Bleached tobacco residue and its manufacturing method, regenerated tobacco material and its manufacturing method, and tobacco product

The method of treating tobacco residue with a peracetic acid-based bleaching solution and processing the extract to remove colored components addresses the issues of visible color and high NNK levels in tobacco products, resulting in a safer and more aesthetically pleasing tobacco residue for use in tobacco products.

JP7681726B2Active Publication Date: 2025-05-22JAPAN TOBACCO INC
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Patent Information

Application Number
JP2023568904
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Filing Date
2021-12-22
Publication Date
2025-05-22
Estimated Expiration
2041-12-22

AI Technical Summary

Technical Problem

Existing tobacco residue used in tobacco products may contain visible color components that seep into packaging and high levels of tobacco-specific nitrosamines (TSNAs), particularly NNK, which are harmful to health.

Method used

A method involving the treatment of tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to bleach the residue, thereby reducing NNK levels and achieving a whitened appearance. Additionally, water-soluble components are extracted, and the pH of the extract is adjusted to remove colored components using a reversed-phase adsorbent, resulting in a tobacco flavor liquid.

Benefits of technology

The method effectively reduces the content of NNK in tobacco residue, achieves a whitened appearance, and removes colored components, resulting in a tobacco product with improved safety and aesthetic qualities.

✦ Generated by Eureka AI based on patent content.

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Abstract

A production method for bleached tobacco residue, wherein tobacco residue is treated with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue.
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Description

[Technical field]

[0001] The present invention relates to bleached tobacco residue and its manufacturing method, reconstituted tobacco material and its manufacturing method, and tobacco products. [Background technology]

[0002] It has been reported that water-soluble components are extracted from tobacco materials such as tobacco leaves, and the obtained tobacco extract or tobacco residue is used as a flavor source for tobacco products. For example, it has been reported that sheet tobacco is prepared from tobacco residue, a tobacco extract is added to the sheet tobacco, and the obtained regenerated tobacco material is used as a flavor source for tobacco products such as cigarettes, oral cigarettes, and flavor inhalers (Patent Document 1).

[0003] When using regenerated tobacco materials as a flavor source for tobacco products, there is a possibility that the regenerated tobacco materials may be visible to users when, for example, replacing a cartridge that contains the regenerated tobacco materials, and that the color components in the regenerated tobacco materials may seep into the packaging material (e.g., paper or nonwoven fabric) that encases the regenerated tobacco materials. For this reason, in terms of appearance, it is preferable that the color of the regenerated tobacco materials is close to white.

[0004] On the other hand, it is known that tobacco-specific nitrosamines (TSNAs) are contained in mainstream cigarette smoke and tobacco vapor from heated inhalers. TSNAs are four compounds: 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), N'-nitrosonornicotine (NNN), N'-nitrosoanatabine (NAT), and N'-nitrosoanabasine (NAB).

[0005] It has been reported that TSNA contained in tobacco mainstream smoke is generated through three pathways (Non-Patent Documents 1 to 3). Specifically, the three pathways are a pathway in which TSNA contained in tobacco filler evaporates and migrates directly into the smoke, a pathway in which alkaloids in the tobacco filler are nitrosated using heat during combustion to synthesize TSNA, and a pathway in which NNK bound to lignin-like polymeric components is dissociated by heat during combustion and migrates into the smoke. NNK bound to lignin-like polymeric components in tobacco filler is called "bound NNK," and NNK that is free in the tobacco filler without being bound to lignin-like polymeric components is called "free NNK." [Prior art documents] [Patent documents]

[0006] [Patent Document 1] U.S. Patent No. 4,895,175 [Non-patent literature]

[0007] [Non-Patent Document 1] Hoffmann D. et al., “Origin in tobacco smoke of N'-nitrosonornicotine, a tobacco-specific carcinogen: Brief Communication”, J. Natl. Cancer Inst., Vol. 58(6), p. 1841-1844, 1977 [Non-Patent Document 2] Adams JD et al., “On the formation of the tobacco-specific carcinogen 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone during smoking”, Cancer Lett., Vol. 17(3), p. 339-346, 1983 [Non-Patent Document 3] Lipowicz PJ and Seeman JI, “A model to estimate the sources of tobacco-specific nitrosamines in cigarette smoke”, Chem. Res. Toxicol., Vol. 30(8), p. 1556-1561, 2017 Summary of the Invention [Problem to be solved by the invention]

[0008] The present invention aims to provide a technology relating to tobacco residue that has reduced levels of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (hereinafter also referred to as NNK), a type of tobacco-specific nitrosamine, and has been whitened. [Means for solving the problem]

[0009] According to one aspect, there is provided a method for producing bleached tobacco residue, comprising treating tobacco residue with an aqueous solution comprising peracetic acid, acetic acid, and hydrogen peroxide to bleach said tobacco residue. According to another aspect, there is provided a bleached tobacco residue obtainable by the aforementioned method.

[0010] According to yet another aspect, extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and a tobacco residue; treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to obtain a bleached tobacco residue; adjusting the pH of the tobacco extract to 4.1 or less to obtain an acidic tobacco extract; treating the acidic tobacco extract with a reversed phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid; mixing said bleached tobacco residue with said tobacco flavor liquid; A method for producing reconstituted tobacco material is provided, comprising: According to yet another aspect, there is provided a reconstituted tobacco material obtainable by the aforementioned method. According to yet another aspect, there is provided a tobacco product comprising the reconstituted tobacco material described above. Effect of the Invention

[0011] According to the present invention, there is provided a technology relating to tobacco residue in which the content of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), a type of tobacco-specific nitrosamine, is reduced and the tobacco residue is whitened. [Brief description of the drawings]

[0012] [Figure 1] FIG. 1 is a flow chart illustrating one example of a method for producing bleached tobacco residue and reconstituted tobacco material. [Diagram 2] FIG. 2 is a perspective view showing an example of a non-combustion heating type flavor inhaler. [Diagram 3] FIG. 3 is a cross-sectional view of a non-combustion heating type flavor inhalation article. [Figure 4] FIG. 4 is a diagram showing the internal structure of the aerosol generating device. [Diagram 5] FIG. 5 is a graph showing the relationship between bleach concentration and tobacco residue color. [Figure 6] FIG. 6 is a graph showing the relationship between bleach concentration and tobacco residue color. [Figure 7] FIG. 7 is a graph showing the relationship between reaction time and tobacco residue color. [Figure 8] FIG. 8 is a graph showing the relationship between the concentration of the bleaching solution and the amount of bound NNK. [Figure 9] FIG. 9 is a graph showing the relationship between the concentration of bleach in the bleaching solution and the amount of bound NNK. [Figure 10] FIG. 10 is a graph showing the relationship between reaction time and the amount of bound NNK. [Figure 11] FIG. 11 is a graph showing the relationship between the amount of bleaching solution relative to tobacco residue and the amount of bound NNK. [Figure 12]FIG. 12 is a graph showing the relationship between the concentration of the bleaching solution and the mass ratio of tobacco residue. [Figure 13] FIG. 13 is a graph showing the relationship between the concentration of the bleaching solution and the mass ratio of tobacco residue. [Figure 14] FIG. 14 is a graph showing the results of color analysis of tobacco flavor liquid. [Figure 15] FIG. 15 is a graph showing the relationship between the pH of an acidic tobacco extract and the nicotine content in a tobacco flavor liquid. [Figure 16] FIG. 16 is a graph showing the relationship between the ethanol concentration in an acidic tobacco extract and the benzaldehyde content in a tobacco flavor liquid. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0013] The present invention will be described in detail below. However, the following description is for the purpose of explaining the present invention and is not intended to limit the present invention.

[0014] <1. Manufacturing method of bleached tobacco residue> According to one embodiment, the method for producing bleached tobacco residue includes treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue. According to a preferred embodiment, the method for producing bleached tobacco residue further includes extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent prior to the bleaching treatment to prepare the tobacco residue.

[0015] That is, according to a preferred embodiment, a method for producing bleached tobacco residue comprises: (S1) extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco residue; (S2) treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to bleach the tobacco residue; Includes.

[0016] A method according to a preferred embodiment is shown in Figure 1. In addition to the "method of producing bleached tobacco residue", Figure 1 also shows the "method of producing reconstituted tobacco material".

[0017] The method according to the preferred embodiment will be described below in the order of the "extraction step (S1)" and the "bleaching step (S2)".

[0018] [Extraction process (S1)] In the extraction step (S1), water-soluble components contained in the tobacco material are extracted from the tobacco material with an aqueous solvent to obtain a tobacco residue. In the extraction step (S1), a tobacco extract is obtained at the same time as the tobacco residue (see FIG. 1).

