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WO2016063775A1 - Procédé de fabrication d'ingrédient de cigarette - Google Patents

Procédé de fabrication d'ingrédient de cigarette Download PDF

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Publication number
WO2016063775A1
WO2016063775A1 PCT/JP2015/079053 JP2015079053W WO2016063775A1 WO 2016063775 A1 WO2016063775 A1 WO 2016063775A1 JP 2015079053 W JP2015079053 W JP 2015079053W WO 2016063775 A1 WO2016063775 A1 WO 2016063775A1
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WO
WIPO (PCT)
Prior art keywords
solvent
raw material
tobacco raw
closed space
capture
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2015/079053
Other languages
English (en)
Japanese (ja)
Inventor
仁紀 藤澤
健 秋山
信哉 大須賀
竹内　学
山田　学
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Japan Tobacco Inc
Original Assignee
Japan Tobacco Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PCT/JP2014/078410 external-priority patent/WO2015129098A1/fr
Application filed by Japan Tobacco Inc filed Critical Japan Tobacco Inc
Priority to EP15852051.0A priority Critical patent/EP3207809B1/fr
Priority to JP2016555187A priority patent/JP6259927B2/ja
Publication of WO2016063775A1 publication Critical patent/WO2016063775A1/fr
Priority to US15/493,400 priority patent/US10624387B2/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/241—Extraction of specific substances
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26—Use of organic solvents for extraction
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B13/00—Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff

Definitions

  • This invention relates to the manufacturing method of the tobacco raw material containing a flavor component.
  • a technique for containing a flavor ingredient for example, alkaloid containing a nicotine ingredient
  • a technique for utilizing a tobacco raw material itself as a flavor source, or extracting a flavor ingredient from a tobacco raw material to obtain a flavor source Techniques for supporting a substrate are known.
  • the first feature is a method for producing a tobacco raw material containing a flavor component, wherein the tobacco raw material subjected to alkali treatment is heated in a closed space, and the flavor component released as a gas phase from the tobacco raw material is Step A to be taken out of the closed space; and outside the closed space, the first flavoring component released as a gas phase in Step A is brought into contact with a first solvent that is a liquid substance at room temperature, thereby The step B for capturing the flavor component in the step, and after the step A, the second solvent is supplied to the tobacco raw material in the closed space, and is normally released as a liquid phase from the tobacco raw material to the second solvent.
  • step C the component is taken out together with the second solvent, and after step B and step C, the first solvent that has captured the flavor component in step B is the closed space in step A. And summarized in that and a step D to be added to the tobacco material after releasing the flavor and taste components to the outside.
  • the second feature is that, in the first feature, the step D includes, after the step B and the step C, the first solvent that has captured the flavor component in the step B in the closed space.
  • the gist is that it is a step of adding to the tobacco raw material after releasing the flavor component out of the closed space in the step A.
  • the third feature is summarized in that, in the first feature or the second feature, the step C is repeated at least twice before the step D.
  • the fourth feature is that, in the third feature, when n is an integer equal to or greater than 1, the solvent A is used as the second solvent in the n-th step C, and the n-th step C includes the first
  • the gist is that a solvent B different from the solvent A is used as the two solvents.
  • the fifth feature is summarized in that, in the third feature or the fourth feature, the step C is repeated at least twice using the second solvents having different temperatures.
  • the sixth feature is summarized in that, in the fifth feature, the step C includes a step of bubbling while adding CO 2 gas to the second solvent having the lowest temperature among different temperatures. .
  • the seventh feature is that, in the fifth feature or the sixth feature, the step C includes a step of bubbling while adding CO 2 gas to the second solvent having a temperature of 20 ° C. or less. To do.
  • the step C takes out the normal component out of the closed space using water having a first temperature as the second solvent. And using the water having a second temperature lower than the first temperature as the second solvent and bubbling while adding CO 2 gas to the water having the second temperature, And a step of taking it out of the closed space.
  • the step A includes a step of subjecting the tobacco source to a water treatment.
  • a tenth feature is characterized in that, in the ninth feature, in step A, the amount of water in the tobacco source before heating the tobacco source is 30% by weight or more by the hydration treatment. .
  • the eleventh feature is summarized in any one of the first to tenth features, wherein the step A includes a step of adding a non-aqueous solvent to the tobacco raw material.
  • the twelfth feature is summarized in that, in the eleventh feature, the amount of the non-aqueous solvent is 10% by weight or more based on the tobacco raw material.
  • the thirteenth feature is summarized in that, in the eleventh feature or the twelfth feature, the step A includes a step of adding water to the tobacco raw material in addition to the non-aqueous solvent.
