Manufacturing method of tobacco material

Abstract

A tobacco material production method comprising: a step for impregnating a tobacco raw material with a medium in a state selected from the group consisting of gas, liquid, and a supercritical state; and a step for obtaining a tobacco material having a surface migration rate X as defined below, exceeds 1, wherein surface migration rate X equals S / P, where S represents a peak area, as determined by GC, of flavor components present on the surface of the tobacco raw material after impregnation, and P represents a peak area, as determined by GC, of flavor components present on the surface of the tobacco raw material prior to impregnation.

Description

[Technical field]

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

[0002] Research has been conducted on the aroma components of tobacco leaves using a wide variety of tobacco raw materials, including flue-cured, burley, Oriental, and Maryland tobacco, and characteristic components have been reported for each raw material variety. More than 4,000 types of components have been reported so far (Non-Patent Document 1). Components that contribute to characteristic tobacco leaf aromas can be roughly divided into two groups based on whether they are localized inside or outside the cells of tobacco leaves. The first group includes components present in the cellular tissue of tobacco leaves. These are aromas that are mainly composed of decomposition products derived from pigments generated during the maturation or drying process of tobacco leaves, that is, pigment decomposition products such as ionone, megastigmatrienone, and phytol, monoterpenes, and phenols. All of these are accumulated inside the cellular tissue of tobacco leaves via metabolic pathways related to the generation of general aroma components, such as the pigment decomposition pathway, the mevalonic acid pathway, and the shikimic acid pathway.

[0003] The second is the components present on the surface of tobacco leaves. This is generally called leaf surface resin, and is made up of relatively high molecular weight organic acids, hydrocarbons, glycosides, etc., that are produced and secreted by hair fungi and other organelles to protect the tissue from pests and diseases or the growing environment. Its aroma components are characterized by being 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. A method for extracting the components using liquefied carbon dioxide or supercritical carbon dioxide has been proposed, taking advantage of the characteristics of the components of interest (e.g., Patent Documents 1 and 2). As one of the raw materials for combustion tobacco, a raw material obtained by expanding tobacco leaves with liquefied carbon dioxide has been considered, but the process is very similar to the above-mentioned extraction process using carbon dioxide. Therefore, a method that applies a part of the expansion process has 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 brings the tobacco raw material into contact with carbon dioxide in a supercritical state and dissolves the tobacco components in the carbon dioxide, a separation vessel connected to the extraction vessel that separates and recovers the fat-soluble portion 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 storing pure water while purifying it with a purification layer of activated carbon, and absorbs the water-soluble portion of the tobacco components into the pure water, and a recovery vessel that recovers the pure water that has absorbed the water-soluble portion of the tobacco components from the absorption vessel as absorbed water. The fat-soluble portions of the tobacco components and the 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 cells of the tobacco leaf as described above, they are likely to be transferred to mainstream smoke, and the effect of localization is thought to be very small.