[0019] The tobacco material may be tobacco shreds that are ready to be incorporated into tobacco products, such as combustion-type or heat-type flavor inhalers. "Tobacco shreds ready to be incorporated into tobacco products" refers to tobacco shreds that have been subjected to various processing steps, such as drying at the farm, a long-term aging process of one to several years at a raw material factory, and then blending and cutting at a manufacturing factory, and are ready to be incorporated into tobacco products.

[0020] Tobacco shreds are cut leaves of tobacco. Tobacco shreds may be shredded leaves, shredded backbones, shredded reconstituted tobacco (i.e., tobacco material produced by processing leaf waste, shredded waste, backbone waste, fine powder, etc., generated during the manufacturing process of a factory into a reusable form), or a mixture thereof. Tobacco shreds may be crushed to increase the extraction efficiency, and the resulting crushed material may be used for extraction.

[0021] The tobacco shreds may be of any variety, such as flue-cured, burley, orient, etc. The tobacco shreds may be of a single variety or a mixture of different varieties.

[0022] The aqueous solvent may be water or an aqueous ethanol solution with a concentration of 10% by mass or less. The aqueous solvent is generally water, and is preferably water at room temperature (e.g., about 20° C.) to 70° C. The aqueous solvent may be used in an amount of, for example, 500 to 5000% by mass relative to the tobacco material.

[0023] The extraction can be carried out, for example, by immersing the tobacco material in warm water at 40 to 60° C. for 30 to 180 minutes, or by shaking the tobacco material (eg, at 200 rpm) in warm water at 40 to 60° C. for 30 to 180 minutes.

[0024] The extraction may also be performed by repeating the extraction procedure several times. Specifically, the water-soluble components contained in the tobacco material are extracted from the tobacco material with an aqueous solvent, and then the obtained tobacco residue is placed in a new aqueous solvent to perform a second extraction procedure, and if necessary, the extraction procedure with the new aqueous solvent is further repeated.

[0025] The extraction produces a mixture of tobacco residue and tobacco extract. The tobacco extract contains water-soluble components contained in the tobacco material. Examples of "water-soluble components contained in the tobacco material" include components that contribute to tobacco flavor (e.g., organic acids, leaf surface resins, terpenoids, polyphenols, etc.).

[0026] After extraction, the tobacco residue and the tobacco extract are separated, and the tobacco extract can be used as a raw material for obtaining a tobacco flavor liquid. On the other hand, the tobacco residue can be mixed with the final tobacco flavor liquid, and the resulting mixture can be appropriately processed to prepare a tobacco filler (hereinafter also referred to as a reconstituted tobacco material). For example, the tobacco residue can be mixed with the final tobacco flavor liquid, and the resulting mixture can be used to prepare a tobacco molded product such as a sheet tobacco. Alternatively, the tobacco residue can be mixed with the final tobacco flavor liquid, and the resulting mixture can be dried and pulverized to prepare a tobacco powder.

[0027] [Bleaching process (S2)] In the bleaching step (S2), the tobacco residue obtained in the extraction step (S1) is treated with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue (see FIG. 1). This results in a bleached tobacco residue. In this specification, "bleached tobacco residue" refers to tobacco residue that has been subjected to a bleaching treatment. In other words, "bleached tobacco residue" only needs to have been subjected to a bleaching treatment, and does not need to have been completely changed to white by the bleaching treatment.

[0028] The bleaching step can be carried out by immersing the tobacco residue in an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide.

[0029] When an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide is used as a bleaching solution, the amount of peracetic acid consumed by the reaction between tobacco residue and peracetic acid can be compensated for by the peracetic acid produced by the reaction between acetic acid and hydrogen peroxide, and thus peracetic acid can be present in the reaction solution at a concentration equal to or higher than a predetermined concentration, thereby improving the bleaching efficiency of tobacco residue.

[0030] The concentration of peracetic acid in the aqueous solution is, for example, 0.015 to 10% by mass, preferably 0.15 to 1.5% by mass. The concentration of acetic acid in the aqueous solution is, for example, 0.04 to 4% by mass, preferably 0.4 to 4% by mass. The concentration of hydrogen peroxide in the aqueous solution is, for example, 0.0055 to 0.55% by mass, preferably 0.055 to 0.55% by mass.

[0031] The aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide may be a commercially available peracetic acid preparation. Preferably, a peracetic acid preparation approved as a food additive may be used. For example, Persan MP2-J (Kanto Chemical Co., Ltd.) may be used. Persan MP2-J is composed of 15% by mass of peracetic acid, 40% by mass of acetic acid, 5.5% by mass of hydrogen peroxide, less than 1% by mass of a stabilizer, and the remaining amount of water.

[0032] The bleaching step can be carried out by immersing the tobacco residue in a bleaching solution under conditions that allow the tobacco residue to be bleached. For example, the bleaching step can be carried out at a temperature of 22 to 100°C for 15 to 240 minutes. The bleaching step is preferably carried out while heating, for example, at a temperature of 40 to 100°C. By carrying out the bleaching step while heating, the bleaching effect of the tobacco residue can be enhanced, and the effect of reducing the amount of bound NNK in the tobacco residue can be enhanced.

[0033] In the bleaching step, the ratio (solid-liquid ratio) of the mass of the tobacco residue to the mass of the aqueous solution (bleaching solution) can be, for example, 1:30 to 1:100.

[0034] [effect] According to the above-mentioned method, the tobacco residue can be efficiently bleached and the amount of bound NNK in the tobacco residue can be reduced (see Examples 1 and 2 described below). Therefore, the above-mentioned method can produce a whitened tobacco residue that has an excellent appearance (i.e., a color desired by users when incorporated into a tobacco product) and contains a reduced amount of bound NNK. In this specification, the term "whitened" refers to the visual color of the tobacco residue being changed to a lighter color by the bleaching treatment. In other words, the term "whitened" includes not only the case where the tobacco residue is visually changed to a completely white color, but also the case where the tobacco residue is not visually changed to a completely white color.

[0035] <2. Manufacturing method of regenerated tobacco material> The bleached tobacco residue obtained in the above bleaching step (S2) can be combined with the decolorized tobacco extract to produce a whitened reconstituted tobacco material.

[0036] According to one embodiment, a method for producing reconstituted tobacco material comprises the steps of: adjusting the pH of the tobacco extract obtained in the extraction step (S1) to 4.1 or less to obtain an acidic tobacco extract; treating the acidic tobacco extract with a reversed-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid (i.e., a decolorized tobacco extract); Mixing the bleached tobacco residue obtained in the bleaching step (S2) with the tobacco flavor liquid. (See Figure 1).

[0037] That is, according to one embodiment, a method for producing regenerated tobacco material comprises: (S1) extracting water-soluble components contained in a tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and a tobacco residue; (S2) treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to obtain a bleached tobacco residue; (S3) adjusting the pH of the tobacco extract to 4.1 or less to obtain an acidic tobacco extract; (S4) treating the acidic tobacco extract with a reversed-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid (i.e., a decolorized tobacco extract); (S5) mixing the bleached tobacco residue with the tobacco flavor liquid; (See Figure 1).

[0038] In this specification, the liquid obtained by extracting water-soluble components from tobacco material is referred to as "tobacco extract," the solid obtained during this extraction is referred to as "tobacco residue," the liquid obtained by adjusting the pH of the tobacco extract to 4.1 or less is referred to as "acidic tobacco extract," and the liquid obtained by treating the acidic tobacco extract with a reversed-phase adsorbent is referred to as "tobacco flavor liquid."

[0039] The method according to this embodiment will be described below in the order of steps (S1) to (S5).

[0040] [Extraction process (S1) and bleaching process (S2)] The "extraction step (S1)" and the "bleaching step (S2)" can be carried out as described in the section <1. Production method of tobacco residue>.

[0041] [pH adjustment step (S3)] In the pH adjustment step (S3), the pH of the tobacco extract obtained in the extraction step (S1) is adjusted to 4.1 or less to obtain an acidic tobacco extract (see FIG. 1).

[0042] In the pH adjustment step (S3), the pH of the tobacco extract is adjusted to preferably within the range of 1 to 4.1, more preferably 2 to 3. The pH can be adjusted by adding a pH adjuster to the tobacco extract in an amount necessary to reach a desired pH in order to lower the pH of the tobacco extract. As the pH adjuster, for example, a weak acid such as phosphoric acid, citric acid, or acetic acid may be used, or a strong acid such as nitric acid, hydrochloric acid, or sulfuric acid may be used.