  • the fourteenth feature is summarized as any one of the first to thirteenth features, wherein the temperature of the first solvent is 10 ° C. or higher and 40 ° C. or lower.
  • the volume of the closed space referred to in the first feature is preferably not significantly different from the volume of the tobacco raw material from the viewpoint of reducing the loss of the tobacco raw material by reducing the inner surface of the closed space. . Moreover, it is preferable that the volume of the closed space referred to in the first feature is not extremely different from the volume of the tobacco raw material from the viewpoint of efficient cleaning.
  • the shape of the closed space referred to in the first feature preferably does not include an extremely elongated portion from the viewpoint of reducing the loss of the tobacco raw material by reducing the inner surface of the closed space. In addition, it is preferable that the shape of the closed space mentioned in the first feature does not include an extremely long and narrow portion from the viewpoint of efficient cleaning.
  • the volume of the closed space is preferably 3 to 50 times the volume of the tobacco raw material.
  • the lengths of the longest portions in the X direction, the Y direction, and the Z direction, which are directions that intersect each other at 90 degrees in the closed space are X, Y, and Z, respectively.
  • L is preferably 10 times or less of S.
  • the area where the tobacco material contacts the inner surface of the closed space is reduced, and the closed space is closed. It should be noted that the tobacco raw material loss is reduced because the tobacco raw material that adheres to the inner surface of the space also decreases.
  • FIG. 1 is a diagram illustrating an example of a manufacturing apparatus according to the first embodiment.
  • FIG. 2 is a diagram illustrating an example of the manufacturing apparatus according to the first embodiment.
  • FIG. 3 is a diagram for explaining an application example of the flavor component.
  • FIG. 4 is a flowchart showing the manufacturing method according to the first embodiment.
  • FIG. 5 is a diagram for explaining the first experiment.
  • FIG. 6 is a diagram for explaining the first experiment.
  • FIG. 7 is a diagram for explaining the first experiment.
  • FIG. 8 is a diagram for explaining the second experiment.
  • FIG. 9 is a diagram for explaining the second experiment.
  • FIG. 10 is a diagram for explaining the third experiment.
  • FIG. 11 is a diagram for explaining the third experiment.
  • FIG. 12 is a diagram for explaining the fourth experiment.
  • FIG. 13 is a diagram for explaining the fourth experiment.
  • FIG.1 and FIG.2 is a figure which shows an example of the manufacturing apparatus which concerns on 1st Embodiment.
  • the processing apparatus 10 includes a container 11 and a sprayer 12.
  • the container 11 accommodates the tobacco raw material 50.
  • the container 11 is comprised by the member (for example, SUS; Steel Used Stainless) which has heat resistance and pressure resistance, for example.
  • the container 11 preferably constitutes a closed space.
  • the “closed space” is a space for flavor components (for example, nicotine components) contained in the tobacco raw material 50 in normal handling (processing operation, transportation, storage, etc.) to prevent solid foreign matters from entering the space. It is a space where movement to the outside is suppressed. As a result, the tobacco raw material is kept hygienic, and there is no need to transfer the tobacco raw material, thereby reducing the loss of the tobacco raw material.
  • step S30 capturing process
  • step S60 cleaning
  • the nicotine component is an example of a flavor component that contributes to tobacco flavor, and is used as an indicator of the flavor component in the embodiment.
  • the sprayer 12 applies an alkaline substance to the tobacco raw material 50.
  • the alkaline substance for example, a basic substance such as an aqueous potassium carbonate solution is preferably used.
  • the sprayer 12 applies an alkaline substance to the tobacco raw material 50 until the pH of the tobacco raw material 50 becomes 8.0 or more. More preferably, the sprayer 12 preferably applies an alkaline substance to the tobacco raw material 50 until the pH of the tobacco raw material 50 is in the range of 8.9 to 9.7. Further, in order to efficiently release the flavor component from the tobacco raw material 50 as a gas phase, the moisture content of the tobacco raw material 50 after spraying the alkaline substance is preferably 10% by weight or more, and more preferably 30% by weight or more. Is more preferable. Although the upper limit of the moisture content of the tobacco raw material 50 is not specifically limited, For example, in order to heat the tobacco raw material 50 efficiently, it is preferable to set it as 50 weight% or less.
  • the initial content of the flavor component (here, nicotine component) contained in the tobacco raw material 50 is 2.0% by weight or more when the total weight of the tobacco raw material 50 is 100% by weight in the dry state. Preferably there is. More preferably, the initial content of the flavor component (here, nicotine component) is preferably 4.0% by weight or more.
  • a tobacco genus raw material such as Nicotiana tabacum or Nicotiana rustica can be used.