[0008] On the other hand, in the case of non-combustion cigarettes, compared to conventional combustion cigarettes, the movement inside the cells is restricted by the shielding of structures such as cell walls, so the volatilization of components localized on the surface, mainly consisting of leaf surface resin, takes precedence. In other words, in non-combustion cigarettes, the heating temperature is important for releasing the aroma components present inside the cells, and it was thought that it was necessary to heat to 200°C or higher, which is the thermal denaturation temperature of the cell wall components (Non-Patent Document 2). For example, ionone (Non-Patent Document 1), which is a decomposition product of carotene contained in plastids, is present inside the cells, so its release is suppressed at low temperatures. However, at the thermal denaturation temperature, it volatilizes all at once along with the thermal denaturation of the cell wall components, so it was expected that its delivery would not be easy to control. In contrast, cembratrienediol (CBT) (Non-Patent Document 3), a leaf surface resin component, has a low vapor pressure, so it was expected to be delivered according to the amount of heat given compared to the aroma components present inside the cells mentioned above. In other words, in non-combustion cigarettes, the release of the aroma components is restricted depending on the location where the aroma components are present, so it is not easy to release the aroma components like in combustion cigarettes. 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, in the expansion process of tobacco leaves, aroma components present within tobacco leaf cells move from within the cells to outside the cells when the carbon dioxide is vaporized after the impregnation with gaseous carbon dioxide, and that the aroma components may mix with low-volatility substances such as leaf surface resins that are already present outside the cells at the cell surface, 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 The method includes 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 transfer ratio X greater than 1, as defined below; Surface migration 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 tobacco raw material before impregnation A method for producing tobacco materials. Aspect 2 2. The method of claim 1, wherein the medium is carbon dioxide, water, or an organic solvent. Aspect 3 A method according to any one of the preceding claims, wherein the medium is liquid carbon dioxide or carbon dioxide in a supercritical state. Aspect 4 The method according to any one of aspects 1 to 3, wherein the impregnation step is carried out under a pressure of 2 MPa or more. Aspect 5 The method according to any one of aspects 1 to 4, wherein the impregnation step is carried out for 10 minutes or more. Aspect 6 The S and P are determined under the following conditions: [conditions] 1) Weigh out 5 g of the impregnated tobacco raw material. 2) 100 ml of aprotic solvent is placed in a container, and the sample is placed therein. 3) After adding, shake the container and extract for 30 seconds. 4) Filter the extract to obtain the filtrate. 5) The extract obtained in 4) is filtered, preferably using filter paper. 6) Add a desiccant to the filtered extract and dehydrate overnight. 7) The drying agent is preferably filtered off using filter paper, and the filtrate is concentrated under reduced pressure to obtain a solid dry matter, which is then dissolved in the aprotic solvent to give a 4% solution and 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. The method according to any one of aspects 1 to 5. Aspect 7 The method according to any one of Aspects 1 to 6, wherein the tobacco raw material is blended or unbleached tobacco leaves, lamina, ribs, stem residues, or shreds. Aspect 8 The production method according to any one of aspects 1 to 7, further comprising a step of pulverizing the tobacco raw material after the impregnation. Aspect 9 A method according to any one of aspects 1 to 8, wherein the tobacco material and the medium are not separated after the impregnation, and the tobacco material after separation is pulverized. Aspect 10 A method according to embodiment 9, wherein the grinding is freeze-grinding. Aspect 11 A tobacco material obtained by the method of any one of aspects 1 to 10. Aspect 12 12. The tobacco material according to embodiment 11, having a D90 of 30 μm or less. Effect of the Invention

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

[0011] [Figure 1] FIG. 1 is a diagram showing an embodiment of a non-combustion heating type tobacco flavor inhalation article. [Diagram 2] FIG. 1 shows an embodiment of a non-combustion heating type tobacco flavor inhalation system. [Diagram 3] Gas chromatogram DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[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, to obtain a material having a surface transfer ratio X, as defined below, of greater than 1. Surface migration rate X=S / P S: Peak area by GC of aroma components present on the surface of the tobacco raw material after impregnation P: Peak area by GC of aroma components present on the surface of tobacco raw 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. Among them, it is preferable to use carbon dioxide as the medium from the viewpoint of utilizing the expansion treatment of tobacco leaves.

[0014] These media may be in a gas, 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 expansion treatment of tobacco leaves as described above, it is preferable to use carbon dioxide in a liquid or supercritical state as the medium.

