessel is a gauge pressure. [Example 1] Examination of impregnation conditions and CO2 removal conditions Approximately 600 g of Brazilian flue-cured lamina with an initial moisture content of 10.5% by weight was weighed out and placed in a stainless steel wire mesh container, which was then placed in a pressure vessel (internal volume: 9 liters). The pressure vessel was then purged with carbon dioxide gas for 10 seconds. Carbon dioxide gas was then introduced into the pressure vessel to maintain the pressure at 30 kg / cm. 2The pressure vessel was pressurized to an impregnation pressure of 2.9 MPa (gauge pressure). After stopping the supply of carbon dioxide gas, the supply of liquid carbon dioxide was started from the top of the pressure vessel. Liquid carbon dioxide was gradually supplied until all of the thermocouples installed at the top, middle, and bottom of the tobacco layer indicated the saturation temperature of carbon dioxide gas at the impregnation pressure. Almost simultaneously with the lowest thermocouple indicating the above saturation temperature, a small amount of liquid carbon dioxide began to drip from the bottom of the pressure vessel. At this point, the supply of liquid carbon dioxide was stopped. One minute after the supply was stopped, the pressure inside the pressure vessel was released to atmospheric pressure over a period of approximately one minute (experimental level 1) or approximately 90 minutes (experimental level 2), allowing the carbon dioxide to be thoroughly evaporated and removed within the vessel. The treated tobacco was then removed from the pressure vessel.

[0049] [Example 2] Migration rate of components to the outside Five grams of lamina treated in Example 1 and untreated lamina were separated. Following the extraction method of Severson et al., each lamina was separated using tweezers and immersed in a 300-ml glass container filled with 100 ml of ethyl acetate for no more than 30 seconds to dissolve as many surface-exclusive components as possible. The ethyl acetate was removed under reduced pressure using a rotary evaporator, and the weight of the dried product was measured. The dried product was completely dissolved in chloroform to prepare a solution with a concentration of 4 wt. GC / MS analysis was performed according to the conditions listed in Table 1. Table 2 shows the surface migration ratio. Figure 3 shows a gas chromatogram. According to the method of Severson et al., a surface migration ratio greater than 1 was considered to indicate that the components had migrated from the interior to the exterior of the tobacco leaf cells.

[0050] [Table 1]

[0051] [Table 2-1]

[0052] [Table 2-2]

[0053] [Example 3] Examination of impregnation conditions and CO2 removal conditions A typical lamina was placed in a stainless steel mesh container, which was then housed in a pressure vessel (internal volume 1 L (liter), diameter 80 mm, depth 200 mm). The pressure vessel was then purged with carbon dioxide gas for 10 seconds. Carbon dioxide gas was then introduced into the pressure vessel to maintain the pressure in the vessel at 30 or 50 kg / cm. 2 The pressure vessel was pressurized to an impregnation pressure of 2.9 MPa and 4.9 MPa (gauge pressure, respectively). After stopping the supply of carbon dioxide gas, the supply of liquid carbon dioxide was started from the top of the pressure vessel. Liquid carbon dioxide was gradually supplied until all of the thermocouples installed in the upper, middle, and lowermost parts of the tobacco layer indicated the saturation temperature of carbon dioxide gas at the impregnation pressure. Almost simultaneously with the lowest thermocouple indicating the saturation temperature, a small amount of liquid carbon dioxide began to drip from the bottom of the pressure vessel. At this point, the supply of liquid carbon dioxide was stopped. The time for impregnation with liquid carbon dioxide after the supply was stopped and the time for releasing the pressure inside the pressure vessel to atmospheric pressure were as shown in Table 3. After opening the vessel, the carbon dioxide-impregnated lamina was removed. As described above, the surface migration rate X was determined for each sample.

[0054] [Table 3]

[0055] [Example 4] Freeze-pulverization 60g of yellow-leafed rice (Brazilian yellow-leafed rice) lamina was placed in a stainless steel pressure vessel, and then carbon dioxide was added until the internal pressure reached 50kg / cm. 2 The lamina was filled to a pressure of 4.9 MPa (gauge pressure) and left to stand for 1 minute. The internal temperature at that time was 15.1°C. The valve of the pressure-resistant container was then opened and the pressure was returned to normal over 30 minutes. The moisture content and dry ice content of the lamina at that time were 10% and 16% by weight, respectively. The frozen lamina was pulverized into fine powder using a benchtop pulverizer (Power Mill LM-05, manufactured by Dalton) to an average particle size of 30 μm or less.

[0056] [Example 5] 700g of yellow-leafed rice (Brazilian yellow-leafed rice) lamina was placed in a stainless steel pressure vessel, and then carbon dioxide was added until the internal pressure reached 30kg / cm. 2 The container was filled to a pressure of 2.9 MPa (gauge pressure) and allowed to stand for 1 minute, at which point the internal temperature was -4.4°C. The valve of the pressure-resistant container was then opened, and the pressure was returned to normal over 90 minutes. The moisture content of the lamina at this time was 10% by weight. The lamina was shredded into pieces approximately 1 mm wide and 5-20 mm long using a shredder to obtain shreds. Approximately 700 mg of the shreds were randomly oriented and packed into a cylindrical cigarette paper with a circumference of 24.4 mm and a length of 50 mm to obtain a smoking article. The smoking article was subjected to a smoking evaluation by seven well-trained experts using the method described below.