  • Nicotiana tabacam for example, varieties such as Burley or yellow can be used.
  • tobacco raw materials other than Burley species and yellow species may be used.
  • the tobacco raw material 50 may be composed of tobacco raw materials in chopped or granular form.
  • the particle size of the step or powder is preferably 0.5 mm to 1.18 mm.
  • the capture device 20 includes a container 21, a pipe 22, a discharge portion 23, and a pipe 24.
  • the container 21 accommodates the capture solvent 70 (that is, the first solvent).
  • the container 21 is made of, for example, a member (for example, glass or stainless steel (SUS)) that has resistance to a trapping solvent and volatile flavor components / volatile impurities. It is preferable that the container 21 constitutes a space having airtightness that can suppress the movement of air to the outside of the space.
  • the temperature of the capture solvent 70 is, for example, room temperature.
  • the lower limit of the normal temperature is, for example, a temperature at which the capture solvent 70 does not solidify, preferably 10 ° C.
  • the upper limit of normal temperature is 40 degrees C or less, for example.
  • An arbitrary acid such as malic acid or citric acid may be added to the capture solvent 70 in order to prevent re-volatilization of the flavor component captured by the capture solvent 70.
  • a solvent such as an aqueous citric acid solution may be added to the capture solvent 70 in order to increase the capture efficiency of the flavor component. That is, the capture solvent 70 may be composed of a plurality of types of solvents.
  • the initial pH of the capture solvent 70 is preferably lower than the pH of the tobacco raw material 50 after the alkali treatment.
  • the pipe 22 guides the release component 61 released from the tobacco raw material 50 as a gas phase by heating the tobacco raw material 50 to the trapping solvent 70.
  • the release component 61 includes at least a nicotine component that is an index of the flavor component. Since the tobacco raw material 50 is alkali-treated, the release component 61 may contain ammonium ions depending on the time (processing time) that has elapsed since the start of the step of capturing the flavor component. The release component 61 may contain TSNA depending on the time (processing time) that has elapsed since the start of the capture process.
  • the discharge part 23 is provided at the tip of the pipe 22 and is immersed in the capture solvent 70.
  • the discharge portion 23 has a plurality of openings 23A.
  • the release component 61 guided by the pipe 22 is released into the capture solvent 70 as a foam-like release component 62 from the plurality of openings 23A.
  • the pipe 24 guides the remaining component 63 not captured by the capture solvent 70 to the outside of the container 21.
  • the release component 62 is a component released as a gas phase by heating the tobacco raw material 50, the temperature of the trapping solvent 70 may be increased by the release component 62. Therefore, the capture device 20 may have a function of cooling the capture solvent 70 in order to maintain the temperature of the capture solvent 70 at room temperature.
  • the capture device 20 may have a Raschig ring to increase the contact area of the release component 62 with the capture solvent 70.
  • FIG. 3 is a diagram for explaining an application example of the flavor component.
  • the flavor component is given to a component of a luxury item (for example, a flavor source of a flavor suction tool).
  • the flavor suction device 100 includes a holder 110, a carbon heat source 120, a flavor source 130, and a filter 140.
  • the holder 110 is, for example, a paper tube having a cylindrical shape.
  • the carbon heat source 120 generates heat for heating the flavor source 130.
  • the flavor source 130 is a substance that generates a flavor, and is an example of a flavor source base material to which a flavor component is imparted.
  • the filter 140 suppresses the contamination material from being guided to the inlet side.
  • the flavor suction tool 100 has been described as an application example of the flavor component, but the embodiment is not limited thereto.
  • the flavor component may be applied to other suction devices such as an electronic cigarette aerosol source (so-called E-ligid).
  • a flavor component may be provided to flavor source base materials, such as a gum, a tablet, a film, and a candy.
  • FIG. 4 is a flowchart showing the manufacturing method according to the first embodiment.
  • an alkaline substance is applied to the tobacco raw material 50 using the processing apparatus 10 described above.
  • the alkaline substance for example, a basic substance such as an aqueous potassium carbonate solution can be used.
  • the initial content of the flavor component (here, nicotine component) contained in the tobacco raw material 50 is 2.0% by weight or more when the total weight of the tobacco raw material 50 is 100% by weight in the dry state. Preferably there is. More preferably, the initial content of the flavor component (here, nicotine component) is preferably 4.0% by weight or more.
  • the pH of the tobacco raw material 50 after the alkali treatment is preferably 8.0 or more. More preferably, the pH of the tobacco raw material 50 after the alkali treatment is preferably in the range of 8.9 to 9.7.