[0015] (2) Tobacco raw materials The tobacco raw material is not limited as long as it is derived from a Nicotiana plant, but from the viewpoint of ease of availability, tobacco leaves, lamina, midrib, stem residue, or shreds are preferred. Tobacco leaves are a collective term for harvested tobacco leaves before aging. One form of aging includes curing. Lamina are tobacco leaves that have had their bones removed, 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 midribs that have been chopped into a specified size. Among them, midribs that have been chopped into a specified size are also called midrib shreds. These may be subjected to a harmonization treatment. Harmonization treatment refers to adjusting the state to make the moisture content constant. For example, harmonization treatment can be performed by storing the lamina at 22°C and 60% for 24 hours or more. There is no upper limit to the storage time, but it is preferable that it is within 30 hours. If the moisture content of the raw material is high, the raw material will swell, making it easier for the medium to diffuse into the cells, and the aroma components present inside the cells will be more likely to move to the outside. On the other hand, if the raw material has a high moisture content, 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% by weight, more preferably 10 to 30% by weight.

[0016] (3) Impregnation process Impregnation refers to permeating the medium into the tobacco raw material. It is sufficient that the medium permeates at least a part of the tobacco raw material, but it is preferable that the medium permeates the entire tobacco raw material. The pressure and temperature during impregnation are adjusted to bring the medium into a desired state. For example, when liquid carbon dioxide is used, the atmospheric pressure of the tobacco raw 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 (both 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 (both 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 raw material at this time (e.g., the product temperature or the temperature inside the container) can be more than 35°C to 70°C.

[0017] The impregnation process causes aroma components present inside the cells of the tobacco raw material to move outside the cells and further to the surface of the tobacco raw material. The reason for this is not limited, but it is presumed that the contact of the medium impregnated in the tobacco raw material with 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 move toward the medium. When carbon dioxide is used, in addition to the above, the impregnated carbon dioxide cools the water in the tobacco leaves, and ice is generated inside the cells, which partially destroys the aroma-storing organs such as oil vacuoles and vacuoles, making it easier for the aroma components present inside the tobacco raw material to move toward the medium. In order to make this movement smoother, it is preferable for the medium to penetrate (impregnate) into 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. For this reason, in the present invention, the aroma components present inside the cells can be retained on the surface of the tobacco raw material by a combination of efficiently penetrating the solvent into the cells of the raw material to dissolve the desired aroma components in the solvent and removing the solvent as gently as possible.

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

[0019] S is determined by collecting aroma components present on the surface of the processed tobacco raw material and analyzing them using gas chromatography (GC). Specifically, the tobacco raw material is contacted with an aprotic solvent such as ethyl acetate to extract the aroma components 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 components. P is determined in the same manner as S, using the tobacco raw 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 raw material. 2) 100 ml of 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 (like washing the surface of the ingredients). 4) Filter the extract to obtain a filtrate (preferably in a 200 ml Erlenmeyer flask). 5) The extract obtained in 4) above 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 solidified product. In this case, it is preferable to use filter paper. This is dissolved in the aprotic solvent to obtain a 4% solution, and 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 raw 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 (imagine 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 4) above is filtered, preferably using filter paper. 6) Add a desiccant to the filtered extract and dehydrate overnight. 7) Filter off the anhydrous sodium sulfate, and concentrate the filtrate under reduced pressure to obtain a dry solid. In this case, it is preferable to use filter paper. This is dissolved in the aprotic solvent to make a 4% solution, and 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 drying agent 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 drying agent.

[0023] The aroma components that are the subject of the surface migration rate X include terpene aroma components from the mevalonic acid pathway, such as monoterpenes and sesquiterpenes, such as limonene, geraniol, and farnesol; phenolic aroma components 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, which are specific to tobacco, and pigment decomposition products, such as ionone, damascenone, and megastigmatrienone, which are derived from carotenoid pigments, which are specific to dried leaves. All of these are accumulated or dried and fixed inside the cells. In addition, examples of secretory aroma components include sesquiterpenes, such as cembratrienediol (CBT) and abienol, and diterpenes. Although CBT and the like are substances present outside the cells, they are held near the surface by the components present inside the cells. Among them, the following are particularly important components as targets for the surface migration rate X:

[0024] [Table A]

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

[0026] After the impregnation, the treated tobacco raw material and the medium are separated, and the impregnation process is completed. The method of separation is not limited, but the medium can be removed by evaporating it. For example, when liquid or supercritical carbon dioxide is used, 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, and can be, for example, 0.1 to 100 minutes.