[0043] In this specification, pH refers to a value measured with a pH meter using a glass electrode according to the pH measurement method described in JIS Z 8802:2011, that is, a value obtained by using two electrodes, a glass electrode and a reference electrode, and measuring the potential difference generated between these two electrodes. As the pH meter, a commercially available pH meter based on the glass electrode method, such as LAQUA F-72 (HORIBA), can be used. The pH can be measured, for example, for a tobacco extract at 20°C. When the measured pH value is obtained to two decimal places or less, the two decimal places or less can be rounded off and the obtained value can be regarded as the pH value.

[0044] The acidic tobacco extract may be prepared to contain ethanol at a concentration of 10% by mass or less. Preferably, the acidic tobacco extract may be prepared to contain ethanol at a concentration of 1 to 10% by mass. That is, the preparation of the acidic tobacco extract may further include adding ethanol to the tobacco extract obtained in the extraction step (S1) or the tobacco extract adjusted to a pH of 4.1 or less, so that the final concentration is 10% by mass or less (preferably 1 to 10% by mass).

[0045] When the acidic tobacco extract contains ethanol at a concentration of 10% by mass or less, the tobacco flavor liquid obtained as the final product can contain a greater amount of tobacco flavor components while being colorless or nearly colorless (see Example 7 below).

[0046] [Treatment step with reversed-phase adsorbent (S4)] In the treatment step (S4), the acidic tobacco extract is treated with a reversed-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid (see FIG. 1).

[0047] The reversed-phase adsorbent can be any adsorbent used in reversed-phase solid-phase extraction. "Reversed-phase solid-phase extraction" refers to a method in which a polar solution or suspension (mobile phase) is passed through a non-polar solid (stationary phase) to adsorb hydrophobic components contained in the mobile phase to the stationary phase for separation.

[0048] Examples of reversed-phase adsorbents include adsorbents in which hydrophobic groups such as octadecylsilyl groups (ODS) are bonded to silica gel carrier particles, and adsorbents made of hydrophobic polymer particles such as styrene-divinylbenzene copolymers. Reverse-phase adsorbents are commercially available, and examples include InterSep C18 (GL Sciences Inc.) solid-phase extraction cartridges, Oasis HLB (Nihon Waters Inc.) solid-phase extraction cartridges, as well as synthetic adsorbents such as Diaion HP series (Mitsubishi Chemical Corporation) and Amberlite XAD series (Organo Corporation). Note that the reversed-phase adsorbents are not limited to those exemplified, and known adsorbents having the same separation mode as those exemplified can be used.

[0049] The treatment step (S4) may be carried out by passing the acidic tobacco extract through a solid phase consisting of a reversed-phase adsorbent, or by adding particles of the reversed-phase adsorbent to the acidic tobacco extract and then removing the particles of the reversed-phase adsorbent from the acidic tobacco extract by filtration or the like.

[0050] In a preferred embodiment, the processing step (S4) can be carried out by passing the acidic tobacco extract through a solid phase consisting of a reversed-phase adsorbent. In a more preferred embodiment, the processing step (S4) can be carried out by passing the acidic tobacco extract through a column packed with a reversed-phase adsorbent. The "reverse-phase adsorbent" can generally be composed of an aggregate of particles of the reversed-phase adsorbent.

[0051] By carrying out the treatment step (S4), it is possible to remove colored components and tobacco specific nitrosamines (TSNAs) from the tobacco extract without impairing the tobacco flavor components contained in the tobacco extract (see Examples 4 to 6 described below). For example, when the acidic tobacco extract is passed through a column packed with a reversed-phase adsorbent, the colored components and tobacco specific nitrosamines (TSNAs) contained in the tobacco extract can be adsorbed onto the column, and the tobacco flavor components contained in the tobacco extract can be eluted into the eluate.

[0052] Tobacco-specific nitrosamines (TSNAs) are nitrosamines that are specifically present in tobacco filler materials such as tobacco leaves and in cigarette smoke, and refer to the four components: 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), N'-nitrosonornicotine (NNN), N'-nitrosoanatabine (NAT), and N'-nitrosoanabasine (NAB).

[0053] [Mixing process (S5)] In the mixing step (S5), the bleached tobacco residue obtained in the bleaching step (S2) is mixed with the tobacco flavor liquid obtained in the treatment step (S4), thereby obtaining a reconstituted tobacco material (see FIG. 1).

[0054] The bleached tobacco residue may be molded into a specific form such as a sheet or granules to prepare a tobacco molded product such as a tobacco sheet or tobacco granules, and the obtained tobacco molded product may be mixed with a tobacco flavor liquid. The tobacco flavor liquid may also be concentrated to prepare a tobacco flavor liquid concentrate, and the obtained concentrate may be mixed with the tobacco residue or the tobacco molded product.

[0055] In the above embodiment, the bleached tobacco residue is mixed with the decolorized tobacco extract (i.e., tobacco flavor liquid) to produce a reconstituted tobacco material. The present invention is not limited to this embodiment, and the bleached tobacco residue may be mixed with the tobacco extract obtained in the extraction step (S1) to produce a reconstituted tobacco material.

[0056] [effect] According to the above-mentioned method, the tobacco residue can be efficiently bleached and the amount of bound NNK in the tobacco residue can be reduced (see Examples 1 and 2 described below). In addition, according to the above-mentioned method, colored components and tobacco specific nitrosamines (TSNAs) can be removed from the tobacco extract while maintaining the tobacco flavor components contained in the tobacco extract (see Examples 4 to 6 described below). Therefore, when a regenerated tobacco material is produced according to the above-mentioned method, it is possible to produce a regenerated tobacco material that is whitened and has an excellent appearance (i.e., a color desired by users when incorporated into a tobacco product), contains a sufficient amount of tobacco flavor components, but contains a reduced amount of tobacco specific nitrosamines (TSNAs).

[0057] <3. Bleached tobacco residue> According to another aspect, there is provided bleached tobacco residue obtainable by the above-mentioned "method for producing bleached tobacco residue."

[0058] As described above, bleached tobacco residue is whitened, has an excellent appearance, and contains a reduced amount of bound NNK. Therefore, when bleached tobacco residue is incorporated into a tobacco product, it can provide a desirable appearance to the user and provide a reduced amount of NNK to the user when using the tobacco product. As described in the Background Art section, the bound NNK in the tobacco residue is dissociated by heat and converted to free NNK, which is transferred into the smoke, so that the bleached tobacco residue can provide a reduced amount of NNK to the user, especially when heated by a heated flavor inhaler.

[0059] In addition, the bleached tobacco residue has a reduced mass compared to the tobacco residue prior to the bleaching process (see Example 3 below), and therefore, when the bleached tobacco residue is incorporated into a tobacco product, a greater amount of the tobacco residue can be incorporated into the tobacco product.

[0060] The bleached tobacco residue can be incorporated into tobacco products, such as flavor inhalers, according to known techniques. Examples of uses for the bleached tobacco residue are described below.

[0061] For example, bleached tobacco residue can be mixed with the tobacco flavor liquid obtained in the above-mentioned processing step (S4), the resulting mixture can be dried, and the resulting dried product can be used as a tobacco flavor source for tobacco products.

[0062] Alternatively, the bleached tobacco residue can be mixed with the tobacco flavor liquid obtained in the above-mentioned processing step (S4), and the resulting mixture can be used to produce tobacco molded bodies such as tobacco sheets or tobacco granules, which can then be used as a tobacco flavor source for tobacco products.

[0063] Alternatively, the bleached tobacco residue can be mixed with the tobacco flavor liquid obtained in the above-mentioned processing step (S4), the resulting mixture can be dried and ground to produce tobacco powder, the tobacco powder can be added to tobacco materials (e.g., deboned leaves or leaf tobacco), and the resulting mixture can be used as a tobacco flavor source in tobacco products.

[0064] Alternatively, the bleached tobacco residue can be mixed with the tobacco flavor liquid obtained in the above-mentioned processing step (S4), the resulting mixture can be dried and ground to produce tobacco powder, the tobacco powder can be suspended in water to prepare a tobacco slurry, the tobacco slurry can be added to tobacco materials (e.g., deboned leaves or leaf tobacco), and the resulting mixture can be used as a tobacco flavor source for tobacco products.

[0065] <4. Recycled tobacco materials> According to another aspect, there is provided a reconstituted tobacco material obtained by the above-mentioned "method for producing a reconstituted tobacco material".

[0066] As described above, the reconstituted tobacco material has a whitened and excellent appearance, contains a sufficient amount of tobacco flavor components, but contains a reduced amount of tobacco specific nitrosamines (TSNAs), and thus, when incorporated into a tobacco product, the reconstituted tobacco material can provide a desirable appearance to the user, and can provide a sufficient amount of tobacco flavor components and a reduced amount of tobacco specific nitrosamines (TSNAs) to the user during use of the tobacco product.