  • step S20 the tobacco raw material 50 subjected to alkali treatment is heated in a closed space (in the above-described container 11 in the embodiment), and a flavor component released from the tobacco raw material 50 as a gas phase. Is taken out of the closed space.
  • the tobacco raw material 50 can be heated together with the container 11 in a state where the tobacco raw material 50 is accommodated in the container 11 of the processing apparatus 10.
  • the pipe 22 of the capturing device 20 is attached to the container 11.
  • the heating temperature of the tobacco raw material 50 is in the range of 80 ° C. or more and less than 150 ° C.
  • the timing at which a sufficient flavor component is released from the tobacco raw material 50 can be advanced.
  • the timing at which TSNA is released from the tobacco raw material 50 can be delayed.
  • a treatment for subjecting the tobacco raw material 50 to a hydration treatment may be performed before the tobacco raw material 50 is heated.
  • a hydration process may be performed in step S10, and may be performed before heating the tobacco raw material 50 in step S20.
  • the hydration treatment may be performed while heating the tobacco raw material 50 in step S20 in order to compensate for moisture that decreases with the heating of the tobacco raw material 50 in step S20.
  • the hydration treatment may be performed intermittently at least once.
  • the water treatment may be performed continuously over a predetermined period.
  • the moisture content of the tobacco raw material 50 before heating the tobacco raw material 50 is preferably 30% by weight or more.
  • the upper limit of the moisture content of the tobacco raw material 50 is not specifically limited, For example, in order to heat the tobacco raw material 50 efficiently, it is preferable to set it as 50 weight% or less.
  • step S20 heat treatment preferably includes a step of adding a non-aqueous solvent to the tobacco raw material 50.
  • the amount of the non-aqueous solvent is preferably 10 wt% or more and 50 wt% or less with respect to the tobacco raw material 50.
  • the non-aqueous solvent may be a solvent other than water.
  • non-aqueous solvent examples include glycerin, propylene glycol, ethanol, alcohol, acetonitrile, hexane and the like.
  • water may be added to the tobacco raw material 50 in addition to the non-aqueous solvent.
  • the timing of adding the non-aqueous solvent to the tobacco raw material 50 may be the timing until step S20 (heat treatment) is completed.
  • the timing at which the non-aqueous solvent is added to the tobacco raw material 50 may be the timing between step S10 (alkali treatment) and step S20 (heat treatment).
  • the timing which adds a non-aqueous solvent to the tobacco raw material 50 may be the timing in the middle of step S20 (heating process).
  • the nonaqueous solvent is preferably a solvent that does not substantially vaporize at the heating temperature in step S20 (heat treatment). Thereby, in Step S30 to be described later, it is possible to prevent the non-aqueous solvent and the contaminants dissolved in the non-aqueous solvent from being mixed into the capture solvent.
  • the tobacco raw material 50 may be subjected to a hydration treatment while the tobacco raw material 50 is being heated. It is preferable that the moisture content of the tobacco raw material 50 is maintained at 10% or more and 50% or less by the hydration treatment.
  • the tobacco raw material 50 may be continuously hydrated. The amount of water added is preferably adjusted so that the moisture content of the tobacco raw material 50 is 10% or more and 50% or less. Furthermore, you may add the non-aqueous solvent mentioned above to the tobacco raw material 50 with a hydration process.
  • step S20 it is preferable to subject the tobacco material 50 to aeration.
  • the amount of flavor components contained in the release component 61 released from the tobacco-treated tobacco material 50 into the gas phase can be increased.
  • the aeration treatment for example, saturated water vapor at 80 ° C. is brought into contact with the tobacco raw material 50. Since the aeration time in the aeration treatment varies depending on the apparatus for treating the tobacco raw material 50 and the amount of the tobacco raw material 50, it cannot be specified in general. For example, when the tobacco raw material 50 is 500 g, the aeration time is Within 300 minutes.
  • the total aeration amount in the aeration treatment also varies depending on the apparatus for treating the tobacco raw material 50 and the amount of the tobacco raw material 50, and thus cannot be generally specified. For example, when the tobacco raw material 50 is 500 g, 10 L / It is about g.
  • the air used in the ventilation process may not be saturated water vapor.
  • the moisture content of the air used in the aeration treatment does not particularly require humidification of the tobacco raw material 50, for example, so that the moisture contained in the tobacco raw material 50 to which the heat treatment and the aeration treatment are applied falls within a range of less than 50%. May be adjusted.
  • the gas used in the aeration process is not limited to air, and may be an inert gas such as nitrogen or argon.