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

[0028] (4) Crushing process The separated tobacco material can be pulverized to a desired size by a known method. The tobacco material obtained as a mixture can also be subjected to pulverization. When liquid or supercritical carbon dioxide is used as the medium, the tobacco material is a mixture of the treated tobacco raw material and dry ice, and since the tobacco raw material is in a frozen state, it can be freeze-pulverized as it 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 treated tobacco raw material and the liquid. In this case, it can also be subjected to wet pulverization. In one embodiment, the D90 of the pulverized tobacco material is preferably 30 μm or less.

[0029] 2. Tobacco materials In the tobacco material obtained by the manufacturing 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. That is, the tobacco material of the present invention is characterized in that the surface migration rate X exceeds 1. Therefore, when used as a flavor inhalation article, the aroma components are easily released and provide 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., as described 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 a known method such as a papermaking method, a casting method, or a rolling method. Details of various tobacco sheets molded by such 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, 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, the ground tobacco leaves or lamina can be mixed with a binder to form a mixture, the mixture can be sandwiched between nonwoven fabric, and the laminate can be molded into a certain shape by thermal welding to obtain a nonwoven tobacco sheet.

[0033] The tobacco sheet may contain an aerosol-generating substrate. The type of the aerosol-generating substrate is not particularly limited, and various extracts from natural products or their components can be selected according to the application. Specific examples of the aerosol-generating substrate 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 is usually 5% by weight or more, preferably 10% by weight or more, and more preferably 15% by weight or more, and usually 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 viewpoint of obtaining a good flavor.

[0034] (2) time The tobacco leaves or lamina may be chopped to obtain tobacco shreds, and the midrib may be chopped to obtain midrib shreds. The size of the shreds is not limited, and examples include shreds with a width of 0.5 to 2.0 mm and a length of 3 to 10 mm. Shreds of such a size are preferable in the embodiment of filling a filling material described below. In addition, the shreds may be strand-type shreds obtained by chopping processed tobacco leaves to a width of 0.5 to 2.0 mm and a length longer than the tobacco shreds described above, preferably about the same length as the cigarette paper.

[0035] The shredded meat may contain the aerosol-forming base material. When the aerosol-forming base material is contained in the shredded meat, the content of the aerosol-forming base material is usually 5% by weight or more, preferably 10% by weight or more, more preferably 15% by weight or more, based on the weight of the shredded meat, 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, more preferably 25% by weight or less.

[0036] 4. Tobacco-flavored inhalation products In the present invention, the term "flavor inhalation article" refers to an article for a user to inhale 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 called "smoking articles") that generate flavor by combustion, and "non-combustion type tobacco flavor inhalation articles" that generate flavor without combustion. Furthermore, non-combustion type tobacco flavor inhalation articles are broadly classified into "non-combustion heating type tobacco flavor inhalation articles" that generate flavor by 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) Combustion-type tobacco flavor 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 heating tobacco flavor inhalation products FIG. 1 shows an 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 the circumference, and a filter portion 20C. The non-combustion heating tobacco flavor inhalation article 20 may include other members. 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 or less. 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, an embodiment in which the length of the tobacco rod portion 20A is 20 mm, the length of the cooling portion 20B is 20 mm, and the length of the filter portion 20C is 7 mm can be mentioned. The length of each of these members can be appropriately changed according to the manufacturing suitability, the required quality, and the like. FIG. 1 shows an embodiment in which the first segment 25 is disposed, but it is also possible to dispose the first segment 25 and to dispose only the second segment 26 downstream of the cooling section 20B.