[0067] In addition, the bleached tobacco residue contained in the reconstituted tobacco material has a reduced mass compared to the tobacco residue before the bleaching treatment (see Example 3 below). Therefore, when the reconstituted tobacco material is incorporated into a tobacco product, a greater amount of the reconstituted tobacco material can be incorporated into the tobacco product.

[0068] Specific examples of reconstituted tobacco materials are described below. For example, the reconstituted tobacco material may be a product obtained by drying a mixture of the bleached tobacco residue obtained in the above bleaching step (S2) and the tobacco flavor liquid obtained in the above treatment step (S4), which can be used as a tobacco flavor source for tobacco products.

[0069] Alternatively, the regenerated tobacco material may be a tobacco molded product obtained by molding a mixture of the bleached tobacco residue obtained in the above bleaching step (S2) and the tobacco flavor liquid obtained in the above treatment step (S4) into a specific shape such as a sheet shape or a granular shape. The tobacco molded product can be used as a tobacco flavor source for tobacco products.

[0070] Alternatively, the regenerated tobacco material may be tobacco powder obtained by drying a mixture of the bleached tobacco residue obtained in the bleaching step (S2) and the tobacco flavor liquid obtained in the treatment step (S4) and grinding it into a powder form. The tobacco powder can be added to tobacco materials (e.g., deboned leaves or tobacco leaves) to enhance the flavor of the tobacco materials. The flavor-enhanced tobacco materials can be used as a tobacco flavor source for tobacco products.

[0071] Alternatively, the regenerated tobacco material may be a tobacco slurry obtained by drying a mixture of the bleached tobacco residue obtained in the above bleaching step (S2) and the tobacco flavor liquid obtained in the above treatment step (S4), grinding the mixture into a powder, and suspending the obtained powder in water. The tobacco slurry can be added to a tobacco material (e.g., deboned leaves or tobacco leaves) to enhance the flavor of the tobacco material. The flavor-enhanced tobacco material can be used as a tobacco flavor source for tobacco products.

[0072] The reconstituted tobacco material may contain additives such as binders, pH adjusters, preservatives, and antioxidants, as necessary.

[0073] <5. Tobacco products> The above-mentioned "reconstituted tobacco material" can be incorporated into any tobacco product. That is, according to another aspect, a tobacco product containing the above-mentioned "reconstituted tobacco material" is provided. The tobacco product includes a combustion-type flavor inhaler, a heating-type flavor inhaler, a non-heating-type flavor inhaler, and a smokeless tobacco.

[0074] A "combustion type flavor inhaler" is a flavor inhaler that provides a user with tobacco flavor by burning a tobacco filler (such as tobacco shreds or a molded tobacco body). Examples of combustion type flavor inhalers include cigarettes, pipes, kiseru, cigars, and cigarillos.

[0075] A "heated flavor inhaler" is a flavor inhaler that provides a tobacco flavor to a user by heating a tobacco filler without burning it. Examples of heated flavor inhalers include: A carbon heat source type flavor inhaler that heats tobacco filler with the combustion heat of a carbon heat source (see, for example, WO2006 / 073065); An electrically heated flavour inhaler comprising a tobacco stick containing a tobacco filler and a heating device for electrically heating the tobacco stick (see, for example, WO2010 / 110226); or A liquid atomization type flavor inhaler that generates an aerosol by heating a liquid aerosol source with a heater and inhales flavor derived from a tobacco filler together with the aerosol (see, for example, WO2015 / 046385) etc.

[0076] A "non-heating flavor inhaler" is a flavor inhaler that provides a tobacco flavor to a user without burning or heating a tobacco filler. An example of a non-heating flavor inhaler is a non-heating tobacco flavor inhaler that includes an inhaler body having an air flow passage that allows air to flow by inhalation, and tobacco flavor-releasing granules arranged in the air flow passage (see, for example, WO2012 / 023515).

[0077] "Smokeless tobacco" is a product that allows users to enjoy tobacco flavor by inhaling the product directly into the nasal or oral cavity. The former are called nasal tobacco products, and the latter are called oral tobacco products. An example of the former is snuff, and an example of the latter is chewing tobacco.

[0078] (Typical examples of tobacco products) According to a representative example, the above-mentioned "regenerated tobacco material" can be incorporated into a heated flavor inhaler. That is, according to a representative example, a heated flavor inhaler containing the above-mentioned "regenerated tobacco material" is provided. The heated flavor inhaler may further include a heater for heating the tobacco filler containing the regenerated tobacco material.

[0079] Alternatively, according to a representative example, the above-mentioned "reconstituted tobacco material" can be incorporated into an oral tobacco product. That is, according to a representative example, an oral tobacco product containing the above-mentioned "reconstituted tobacco material" is provided. The oral tobacco product may further include a liquid-permeable wrapping material (e.g., a nonwoven pouch) that wraps the tobacco filler material containing the reconstituted tobacco material. Specifically, the oral tobacco product may have a teabag shape in which a tobacco flavor source is wrapped in a nonwoven pouch.

[0080] (Example of a heated flavor inhaler) An example of a heated flavor inhaler containing the above-mentioned "regenerated tobacco material" will be described below with reference to Figs. 2 to 4. Fig. 2 is a perspective view showing an example of a non-combustion heated flavor inhaler. Fig. 3 is a cross-sectional view of a non-combustion heated flavor inhalation article. Fig. 4 is a diagram showing the internal structure of an aerosol generating device.

[0081] As shown in FIG. 2, the flavor inhaler 100 includes: A flavor inhalation article 110 comprising the above-mentioned "reconstituted tobacco material" and an aerosol source; an aerosol generating device 120 that heats the flavor inhalation article 110 to atomize the aerosol source and release flavor components from the regenerated tobacco material; It is equipped with:

[0082] The flavor inhalation article 110 is a replaceable cartridge and has a columnar shape extending in one direction. The flavor inhalation article 110 is configured to generate an aerosol containing a flavor component by being heated while being inserted into the aerosol generating device 120.

[0083] 3, the flavor inhalation article 110 has a base member 110A that forms one end of the flavor inhalation article 110 and includes a filling material 111 and a first wrapping paper 112 that wraps the filling material 111, and a mouthpiece 110B that forms the end opposite to the base member 110A. The base member 110A and the mouthpiece 110B are connected by a second wrapping paper 113.

[0084] The suction mouth part 110B has a cardboard tube part 114 and a filter 118 adjacent thereto. The filter 118 has a filter plug 115, a hollow plug 116, and a formed paper 117 that covers and connects these. The cardboard tube part 114 is a cardboard tube formed by rolling paper into a cylindrical shape, and is hollow inside. The hollow plug 116 is disposed adjacent to the cardboard tube part 114, and the filter plug 115 is disposed at the end of the suction mouth part 110B.

[0085] The filter plug 115 includes a filter medium 102 such as acetate tow, and a first plug wrapping paper 101 around which the filter medium 102 is wound.

[0086] The hollow plug 116 includes a packed layer 104 and a second plug wrapping paper 103 that wraps the packed layer 104. The packed layer 104 is made of densely packed fibers and has one or more channels (hollow portions). Each of the one or more channels extends in the length direction (hereinafter referred to as the longitudinal direction) of the flavor inhalation article 110. Therefore, during inhalation, air and aerosol flow only through the channels and hardly flow through the gaps between the fibers. In the flavor inhalation article 110, when it is desired to reduce the loss of aerosol components due to filtration by the filter plug 115, shortening the length of the filter plug 115 and replacing it with the hollow plug 116 is effective in increasing the amount of aerosol delivered.

[0087] The filter 118 may be composed of two plugs, three or more plugs, or only one plug, as shown in Fig. 3. For example, the filter 118 may omit the hollow plug 116 and be composed of only the filter plug 115. That is, the filter plug 115 and the cardboard tube portion 114 may be disposed adjacent to each other to form the suction mouth portion 110B.

[0088] The suction mouth portion 110B is composed of two segments, a paper tube portion 114 and a filter 118, but the suction mouth portion 110B may be composed of one segment, or may be composed of three or more segments.

[0089] Although not shown in the figure, the suction port portion 110B may be provided with an opening to take in air from the outside in order to appropriately adjust the airflow resistance of the flavor inhalation article 110. In this case, it is preferable to provide the cardboard tube portion 114 with an opening.

[0090] The longitudinal dimension, i.e., the length, of the flavor inhalation article 110 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 flavor inhalation article 110 is preferably 15 to 25 mm, more preferably 17 to 24 mm, and even more preferably 20 to 23 mm. In the flavor inhalation article 110, the length of the base material portion 110A may be 20 mm, the length of the cardboard tube portion 114 may be 20 mm, the length of the hollow plug 116 may be 8 mm, and the length of the filter plug 115 may be 7 mm, but the lengths of these individual segments can be appropriately changed depending on the manufacturing suitability, the required quality, and the like.