  • step S30 (that is, step B2), the flavor components released as a vapor phase in step S20 in the capture device 20 outside the closed space (in the embodiment, outside the container 11 described above), that is, in the embodiment, at room temperature.
  • the capturing solvent 70 first solvent which is a liquid substance
  • step S20 and step S30 are shown as separate processes in FIG. 4, but it should be noted that steps S20 and S30 are processes performed in parallel. Note that parallel means that the period in which step S30 is performed overlaps with the period in which step S20 is performed, and step S20 and step S30 do not have to start and end at the same time.
  • the pressure in the container 11 of the processing apparatus 10 is equal to or lower than the normal pressure.
  • the upper limit of the pressure in the container 11 of the processing apparatus 10 is +0.1 MPa or less in gauge pressure.
  • the inside of the container 11 of the processing apparatus 10 may be a reduced pressure atmosphere.
  • the capture solvent 70 for example, glycerin, water, or ethanol can be used as described above.
  • the temperature of the trapping solvent 70 is room temperature.
  • the lower limit of the normal temperature is, for example, a temperature at which the capture solvent 70 does not solidify, preferably 10 ° C.
  • the upper limit of normal temperature is 40 degrees C or less, for example.
  • step S40 in order to increase the concentration of the flavor component contained in the capture solution, the trapping solvent 70 that captures the flavor component is subjected to a vacuum concentration process, a heat concentration process, or a salting-out process.
  • a vacuum concentration process a heat concentration process, or a salting-out process.
  • the process of step S40 is not essential and may be omitted.
  • the vacuum concentration treatment is performed in a space having airtightness that can suppress the movement of air to the outside of the space. Thereby, there is little air contact and it is not necessary to raise the trapping solvent 70 to a high temperature, so there is little concern about component changes. Therefore, the use of vacuum concentration increases the types of capture solvents that can be used.
  • the concentration of the flavor component can be increased as compared with the vacuum concentration treatment, but since the flavor component in the liquid solvent phase / water phase is half, the yield of the flavor component is poor. Moreover, since coexistence of a hydrophobic substance (MCT etc.) is assumed to be essential, salting-out may not occur depending on the ratio of the capture solvent, water and flavor components.
  • MCT hydrophobic substance
  • step S50 the tobacco raw material 50 after releasing the flavor component in step S20 is prepared.
  • the tobacco raw material 50 is still maintained in the closed space (in the embodiment, in the container 11 described above).
  • step S60 that is, step C
  • a cleaning solvent (second solvent) is supplied to the tobacco raw material 50 in the closed space (in the above-described container 11 in the embodiment), and the tobacco raw material 50 is supplied as a liquid phase to the cleaning solvent.
  • the released normal components are taken out of the closed space (in the embodiment, out of the container 11 described above) together with the cleaning solvent.
  • step S30 after the flavor component contained in the tobacco raw material 50 is extracted, in step S60 (cleaning process), the residue after the flavor component is extracted is the cleaning solvent. It is washed by. Thereby, the normal component (contaminating substance) remaining in the tobacco raw material 50 (residue) is removed.
  • step S60 cleaning process
  • the manufacturing method according to the embodiment can easily remove unnecessary contaminants from the tobacco raw material 50 (residue).
  • step S60 cleaning process
  • step S30 capturing process
  • the cleaning solvent is supplied from the sprayer 12 to the tobacco raw material 50 (residue). And spraying, and then cleaning is performed by rotating and shaking the container 11 for about 10 to 60 minutes.
  • the weight ratio of the tobacco raw material 50 (residue) to the washing solvent (washing solvent / residue) can be 10 to 20 when the tobacco raw material 50 (residue) is 1.
  • an aqueous solvent can be mentioned, and specific examples thereof include pure water and ultrapure water, and can include city water. Further, the temperature of the cleaning solvent may be from room temperature (for example, 20 ° C. ⁇ 15 ° C.) to 70 ° C.
  • a solution obtained by bubbling CO 2 gas may be used, and specific examples include an aqueous solution containing carbonated water or supersaturated CO 2 gas.
  • an aqueous solvent such as water may be used in which ozone is bubbled.
  • Step S60 may be repeated at least twice.
  • n is an integer of 1 or more
  • the solvent A is used as the cleaning solvent in the n-th step
  • the solvent B different from the solvent A is used as the cleaning solvent in the n + 1-th step. May be.
  • step S60 (cleaning process) is repeated three times or more
  • three or more types of solvents may be used as the cleaning solvent.
  • step S60 (cleaning process) is repeated three or more times, the same solvent may be used in two or more steps S60 (cleaning process).
  • cleaning may be performed first with water and then with an aqueous solvent in which CO 2 gas is bubbled. Each washing may be performed a plurality of times. When washing is performed using such a procedure or an aqueous solvent, contaminants are efficiently removed.