[0039] 1) Tobacco rod section 20A In the tobacco rod portion 20A, the tobacco material of the present invention in the form of shreds or tobacco sheets can be used as the tobacco filler 21. The method of filling the tobacco filler 21 into the cigarette paper 22 is not particularly limited, but for example, the tobacco filler 21 may be wrapped in the cigarette paper 22, or the tobacco filler 21 may be filled into a cylindrical 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 in the cigarette paper 22, or may be filled so that the tobacco is aligned in the axial direction of the tobacco rod portion 20A or aligned in a direction perpendicular to the axial direction. In addition, the cigarette paper 22 may be a 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 base material, and water contained in the tobacco filler 21 are vaporized and are available for inhalation.

[0040] 2) Cooling section 20B The cooling section 20B is preferably constructed of a cylindrical member. The cylindrical 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 by a sheet of thin material that is wrinkled and then pleated, gathered, or folded to form a channel. For example, a sheet material selected from the group consisting of polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate, polylactic acid, cellulose acetate, and aluminum foil may be used as such a material. The total surface area of ​​the cooling section 20B is appropriately adjusted in consideration of the cooling efficiency, and may be, for example, 300 to 1000 mm2 / mm. 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 inhalation. This allows the tobacco rod section 20 The vaporized aerosol components generated by heating A come into contact with the outside air, and the temperature drops, so that the components are liquefied, forming an aerosol. The diameter (diameter) of the perforations 24 is not particularly limited, and 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 the 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-sectional shape with a diameter of 5 to 10 mm. For example, the diameter of the cooling section may be about 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 layers may be wrapped with one or more wrapping papers. The airflow resistance of the filter part 20C can be appropriately changed depending on the amount and material 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 by an airflow resistance measuring device (product name: SODIMAX, manufactured by SODIM).

[0043] The circumferential length of the filter part 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 part 20C (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 part 20C is preferably 5 to 9 mm, more preferably 6 to 8 mm. The cross-sectional shape of the filter part 20C is not particularly limited, but can be, for example, a circle, an ellipse, a polygon, etc. In addition, a destructible capsule containing a fragrance, fragrance beads, or a fragrance may be directly added to the filter part 20C.

[0044] The filter part 20C may have a center hole part as the first segment 25. The center hole part is composed of a first packed layer 25a having one or more hollow parts and an inner plug wrapper (inner wrapping paper) 25b that covers the packed layer. The center hole part has a function of increasing the strength of the mouthpiece part. The center hole part may not have an inner plug wrapper 25b and may maintain its shape by thermoforming. The filter part 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 φ5.0 to φ1.0 mm. 1 Because the filling layer has a high fiber packing density, air and aerosols flow only through the hollow portion during inhalation, and barely any flow occurs within the second filling layer. Because the second filling layer inside the center hole segment is a fiber filling 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 paper. The tobacco rod portion 20A, the cooling portion 20B, and the first filling layer 25a and the second filling layer 26a that have already been connected 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 winding the three components. These components may be connected in multiple separate passes 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 also referred to as a non-combustion heating type tobacco flavor inhalation system. An example of the 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 the metal tube 13 are disposed at a position corresponding to the tobacco rod portion 20A to be inserted therein. The heater 13 can be a heater using electric resistance, and is heated by being supplied with power from the battery unit 14 in response to an instruction from a control unit 15 that controls 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. In the figure, the heating device 10 is shown as heating the tobacco rod portion 20A from the outside, but may be heating from the inside. The heating temperature by 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. EXAMPLES

[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 (capacity 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 in the vessel at 30 kg / cm. 2The pressure was increased to an impregnation pressure of 2.9 MPa (gauge pressure). After the supply of carbon dioxide gas was stopped, 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 thermocouple at the bottom indicating the above-mentioned saturation temperature, a very small amount of liquid carbon dioxide dripped 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 about one minute (experimental level 1) or about 90 minutes (experimental level 2), and carbon dioxide was thoroughly removed by volatilization within the vessel. Furthermore, each treated tobacco was removed from the pressure vessel.