[0091] Filler 111 includes the above-mentioned "reconstituted tobacco material" and an aerosol source. From the viewpoint of the effects of the invention, it is preferable that filler 111 is composed only of the above-mentioned "reconstituted tobacco material" and an aerosol source. However, as long as the effects of the invention are achieved, filler 111 may also include tobacco filler materials other than the above-mentioned "reconstituted tobacco material."

[0092] The aerosol source is heated to a predetermined temperature to generate vapor. Examples of the aerosol source include glycerin, propylene glycol, triacetin, 1,3-butanediol, and mixtures thereof. The aerosol source can be included in an amount of, for example, 15 to 19% by mass based on the total tobacco filler included in the filling 111.

[0093] When the base portion 110A has a perimeter of 22 mm and a length of 20 mm, the content of the filling material 111 in the flavor inhalation article 110 is, for example, 200 to 400 mg, and preferably 250 to 320 mg.

[0094] The first wrapping paper 112 and the second wrapping paper 113 may be the same as the wrapping paper and the tipping paper used in cigarettes, respectively. The first plug wrapping paper 101, the second plug wrapping paper 103, and the forming paper 117 may be the same as the plug wrapping paper and the forming paper used in cigarettes.

[0095] 4, the aerosol generation device 120 has an insertion hole 130 into which the flavor inhalation article 110 can be inserted. That is, the aerosol generation device 120 has an inner cylindrical member 132 that constitutes the insertion hole 130. The inner cylindrical member 132 may be made of a thermally conductive material such as aluminum or stainless steel (SUS).

[0096] The aerosol generating device 120 may have a lid portion 140 that closes the insertion hole 130. The lid portion 140 is slidable, and can change its state between a state in which the insertion hole 130 is closed and a state in which the insertion hole 130 is exposed (see FIG. 2).

[0097] The aerosol generating device 120 may have an air flow path 160 that communicates with the insertion hole 130. One end of the air flow path 160 is connected to the insertion hole 130, and the other end of the air flow path 160 communicates with the outside of the aerosol generating device 120 (outside air) at a location separate from the insertion hole 130.

[0098] The aerosol generating device 120 may have a lid 170 that covers the end of the air flow path 160 that communicates with the outside air. The lid 170 may cover the end of the air flow path 160 that communicates with the outside air, or may leave this end exposed.

[0099] Here, the lid 170 covers the end of the air flow path 160, but does not airtightly close the air flow path 160. In other words, the lid 170 covers the air flow path 160, but is spaced from the end of the air flow path 160, and is configured to allow outside air to flow into the air flow path 160 through the gap therebetween.

[0100] With the flavor inhalation article 110 inserted into the aerosol generating device 120, the user holds one end of the flavor inhaler 110, specifically, the mouthpiece portion 110B shown in Fig. 3, in his / her mouth and performs an inhalation action. When the user inhales, outside air flows into the air flow path 160. The air that flows into the air flow path 160 passes through the flavor inhalation article 110 in the insertion hole 130 and is guided into the user's oral cavity.

[0101] The aerosol generating device 120 may have a temperature sensor in the air flow path 160 or on the outer surface of the wall portion constituting the air flow path 160. The temperature sensor may be, for example, a thermistor or a thermocouple. When a user inhales through the mouthpiece portion 110B of the flavor inhalation article 110, the internal temperature of the air flow path 160 or the temperature of the wall portion constituting the air flow path 160 decreases due to the influence of air flowing through the air flow path 160 from the lid portion 170 side toward the heater 30 side described later. The temperature sensor can detect the inhalation action of the user by measuring this temperature decrease.

[0102] The aerosol generating device 120 includes a battery 10, a control unit 20, and a heater 30. The battery 10 stores power used in the aerosol generating device 120. The battery 10 may be a chargeable and dischargeable secondary battery. The battery 10 may be, for example, a lithium ion battery.

[0103] The heater 30 may be provided around the inner tubular member 132. The space accommodating the heater 30 and the space accommodating the battery 10 may be separated from each other by a partition wall 180. This makes it possible to prevent air heated by the heater 30 from flowing into the space accommodating the battery 10. Therefore, it is possible to suppress a rise in temperature of the battery 10.

[0104] The heater 30 is preferably in a cylindrical shape capable of heating the outer periphery of the columnar flavor inhalation article 110. The heater 30 may be, for example, a film heater. The film heater may have a pair of film-like substrates and a resistance heating element sandwiched between the pair of substrates. The film-like substrate is preferably made of a material having excellent heat resistance and electrical insulation properties, and is typically made of polyimide. The resistance heating element is preferably made of one or more metal materials such as copper, nickel alloy, chromium alloy, stainless steel, platinum-rhodium, etc., and may be formed, for example, by a stainless steel base material. Furthermore, the resistance heating element may be copper-plated at the connection portion and its lead portion in order to connect to a power source via a flexible printed circuit (FPC).

[0105] Preferably, a heat shrink tube is provided on the outside of the heater 30. The heat shrink tube is a tube that shrinks in the radial direction by heat, and is made of, for example, a thermoplastic elastomer. The heater 30 is pressed against the inner cylindrical member 132 by the shrinking action of the heat shrink tube. This increases the adhesion between the heater 30 and the inner cylindrical member 132, thereby increasing the thermal conductivity from the heater 30 to the flavor inhalation article 110 via the inner cylindrical member 132.

[0106] The aerosol generating device 120 may have a cylindrical insulating material on the radial outside of the heater 30, preferably on the outside of the heat shrink tube. The insulating material can prevent the outer surface of the housing of the aerosol generating device 120 from reaching an excessively high temperature by blocking the heat of the heater 30. The insulating material can be made of aerogels such as silica aerogel, carbon aerogel, and alumina aerogel. The aerogel as the insulating material may typically be silica aerogel, which has high insulating performance and relatively low manufacturing costs. However, the insulating material may be a fiber-based insulating material such as glass wool or rock wool, or a foam-based insulating material such as urethane foam or phenol foam. Alternatively, the insulating material may be a vacuum insulating material.

[0107] An outer cylindrical member 134 is provided on the outside of the thermal insulation material. The thermal insulation material may be provided between the inner cylindrical member 132 facing the flavor inhalation article 110 and the outer cylindrical member 134. The outer cylindrical member 134 may be made of a thermally conductive material such as aluminum or stainless steel (SUS). The thermal insulation material is preferably provided in a sealed space.

[0108] The control unit 20 may include a circuit board, a central processing unit (CPU), a memory, etc. The aerosol generating device 120 may also have a notification unit for notifying the user of various information under the control of the control unit 20. The notification unit may be, for example, a light-emitting element such as a light-emitting diode (LED), a vibration element, or a combination of these.

[0109] When the control unit 20 detects a start-up request from the user, it starts supplying power from the battery 10 to the heater 30. The start-up request from the user is made, for example, by the user operating a push button or a slide switch, or by the user's inhalation action. The start-up request from the user may be made by pressing the push button 150. More specifically, the start-up request from the user may be made by pressing the push button 150 with the lid 140 open. Alternatively, the start-up request from the user may be made by detecting the user's inhalation action. The user's inhalation action can be detected, for example, by a temperature sensor as described above.

[0110] <6. Preferred embodiment> Preferred embodiments are summarized below.

[0111] [A1] A method for producing bleached tobacco residue, comprising treating tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to bleach said tobacco residue. [A2] The method according to [A1], further comprising extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent prior to the treatment, to prepare the tobacco residue. [A3] The method according to [A2], wherein the aqueous solvent is water. [A4] The method according to [A2], wherein the aqueous solvent is an aqueous ethanol solution having a concentration of 10% by mass or less.

[0112] [A5] The method according to any one of [A1] to [A4], wherein the treatment is carried out by immersing the tobacco residue in the aqueous solution. [A6] The method according to any one of [A1] to [A5], wherein the concentration of peracetic acid in the aqueous solution is 0.015 to 10% by mass, preferably 0.15 to 1.5% by mass. [A7] The method according to any one of [A1] to [A6], wherein the concentration of acetic acid in the aqueous solution is 0.04 to 4 mass%, preferably 0.4 to 4 mass%. [A8] The method according to any one of [A1] to [A7], wherein the concentration of hydrogen peroxide in the aqueous solution is 0.0055 to 0.55 mass %, preferably 0.055 to 0.55 mass %.