  • step S60 may be repeated at least twice using second solvents having different temperatures.
  • step S60 cleaning process
  • Step S60 cleaning process
  • Basic substances such as aqueous potassium solution) can be efficiently neutralized and removed.
  • step S60 includes a step of taking out normal components out of the closed space using water having a first temperature (for example, 40 to 80 ° C.) as the second solvent (hereinafter referred to as the first cleaning step).
  • a first temperature for example, 40 to 80 ° C.
  • the second solvent By using water having a second temperature lower than the first temperature (for example, 10 to 15 ° C.) as the second solvent and performing bubbling while adding CO 2 gas to the water having the second temperature, And a step of taking out the outside of the closed space (hereinafter referred to as a second cleaning step). Accordingly, by performing the cleaning process using water having a relatively high first temperature, water-soluble impurities are removed, and bubbling is performed while adding CO 2 gas to water having a relatively low second temperature.
  • the alkaline substance (basic substance such as an aqueous potassium carbonate solution) imparted to the tobacco raw material 50 is efficiently neutralized and removed while suppressing the decrease in the solubility of the CO 2 gas. it can.
  • the second cleaning step is preferably performed after the first cleaning step.
  • the first cleaning step may be performed twice or more.
  • the second cleaning step may be performed twice or more.
  • washing solvent in addition to the above aqueous solvent, a non-aqueous solvent such as propylene glycol, glycerin, ethanol, MCT), hexane, methanol, acetonitrile can also be used. Moreover, these can also be mixed and used for said aqueous solvent.
  • a non-aqueous solvent such as propylene glycol, glycerin, ethanol, MCT), hexane, methanol, acetonitrile.
  • an acidic solvent may be used as a cleaning solvent.
  • an acidic solvent the solvent containing carboxylic acids, such as an acetic acid and malic acid, is mentioned, for example.
  • drying conditions include a mode in which air is circulated at a temperature of about 110 to 125 ° C. (ventilation amount: 10 to 20 L / min / 250 g-min) for about 100 to 150 minutes.
  • step S60 cleaning process
  • the types of contaminant components having high affinity with the cleaning solvent can be made different by properly using the type of cleaning solvent used in each cleaning process. And various kinds of contaminating components can be removed.
  • step S60 cleaning process
  • step S70 backing process
  • step S70 in the closed space (in the embodiment, in the container 11 described above), the trapping solvent (first solvent) that captured the flavor component in step S30 is removed from the closed space in step S20.
  • the capture solvent (first solvent) added to the tobacco raw material 50 (washed tobacco raw material residue) may be neutralized.
  • the tobacco raw material containing the flavor component may be neutralized after being added to the tobacco raw material 50 (washed tobacco raw material residue) to the capture solvent (first solvent).
  • the tobacco raw material containing the savory ingredients is produced by the processing described above. However, as described above, the process of step S40 (concentration process) may be omitted.
  • step S70 may be performed outside the closed space (in the embodiment, outside the container 11 described above).
  • the residue (washed tobacco raw material residue) obtained through the cleaning process in step S60 (cleaning process) may be pulverized and granulated.
  • the pulverization process is, for example, a process of pulverizing the cleaned tobacco raw material residue, adding a binder to the pulverized residue, and mixing the pulverized residue and the binder.
  • the granule molding process is, for example, a process of kneading and extruding a mixture of pulverized residue and binder and then sizing and drying the mixture while stirring the mixture with a mixer.
  • the granule forming process may be performed simultaneously with step S70 (backing process).
  • step S20 heating process
  • step S30 capture process
  • the flavor component contained in the tobacco raw material is captured by the capture solvent
  • the capture solvent capturing the flavor component is added to the tobacco raw material.
  • step S70 extraction process
  • impurities contained in the tobacco raw material such as ammonia can be selectively reduced by a simple and low-cost process.
  • step S60 washing
  • contaminant components such as TSNA are further selectively reduced.
  • step S20 heating process
  • step S60 cleaning process
  • step S30 capture processing
  • the first condition is that the pH of the capture solution after the pH of the capture solution containing the capture solvent 70 and the release component 62 has decreased by 0.2 or more from the maximum value on the time axis that has elapsed since the start of step S20.
  • the time elapsed after the start of step S20 (hereinafter, processing time) is a condition for reaching the start timing of the stable section.
  • the stable section is a section where the fluctuation amount of the pH of the capture solution falls within a predetermined range (for example, the average fluctuation amount per unit time is ⁇ 0.01 / min), and the trapping in the section is performed.