[0057] [Example 6] The lamina was treated in the same manner as in Example 5, except that the valve of the pressure-resistant container was opened and the pressure was returned to normal over 1 minute. The moisture content of the lamina after treatment was 10% by weight. Smoking articles were obtained using the lamina in the same manner as in Example 5 and evaluated.

[0058] [Comparative Example] Laminae from flue-cured tobacco (Brazilian true leaf flue-cured tobacco) were conditioned to a moisture content of approximately 12% by weight. Smoking articles were obtained using the lamina in the same manner as in Example 5 and evaluated. The results are shown in the table below.

[0059] [Table 4]

[0060] [Smoking Rating] Number of puffs: 7-10 Smoking order: The smoking article obtained in the Comparative Example was smoked, followed by the smoking article obtained in Example 5. Next, the smoking article obtained in the Comparative Example was smoked, followed by the smoking article obtained in Example 6. Evaluation items: flavor, sweetness, astringency Score: A Significant increase compared to the comparative example B Increased compared to comparative example C Decreased compared to the comparative example D Significantly reduced compared to the comparative example [Explanation of symbols]

[0061] 10 Heating device 11 Body 12 Heater 13 Metal tube 14 Battery unit 15 Control Unit 16 Recess 17 Ventilation holes 20 Non-combustion heating type flavor inhalation product 20A Tobacco rod part 20B Cooling section 20C filter section 21 Tobacco filler 22 Rolling Paper 23 Paper tube 24 perforation 25 First Segment 25a 1st packed bed 25b inner plug wrapper 26 Second Segment 26a 2nd packed bed 26b Inner plug wrapper 27 Outer plug wrapper 28 Lining Paper

Claims

1. A method of impregnating a tobacco raw material with a medium for 10 minutes or more in a heat-resistant container under a pressure of 2 MPa or more; and then opening the heat-resistant container for 15 minutes or more; the medium is liquid carbon dioxide or supercritical carbon dioxide; Obtaining a tobacco material having a surface transfer ratio X greater than 1, as defined below, Surface transfer rate X=S / P S: Peak area by GC of flavor components present on the surface of the tobacco raw material after impregnation P: Peak area by GC of flavor components present on the surface of the tobacco raw material before impregnation The tobacco raw material is a tobacco leaf, a lamina, a midrib, a stem, or a shred, which may be harmonized or not, The moisture content of the conditioned raw material is 5-40% by weight. A method for producing tobacco materials.

2. 2. The method of claim 1, wherein the tobacco raw material is a conditioned raw material, and the conditioned processing comprises storing the raw material at 22°C and 60% humidity for 24 hours or more.

3. The method according to claim 2, wherein the raw material is stored for 30 hours or less.

4. The manufacturing method according to any one of claims 1 to 3, wherein the impregnation comprises permeating the medium into the entire tobacco raw material.

5. The method according to any one of claims 1 to 4, wherein the solvent used for the impregnation is liquid carbon dioxide.

6. The manufacturing method according to claim 5 , wherein the atmospheric pressure of the tobacco raw material during the impregnation is 2 MPa or more.

7. The method according to claim 6, wherein the pressure is 3 MPa or more.

8. The method according to claim 7, wherein the pressure is 5 MPa or more.

9. The method according to any one of claims 5 to 8, wherein the pressure is less than 100 MPa.

10. The method for producing a tobacco material according to any one of claims 5 to 9, wherein the atmospheric temperature of the tobacco raw material during the impregnation is -10 to 35°C.

11. The method for producing a tobacco material according to any one of claims 1 to 4, wherein the medium used for the impregnation is supercritical carbon dioxide.

12. The method for producing a tobacco material according to claim 11, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 100 MPa or more.

13. The method for producing a tobacco material according to claim 11 or 12, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 200 MPa or more.

14. The method for producing a tobacco material according to any one of claims 11 to 13, wherein the atmospheric pressure of the tobacco raw material during the impregnation is 300 MPa or less.

15. The method for producing a tobacco material according to any one of claims 11 to 14, wherein the atmospheric temperature of the tobacco raw material during the impregnation is greater than 35°C and equal to or less than 70°C.

16. The method according to any one of claims 1 to 15, further comprising a step of wet-grinding the tobacco raw material after the impregnation.

17. A tobacco material obtainable by the method according to any one of claims 1 to 16.

18. The tobacco material according to claim 17, which is in a form selected from the group consisting of tobacco sheets, tobacco shreds, shredded midribs, and combinations thereof.

19. The tobacco material according to claim 18, wherein the tobacco shreds or midrib shreds have a width of 0.5 to 2.0 mm and a length of 3 to 10 mm.

20. 20. The tobacco material according to any one of claims 17 to 19, wherein the tobacco material comprises 5 to 50% by weight of the aerosol-forming substrate, based on the total weight of the tobacco material.

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