[0113] [A9] The method according to any one of [A1] to [A8], wherein the treatment is carried out at a temperature of 22 to 100°C. [A10] The method according to any one of [A1] to [A9], wherein the treatment is carried out at a temperature of 40 to 100°C. [A11] The method according to any one of [A1] to [A10], wherein the treatment is carried out for 15 to 240 minutes. [A12] The method according to any one of [A1] to [A11], wherein the ratio of the mass of the tobacco residue to the mass of the aqueous solution is 1:30 to 1:100. [B1] Bleached tobacco residue obtained by the method according to any one of [A1] to [A12].

[0114] [C1] extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and a tobacco residue; treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to obtain a bleached tobacco residue; adjusting the pH of the tobacco extract to 4.1 or less to obtain an acidic tobacco extract; treating the acidic tobacco extract with a reversed phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid; mixing said bleached tobacco residue with said tobacco flavor liquid; A method for producing a reconstituted tobacco material, comprising: [C2] The method according to [C1], wherein the aqueous solvent is water. [C3] The method according to [C1], wherein the aqueous solvent is an aqueous ethanol solution having a concentration of 10% by mass or less.

[0115] [C4] The method according to any one of [C1] to [C3], wherein the treatment with the aqueous solution is carried out by immersing the tobacco residue in the aqueous solution. [C5] The method according to any one of [C1] to [C4], wherein the concentration of peracetic acid in the aqueous solution is 0.015 to 10% by mass, preferably 0.15 to 1.5% by mass. [C6] The method according to any one of [C1] to [C5], wherein the concentration of acetic acid in the aqueous solution is 0.04 to 4 mass %, preferably 0.4 to 4 mass %. [C7] The method according to any one of [C1] to [C6], wherein the concentration of hydrogen peroxide in the aqueous solution is 0.0055 to 0.55 mass %, preferably 0.055 to 0.55 mass %.

[0116] [C8] The method according to any one of [C1] to [C7], wherein the treatment with the aqueous solution is carried out at a temperature of 22 to 100°C. [C9] The method according to any one of [C1] to [C8], wherein the treatment with the aqueous solution is carried out at a temperature of 40 to 100°C. [C10] The method according to any one of [C1] to [C9], wherein the treatment with the aqueous solution is carried out for 15 to 240 minutes. [C11] The method according to any one of [C1] to [C10], wherein the ratio of the mass of the tobacco residue to the mass of the aqueous solution is 1:30 to 1:100.

[0117] [C12] The method according to any one of [C1] to [C11], wherein the treatment with the reversed-phase adsorbent is carried out by passing the acidic tobacco extract through a solid phase consisting of the reversed-phase adsorbent. [C13] The method according to any one of [C1] to [C12], wherein the treatment with the reversed phase adsorbent is carried out by passing the acidic tobacco extract through a column packed with the reversed phase adsorbent. [C14] The method according to any one of [C1] to [C13], wherein the pH of the tobacco extract is adjusted to 1 to 4.1, preferably 2 to 3. [C15] The method according to any one of [C1] to [C14], wherein obtaining the acidic tobacco extract further comprises adding ethanol to the tobacco extract or to the tobacco extract adjusted to a pH of 4.1 or less so that the final concentration is 10 mass% or less.

[0118] [D1] A regenerated tobacco material obtained by the method according to any one of [C1] to [C15]. [D2] The regenerated tobacco material according to [D1], wherein the regenerated tobacco material is a tobacco molded product obtained by molding a material containing the bleached tobacco residue and the tobacco flavor liquid. [D3] The regenerated tobacco material according to [D2], wherein the tobacco molded product is a tobacco sheet or tobacco granules.

[0119] [E1] A tobacco product comprising the reconstituted tobacco material according to any one of [D1] to [D3]. [E2] A heated flavor inhaler comprising the regenerated tobacco material according to any one of [D1] to [D3]. [E3] The heated flavor inhaler according to [E2], further comprising a heating device for heating the regenerated tobacco material. [E4] A flavor inhalation article comprising the reconstituted tobacco material and an aerosol source; a heating device for heating the flavor inhalation article to atomize the aerosol source and release flavor components from the regenerated tobacco material; The heated flavor inhaler according to [E2],

[0120] [E5] An oral tobacco product comprising the regenerated tobacco material according to any one of [D1] to [D3]. [E6] An oral tobacco product according to [E5], further comprising a liquid-permeable wrapping material that encases the regenerated tobacco material. EXAMPLES

[0121] [Example 1] In Example 1, a color analysis of bleached tobacco residue was performed.

[0122] 1-1. Preparation of bleached tobacco residue 40 mL of distilled water was added to 1 g of Burley tobacco material, and extraction was performed by shaking for 1 hour. After that, the mixture was centrifuged (3000 rpm, 5 minutes), and the supernatant was filtered through a 0.45 μm membrane filter. The same procedure was repeated twice to recover the extraction residue (tobacco residue). The obtained tobacco residue was immersed in an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide for bleaching. A diluted solution of Persun MP2-J (Kanto Chemical Co., Ltd.) was used as the aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide. This resulted in the production of bleached tobacco residue.

[0123] Persan MP2-J is an aqueous solution containing 15% by weight peracetic acid, 40% by weight acetic acid, and 5.5% by weight hydrogen peroxide.

[0124] In the comparative example, bleached tobacco residue was obtained in the same manner as above, except that hydrogen peroxide was used as the bleaching solution.

[0125] 1-2.Analysis method The bleached tobacco residue was subjected to color analysis. Color measurements were performed using a colorimeter (Konica Minolta, CM-5) and analysis software (Konica Minolta, Spectra Magic DX), and the color was quantified using the L*a*b* color system. The bleached tobacco residue was freeze-dried, and the resulting tobacco residue was filled into a glass container with a transparent bottom and measured using the reflection method. The color difference (ΔE*ab) was calculated using the following formula.

[0126]

number

[0127] 1-3.Results The results of the color analysis are shown in Figures 5 to 7.

[0128] FIG. 5 shows the results of an example of the present invention, and FIG. 6 shows the results of a comparative example. In FIGS. 5 and 6, the horizontal axis indicates the concentration of the bleaching solution (the concentration of Persan MP2-J or the concentration of hydrogen peroxide solution), and the vertical axis indicates the color difference. In FIGS. 5 and 6, the open circles indicate the results when the reaction temperature was 22° C., and the closed circles indicate the results when the reaction temperature was 60° C. In the experiments in FIGS. 5 and 6, a reaction time of 120 minutes was used.

[0129] In the examples of the present invention, 10% by mass of Persan MP2-J (aqueous solution containing 1.5% by mass of peracetic acid, 4% by mass of acetic acid, and 0.55% by mass of hydrogen peroxide), 1% by mass of Persan MP2-J (aqueous solution containing 0.15% by mass of peracetic acid, 0.4% by mass of acetic acid, and 0.055% by mass of hydrogen peroxide), and 0.1% by mass of Persan MP2-J (aqueous solution containing 0.015% by mass of peracetic acid, 0.04% by mass of acetic acid, and 0.0055% by mass of hydrogen peroxide) were used as three types of bleaching solutions. On the other hand, in the comparative examples, 10% by mass of hydrogen peroxide, 1% by mass of hydrogen peroxide, and 0.1% by mass of hydrogen peroxide were used as three types of bleaching solutions.

[0130] The example of the present invention (FIG. 5) has a lower concentration of bleaching agent in the bleaching solution compared to the comparative example (FIG. 6). Taking this into consideration, comparing the results of FIG. 5 and FIG. 6, it can be seen that when an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide is used as the bleaching solution, the bleaching efficiency is higher and tobacco residue with a color closer to white is obtained compared to when hydrogen peroxide water is used.

[0131] In addition, the results in Figure 5 show that the bleaching efficiency can be increased by using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and by heating the bleaching process. It is considered that the bleaching reaction temperature should be about 55°C to 100°C.

[0132] Figure 7 shows the results of an example of the present invention. In Figure 7, the horizontal axis represents the reaction time, and the vertical axis represents the color difference. In the experiment of Figure 7, 10% by mass of Percarbon MP2-J was used as the bleaching solution, and a reaction temperature of 60°C was adopted.

[0133] The results of Figure 7 show that a tobacco residue having a color closer to white can be obtained with a reaction time of 15 minutes. From this result, it is considered that the reaction time can be, for example, in the range of 15 minutes to 240 minutes.

[0134] [Example 2] In Example 2, the amount of bound NNK in the bleached tobacco residue was analyzed.

[0135] 2-1. Method According to the method described in Example 1, a bleached tobacco residue was prepared, and the amount of bound NNK in the bleached tobacco residue was analyzed. The analysis was performed by releasing the bound NNK in the tobacco residue. Specifically, 3 mL of water was added to 30 mg of the bleached tobacco residue, and it was heated at 160°C for 2 hours in a sealed container. After cooling, the liquid portion (containing NNK released from the bound NNK) was subjected to LC-MS-MS analysis.