  • the fluctuation range of the pH of the solution falls within a predetermined range (for example, the difference between the pH at the time when the interval starts and the pH when the second condition described later is satisfied is ⁇ 0.2).
  • the start timing of the stable interval is, for example, capture This is the timing when the pH of the solution stops decreasing.
  • the pH profile of the capture solution is measured in advance under the same conditions as in actual processing, and the pH of the capture solution is preferably replaced with the treatment time. That is, it is preferable that the first condition is replaced with the processing time. As a result, it is not necessary to monitor the amount of fluctuation in the pH of the capture solution in real time, and ammonium ions (NH 4 + ) can be removed from the capture solution by simple control.
  • the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 reaches 0.3% by weight. It is a condition to decrease to. More preferably, the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.4. It is a condition that decreases until reaching% by weight. More preferably, the second condition is that, in a dry state, when the weight of the tobacco raw material 50 is 100% by weight, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.6. It is a condition that decreases until reaching% by weight.
  • the profile of the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is measured in advance under the same conditions as those in the actual processing, and the remaining amount of the flavor component is determined by the processing. It is preferred that it be replaced by time. That is, it is preferable that the second condition is replaced with the processing time. Thereby, it is not necessary to monitor the remaining amount of the flavor component in real time, and it is possible to suppress an increase in the content of TSNA contained in the capture solvent by simple control.
  • the total content of sugars contained in the tobacco raw material 50 is 10.0% by weight or less when the total weight of the tobacco raw material 50 is 100% by weight in the dry state.
  • the saccharide contained in the tobacco raw material 50 is fructose, glucose, saccharose, maltose, inositol.
  • step S30 in which the released component is brought into contact with the capture solvent 70 is continued until at least the first condition is satisfied.
  • ammonium ions (NH 4 + ) contained in the release component are sufficiently removed from the capture solution.
  • other volatile impurities specifically, acetaldehyde and pyridine
  • acetaldehyde and pyridine that exhibit the same behavior as ammonium ions in the release from the tobacco raw material 50 and the extraction with the capture solvent are captured by satisfying the first condition. Removed from solution.
  • step S30 in which the released component is brought into contact with the capture solvent 70 ends at least until the second condition is satisfied.
  • step S20 and step S30 it is possible to sufficiently extract the flavor components while suppressing the mixing of ammonium ions (NH 4 + ) and contaminating components such as TSNA. That is, a savory component can be extracted with a simple device.
  • ammonium ions NH 4 +
  • contaminating components such as TSNA
  • the non-volatile component contained in the tobacco raw material 50 does not move to the capture solvent, but only the component that volatilizes at about 120 ° C. can be captured by the capture solvent, the component captured by the capture solvent It can be used as an aerosol source.
  • This makes it possible to deliver an aerosol containing tobacco flavor to the user while suppressing the increase of volatile contaminants such as ammonium ions, acetaldehyde, and pyridine in electronic cigarettes, and further suppresses the migration of non-volatile components to the capture solvent. Therefore, it is possible to suppress the burn of the heater that heats the aerosol source.
  • electrocigarette includes a liquid aerosol source and an electric heater for heating and atomizing the aerosol source, and a non-combustion flavor inhaler or aerosol suction for delivering the aerosol to the user.
  • aerosol inhaler described in Japanese Patent No. 5196673, aerosol electronic cigarette described in Japanese Patent No. 5385418, etc.
  • aerosol suction for delivering the aerosol to the user.
  • step S30 (capturing process) is performed until any timing from when the first condition is satisfied until the second condition is satisfied.
  • the first condition is that, in a dry state, when the weight of the tobacco raw material is 100% by weight, the remaining amount of the flavor component (here, nicotine component) contained in the tobacco raw material reaches 1.7% by weight. It is a condition to decrease to.
  • the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 reaches 0.3% by weight. It is a condition to decrease to. More preferably, the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.4. It is a condition that decreases until reaching% by weight. More preferably, the second condition is that, in a dry state, when the weight of the tobacco raw material 50 is 100% by weight, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.6. It is a condition that decreases until reaching% by weight.
  • the profile of the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is measured in advance under the same conditions as those in the actual processing, and the remaining amount of the flavor component is determined by the processing. It is preferred that it be replaced by time. That is, it is preferable that the second condition is replaced with the processing time. Thereby, it is not necessary to monitor the remaining amount of the flavor component in real time, and it is possible to suppress an increase in the content of TSNA contained in the capture solvent by simple control.
  • step S30 of bringing the released component into contact with the capture solvent 70 continues until at least the first condition is satisfied.