[0049] [Example 2] Migration rate of components to the outside 5 g of the lamina treated in Example 1 and untreated lamina were taken. Referring to the extraction method of Severson et al., each lamina was taken using tweezers and immersed in a 300 ml glass container filled with 100 ml of ethyl acetate for not more than 30 seconds, and the components present only on the surface were dissolved in the ethyl acetate. 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%, and GC / MS analysis was performed according to the conditions in Table 1. Table 2 shows the surface migration rate. Figure 3 shows a gas chromatograph. According to the method of Severson et al., when the surface migration rate exceeded 1, it was determined that the content components had migrated from the inside to the outside 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 representative lamina was placed in a stainless steel wire 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 was increased to an impregnation pressure of 2.9 MPa and 4.9 MPa (gauge pressure, respectively). After the supply of carbon dioxide gas was stopped, 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 thermocouple at the bottom indicating the above-mentioned saturation temperature, a very small amount of liquid carbon dioxide dripped 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 in the pressure vessel to atmospheric pressure were as shown in Table 3. After the vessel was opened, the carbon dioxide-impregnated lamina was taken out. As described above, the surface migration rate X was determined for each sample.

[0054] [Table 3]

[0055] [Example 4] Freeze-grinding 60g of yellow-leafed rice (Brazilian yellow-leafed rice) lamina was placed in a stainless steel pressure vessel, and then carbon dioxide was pumped in 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 vessel 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. The lamina in the frozen state was pulverized into fine powder with an average particle size of 30 μm or less using a benchtop pulverizer (Power Mill LM-05 manufactured by Dalton Co., Ltd.).

[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 pumped in until the internal pressure reached 30kg / cm. 2 (2.9 MPa gauge pressure) and left for 1 minute, at which time 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 cut into pieces with a width of about 1 mm and a length of about 5 to 20 mm using a shredder to obtain shreds. About 700 mg of the shreds were randomly oriented and filled 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. Using the lamina, smoking articles were obtained and evaluated in the same manner as in Example 5.

[0058] [Comparative Example] The lamina of flue-cured tobacco (Brazilian true leaf flue-cured tobacco) was conditioned so that the moisture content was about 12% by weight. Using the lamina, smoking articles were obtained and evaluated in the same manner as in Example 5. 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 Comparative Example was smoked, followed by the smoking article obtained in Example 5. Next, the smoking article obtained in Comparative Example was smoked, followed by the smoking article obtained in Example 6. Evaluation items: Aroma, sweetness, astringency Score: A Significant increase compared to the comparative example B Increased compared to comparative example C Decreased compared to 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 products 20A Tobacco rod part 20B Cooling section 20C Filter section 21 Tobacco filling 22 Scroll 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 carbon dioxide in a supercritical state, 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 A method for producing tobacco materials.

2. The S and P are determined under the following conditions: [conditions] 1) Weigh out 5 g of the impregnated tobacco raw material. 2) 100 ml of an aprotic solvent is placed in a container, and the impregnated tobacco raw material is placed therein. 3) After addition, shake the container and extract for 30 seconds. 4) The extract is filtered to obtain a filtrate. 5) Filter the extract obtained in 4). 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 solid dry matter, which is dissolved in the aprotic solvent to give a 4% solution and analyzed by GC / MS to obtain the S value. 8) The steps 1) to 7) are carried out on the tobacco raw material before impregnation to obtain the P value. The method of claim 1 .

3. The method according to claim 1 or 2, wherein the tobacco raw material is blended or unbleached tobacco leaves, lamina, midribs, stems, or shreds.

4. The method according to any one of claims 1 to 3, further comprising a step of pulverizing the tobacco raw material after the impregnation.

5. The manufacturing method according to any one of claims 1 to 4, wherein the tobacco material and the medium are not separated after the impregnation, and the tobacco material after separation is pulverized.

6. The method according to claim 5 , wherein the grinding is freeze-grinding.

7. A tobacco material obtained by the method according to claims 1 to 6.

8. 8. The tobacco material according to claim 7, having a D90 of 30 μm or less.

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