[0136] 2-2. Results The analysis results of the amount of bound NNK are shown in Figures 8 to 11.

[0137] Figure 8 shows the results of an example of the present invention, and Figure 9 shows the results of an example of the present invention and a comparative example. In Figure 8, the horizontal axis represents the concentration of the bleaching solution (concentration of Percarbon MP2-J), and the vertical axis represents the amount of bound NNK as a relative value. In Figure 8, white circles show the results when the reaction temperature is 22°C, and black circles show the results when the reaction temperature is 60°C. In Figure 9, the horizontal axis represents the concentration of the bleaching agent in the bleaching solution (concentration of peracetic acid in Percarbon MP2-J or concentration of hydrogen peroxide in hydrogen peroxide water), and the vertical axis represents the amount of bound NNK as a relative value. In Figure 9, white circles show the results of the comparative example, and black circles show the results of an example of the present invention. In the experiments of Figures 8 and 9, a reaction time of 120 minutes was adopted.

[0138] The results in Fig. 8 show that the amount of bound NNK in tobacco residue can be reduced by bleaching tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide. The results in Fig. 8 and Fig. 9 also show that when an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide is used as a bleaching solution, the effect of reducing bound NNK is greater than when hydrogen peroxide is used, and thus tobacco residue containing a reduced amount of bound NNK is obtained.

[0139] In addition, the results of Figure 8 show that the effect of reducing bound NNK can be enhanced by using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and heating the bleaching process. The bleaching reaction temperature is thought to be about 55°C to 100°C.

[0140] Figure 10 shows the results of the example of the present invention. In Figure 10, the horizontal axis shows the reaction time, and the vertical axis shows the amount of bound NNK in relative values. In the experiment of Figure 10, 10% by mass of Persan MP2-J was used as the bleaching solution, and the reaction temperature was 60°C.

[0141] The results in Figure 10 show that the amount of bound NNK in tobacco residue can be reduced by performing bleaching treatment with 10% by mass of Persan MP2-J for 15 minutes or more. The reaction time can be, for example, within the range of 15 to 240 minutes.

[0142] Figure 11 shows the results of the example of the present invention. In Figure 11, the horizontal axis shows the amount of bleaching solution relative to the tobacco residue (solid-liquid ratio), and the vertical axis shows the amount of bound NNK in relative values. In the experiment of Figure 11, 10 mass% Persan MP2-J was used as the bleaching solution, and a reaction temperature of 60°C and a reaction time of 30 minutes were used.

[0143] The results in Figure 11 show that a particularly high NNK reduction effect is achieved when the bleaching solution is used in an amount of 5 mL or more per 150 mg of tobacco residue, resulting in tobacco residue with reduced NNK. From these results, it is considered that it is particularly preferable to use a bleaching solution in an amount of 5 mL or more per 150 mg of tobacco residue.

[0144] [Example 3] In Example 3, the mass of bleached tobacco residue was measured.

[0145] 3-1. Method According to the method described in Example 1, a bleached tobacco residue was prepared, and the mass of the bleached tobacco residue was measured.

[0146] 3-2.Results The results of measuring the mass of tobacco residue are shown in Figures 12 and 13.

[0147] FIG. 12 shows the results of an example of the present invention, and FIG. 13 shows the results of a comparative example. In FIG. 12 and FIG. 13, the horizontal axis shows the concentration of the bleaching solution (the concentration of Persan MP2-J or the concentration of hydrogen peroxide solution), and the vertical axis shows the ratio of the mass of the bleached tobacco residue to the mass of the tobacco residue before bleaching. In FIG. 12 and FIG. 13, the open circles show the results when the reaction temperature is 22° C., and the closed circles show the results when the reaction temperature is 60° C. In the experiments in FIG. 12 and FIG. 13, a reaction time of 120 minutes was adopted.

[0148] As described in Example 1, the example of the present invention (FIG. 12) has a lower concentration of bleaching agent in the bleaching solution compared to the comparative example (FIG. 13). Taking this into consideration, comparing the results of FIG. 12 and FIG. 13, it can be seen that when an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide is used as the bleaching solution, the tobacco residue mass reduction effect is higher and tobacco residue with a smaller mass is obtained compared to when hydrogen peroxide water is used.

[0149] In addition, the results in Fig. 12 show that the effect of reducing the mass of tobacco residue can be enhanced by using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and by heating the bleaching process. It is considered that the bleaching reaction temperature should be around 55℃ to 100℃.

[0150] [Example 4] In Example 4, a color analysis of the tobacco flavor liquid was carried out.

[0151] 4-1. Preparation of tobacco flavor liquid 751 g of Burley tobacco material was extracted with hot water at 60°C. Then, an aqueous phosphoric acid solution adjusted to a specified pH was added, and the material was immersed for 30 minutes while stirring, and then subjected to shaking extraction for 1 hour. After that, the material was centrifuged (3000 rpm, 5 minutes), and the supernatant was squeeze-filtered through a 0.45 μm membrane filter to separate the filtrate (tobacco extract) and the extraction residue (tobacco residue).

[0152] Phosphoric acid, potassium hydroxide, and sodium sulfate were added to 0.5 mL of the tobacco extract to adjust the pH to various values. A LAQUA F-72 (HORIBA) pH meter was used. The potassium hydroxide and sodium sulfate aqueous solutions were added for the purpose of flavor component analysis (GC-MS analysis) described later.

[0153] Each of the pH-adjusted solutions (acidic tobacco extracts) was passed through a reversed-phase solid-phase extraction column (Oasis-HLB), which yielded a tobacco flavor solution.

[0154] 4-2.Analysis method The tobacco flavor liquid was diluted 10-fold, and the diluted liquid was subjected to absorbance analysis. As a control, the extract (acid tobacco extract) before passing through the column was also subjected to absorbance analysis.

[0155] 4-3.Results The results of the absorbance analysis are shown in FIG.

[0156] [Table 1]

[0157] Figure 14 shows the analysis results of the tobacco flavor liquid obtained from the acidic tobacco extract of pH 2.2. Table 1 shows the analysis results of the tobacco flavor liquid obtained from the acidic tobacco extract having various pH. In Table 1, an absorbance of about 0.1 or less indicates that the tobacco flavor liquid has a desirable colorlessness.

[0158] The results in Figure 14 show that the acidic tobacco extract is colored, but the tobacco flavor liquid is colorless because the colored components have been removed. The results in Table 1 show that the tobacco flavor liquid obtained from the acidic tobacco extract with a pH of 5.6 or less is colorless because the colored components have been removed.

[0159] [Example 5] In Example 5, the flavor components in the tobacco flavor liquid were analyzed.

[0160] 5-1. Method A tobacco flavor liquid was prepared according to the method described in Example 4, and the tobacco flavor liquid was subjected to GC-MS analysis. The tobacco flavor liquid was prepared from an acidic tobacco extract having a pH of 0.9 to 5.3. The amounts of flavor components, nicotine, myosmine, anabasine, nicotyrine, anatabine, and dipyridyl, were analyzed.

[0161] 5-2.Results The analysis results of nicotine are shown in Figure 15. Figure 15 is a graph showing the relationship between the pH of the acidic tobacco extract and the nicotine content in the tobacco flavor liquid.

[0162] The results in Figure 15 show that when a tobacco flavor liquid is prepared from an acidic tobacco extract adjusted to a pH of 4.1 or less, nicotine is hardly removed from the acidic tobacco extract by treatment with a reverse phase solid phase extraction column, whereas when a tobacco flavor liquid is prepared from an acidic tobacco extract adjusted to a pH of 5.3, nicotine is easily removed from the acidic tobacco extract by treatment with a reverse phase solid phase extraction column.

[0163] In the case of myosmine and nicotine, in all cases in which tobacco flavor solutions were prepared from acidic tobacco extracts adjusted to pH 0.9 to 5.3, the flavor components were hardly removed from the acidic tobacco extracts by treatment with a reverse phase solid-phase extraction column.

[0164] For anabasine, anatabine, and dipyridyl, when the acidic tobacco extract was adjusted to pH 3.2 or less, almost no flavor components were removed from the acidic tobacco extract by treatment with a reverse phase solid phase extraction column, but when the acidic tobacco extract was adjusted to pH 4.1, some flavor components were removed from the acidic tobacco extract, and when the acidic tobacco extract was adjusted to pH 5.3, the flavor components were easily removed from the acidic tobacco extract.

[0165] [Example 6] In Example 6, an analysis of tobacco specific nitrosamines (TSNAs) in tobacco flavor liquid was carried out.

[0166] 6-1. Method A tobacco flavor liquid was prepared according to the method described in Example 4, and the tobacco flavor liquid was subjected to LC-MS-MS analysis. The tobacco flavor liquid was prepared from an acidic tobacco extract having a pH of 0.9 to 5.3.

[0167] 6-2.Results Table 2 shows the analysis results of the TSNA amounts.

[0168] [Table 2]

[0169] The TSNA content shown in Table 2 refers to the sum of the 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) content, the N'-nitrosonornicotine (NNN) content, the N'-nitrosoanatabine (NAT) content, and the N'-nitrosoanabasine (NAB) content. The TSNA reduction rate shown in Table 2 refers to the value calculated by the following formula. TSNA reduction rate [%] = {(TSNA content in acidic tobacco extract) - (TSNA content in tobacco flavoring liquid) / (TSNA content in acidic tobacco extract)} x 100

[0170] The results in Table 2 show that in all cases where tobacco flavor solutions were prepared from acidic tobacco extracts adjusted to pH 0.9 to 4.1, TSNAs were removed by treatment with a reversed-phase solid-phase extraction column.

[0171] The results of Examples 4 to 6 show that when a tobacco flavor liquid is prepared from an acidic tobacco extract adjusted to a pH of 4.1 or less by treatment with a reverse-phase solid-phase extraction column, colored components and tobacco-specific nitrosamines (TSNAs) can be removed from the tobacco extract while maintaining the tobacco flavor components contained in the tobacco extract.

[0172] [Example 7] In Example 7, the effect of adding ethanol to the preparation of a tobacco flavor liquid was examined.

[0173] 7-1. Preparation of tobacco flavor liquid According to the method described in Example 4, an acidic tobacco extract (pH 2.2 or 3.2) was prepared, and ethanol was added to the acidic tobacco extract to obtain a predetermined ethanol concentration. Then, the acidic tobacco extract was passed through a reversed-phase solid-phase extraction column (Oasis-HLB). Thus, a tobacco flavor liquid was obtained.

[0174] 7-2.Analysis method Tobacco flavor liquids were analyzed by GC-MS. Tobacco flavor liquids were prepared from acidic tobacco extracts containing various concentrations of ethanol. The amounts of the flavor components myosmine, anabasine, anatabine, dipyridyl, benzaldehyde, phenethyl alcohol, and megastigmatrienone were analyzed.

[0175] 7-3.Results The analysis results of benzaldehyde are shown in Figure 16. Figure 16 is a graph showing the relationship between the ethanol concentration in the acidic tobacco extract and the benzaldehyde content in the tobacco flavor liquid.

[0176] The results in FIG. 16 show that adding ethanol to an acidic tobacco extract and using the resulting tobacco extract to prepare a tobacco flavor liquid can increase the benzaldehyde content in the tobacco flavor liquid.

[0177] As with benzaldehyde, for other flavor components (myosmine, anabasine, anatabine, dipyridyl, phenethyl alcohol, and megastigmatrienone), the content of flavor components in the tobacco flavor liquid could be increased by adding ethanol to an acidic tobacco extract and using the resulting tobacco extract to prepare a tobacco flavor liquid.

[0178] However, as the ethanol content in the acidic tobacco extract increased, it became more difficult to remove colored components by treatment with a reversed-phase solid-phase extraction column, and the colorlessness of the tobacco flavor liquid decreased. For example, when the ethanol content in the acidic tobacco extract was 50% by mass, the tobacco flavor liquid was colored brown, and when the ethanol content in the acidic tobacco extract was 10% by mass, the tobacco flavor liquid was almost colorless. Therefore, it is preferable to add ethanol to the acidic tobacco extract so that the final concentration is 10% by mass or less.

[0179] The results of Example 7 show that when the acidic tobacco extract contains ethanol at a concentration of 10% by mass or less, the tobacco flavor liquid obtained as the final product can contain a greater amount of tobacco flavor components while being colorless or nearly colorless.

[0180] [Example 8] In Example 8, a flavor evaluation was carried out using a non-combustion heating type flavor inhaler containing regenerated tobacco material.

[0181] 8-1. Preparation of tobacco sheets As a regenerated tobacco material, we prepared a tobacco sheet made from paper.

[0182] First, a tobacco material consisting of 60% by mass of flue-cured tobacco and 40% by mass of burley was extracted with hot water at 50°C for 1 hour. The ratio of the mass of the tobacco material to the mass of the hot water (solid-liquid ratio) was 1:20. The obtained extract was separated into a liquid (tobacco extract) and a solid (tobacco residue), and each was collected. A bleaching solution (i.e., an aqueous solution containing 1.5% by mass of peracetic acid, 4% by mass of acetic acid, and 0.55% by mass of hydrogen peroxide) was added to the tobacco residue, and the mixture was treated at 60°C for 0.5 hours. The ratio of the mass of the tobacco residue to the mass of the bleaching solution (solid-liquid ratio) was 1:40. The obtained bleached tobacco residue was washed with water, and then paper was made to prepare a base sheet tobacco. The above tobacco extract was poured back onto this base sheet tobacco to prepare a paper-made sheet tobacco. The paper-made sheet tobacco was cut into 0.8 mm widths to prepare shredded sheet tobacco (an example of the present invention).

[0183] The control sheet tobacco was prepared in the same manner as the above-mentioned sheet tobacco, except that the tobacco residue was not bleached. The control sheet tobacco was also shredded to a width of 0.8 mm to prepare shredded sheet tobacco (control).

[0184] 8-2. Preparation of flavor suction article The shredded sheet tobacco (example of the present invention) and the shredded sheet tobacco (control) were used as tobacco fillers to prepare the flavor inhalation article shown in FIG. 3. First, the shredded sheet tobacco was wrapped in cigarette paper to prepare a tobacco rod. The tobacco rod had a length of 20 mm and contained 260 mg of shredded sheet tobacco. A tobacco stick of a commercially available heated tobacco product (Ploom X, Japan Tobacco Inc.) was cut to remove the filter portion, and the above-mentioned tobacco rod was connected to this to prepare a flavor inhalation article.

[0185] Evaluation method A heating device from a commercially available heated tobacco product (Ploom X, Japan Tobacco Inc.) was used as an aerosol generating device to heat the flavor inhalation product, and a test evaluation was conducted by two expert panelists.

[0186] 8-4.Results The flavor inhalation article of the example of the present invention did not show a significant difference in overall impression of the flavor when compared with the control flavor inhalation article. No significant negative points were found in the flavor inhalation article of the example of the present invention with respect to the flavor. [Explanation of symbols]

[0187] 100: flavor inhaler, 110: flavor inhalation article, 120: aerosol generating device, 130: insertion hole, 140: lid portion, 150: push button, 110A...base material portion, 110B...suction mouth portion, 101...first plug wrapping paper, 102...filter material, 103...second plug wrapping paper, 104...filling layer, 111...filler, 112...first wrapping paper, 113...second wrapping paper, 114...paper tube portion, 115...filter plug, 116...hollow plug, 117...molded paper, 118...filter, 10: battery, 20: control unit, 30: heater, 132: inner tubular member, 134: outer tubular member, 160: air flow path, 170: lid portion, 180: partition wall

Claims

1. 1. A method for producing bleached tobacco residue comprising treating tobacco residue with an aqueous solution comprising peracetic acid, acetic acid and hydrogen peroxide to bleach said tobacco residue.

2. The method of claim 1 , further comprising extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent prior to the processing to prepare the tobacco residue.

3. 3. Bleached tobacco residue obtainable by the method of claim 1 or 2.

4. extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and a tobacco residue; treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to obtain a bleached tobacco residue; adjusting the pH of the tobacco extract to 4.1 or less to obtain an acidic tobacco extract; treating the acidic tobacco extract with a reversed phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid; mixing said bleached tobacco residue with said tobacco flavor liquid; A method for producing a reconstituted tobacco material, comprising:

5. 5. The method of claim 4, wherein said treatment with said reversed phase adsorbent is carried out by passing said acidic tobacco extract through a solid phase comprising said reversed phase adsorbent.

6. The method according to claim 4 or 5, wherein obtaining the acidic tobacco extract further comprises adding ethanol to the tobacco extract or to the tobacco extract adjusted to a pH of 4.1 or less so that the final ethanol concentration is 10% by mass or less.

7. A regenerated tobacco material obtained by the method according to any one of claims 4 to 6.

8. A tobacco product comprising the reconstituted tobacco material of claim 7.

9. A heated flavor inhaler comprising the reconstituted tobacco material according to claim 7.

10. An oral tobacco product comprising the reconstituted tobacco material according to claim 7.

Citation Information

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