  • step S30 is continued in a section where the rate of decrease in the remaining amount of flavor components contained in the tobacco raw material (that is, the speed at which the nicotine component volatilizes from the tobacco raw material 50) is equal to or higher than the predetermined speed.
  • the taste component can be recovered.
  • step S30 for bringing the released component into contact with the trapping solvent 70 ends at least until the second condition is satisfied. As a result, by terminating S30 before the amount of TSNA released increases, an increase in the TSNA content contained in the capture solution is suppressed.
  • step S20 and step S30 it is possible to sufficiently extract the flavor components while suppressing the mixing of the miscellaneous components such as TSNA. That is, a savory component can be extracted with a simple device.
  • the non-volatile component contained in the tobacco raw material 50 does not move to the capture solvent, but only the component that volatilizes at about 120 ° C. can be captured by the capture solvent, the component captured by the capture solvent It can be used as an aerosol source.
  • This makes it possible to deliver an aerosol containing tobacco flavor to the user while suppressing the increase of volatile contaminants such as ammonium ions, acetaldehyde, and pyridine in electronic cigarettes, and further suppresses the migration of non-volatile components to the capture solvent. Therefore, it is possible to suppress the burn of the heater that heats the aerosol source.
  • electrocigarette includes a liquid aerosol source and an electric heater for heating and atomizing the aerosol source, and a non-combustion flavor inhaler or aerosol suction for delivering the aerosol to the user.
  • aerosol inhaler described in Japanese Patent No. 5196673, aerosol electronic cigarette described in Japanese Patent No. 5385418, etc.
  • aerosol suction for delivering the aerosol to the user.
  • the nicotine content (Nic. Amount) and ammonium ion content (NH 4 + amount) of Sample A to Sample C are as shown in FIG.
  • the content of saccharide (fructose, glucose, saccharose, maltose, inositol) in sample A is almost zero (less than the detection limit), and the saccharide (fructose, glucose, saccharose, maltose, inositol) in sample B is almost all.
  • the total content is 9.37% by weight, and the total content of saccharides (fructose, glucose, saccharose, maltose, inositol) of Sample C is 18.81% by weight.
  • processing time is the time which passed after starting the heat processing (S20) of a tobacco raw material. You may think that processing time is the time which passed since the capture
  • the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
  • the stable section is a section in which the amount of fluctuation in the pH of the capture solution falls within a predetermined range (for example, the average amount of fluctuation per unit time is ⁇ 0.01 / min), and
  • the range in which the fluctuation range of the pH of the capture solution in the section falls within a predetermined range for example, the difference between the pH when the section starts and the pH when the second condition described later is satisfied is ⁇ 0.2). It is.
  • the saccharides fructtose, glucose, saccharose, maltose, inositol
  • the volatile organic acid acetic acid / formic acid
  • the increase amount of the volatile organic acid was sample C> sample B> sample A, and it was confirmed that the increase amount of a volatile organic acid is so large that the content of the saccharide contained in a tobacco raw material is high. This is considered to be because an acidic substance is generated by the decomposition of the sugar and moves to the capture solution.
  • the tobacco raw material of the Burley species having a low content of saccharides contained in the tobacco raw material specifically, the total content of saccharides contained in the tobacco raw material is 10.0% by weight or less. It was confirmed that by using the tobacco raw material, it was possible to clearly determine a stable pH section indicating that the ammonium ion concentration in the capture solution was sufficiently reduced.
  • the use of a Burley-type tobacco raw material having a high ammonium ion (NH 4 + ) concentration makes it easy to determine the profile accompanying a decrease in pH.
  • Example A a sample of a burley tobacco material (sample A described above) was prepared, and the remaining amount of alkaloid (here, nicotine component) contained in the tobacco material in a dry state under the following conditions (hereinafter referred to as nicotine component) Nicotine concentration in the tobacco raw material), and the concentration of TSNA contained in the capture solution (hereinafter referred to as capture solution TSNA concentration).
  • the measurement result of the nicotine concentration in the tobacco raw material is as shown in FIG. 8, and the measurement result of the concentration of TSNA contained in the capture solution is as shown in FIG.
  • the residual amount of the nicotine component contained in the tobacco raw material is indicated by weight% when the weight of the tobacco raw material is 100% by weight in the dry state.
  • the concentration of TSNA contained in the capture solution is shown in wt% when the capture solution is 100 wt%. 8 and 9, the processing time is the time that has elapsed since the start of the tobacco raw material heat treatment (S20). You may think that processing time is the time which passed since the capture processing (S30) of a nicotine component was started.
  • NNK N′-Nitrosonoricotine
  • NNN N′-Nitrosonatabine
  • NAB Nitrosonabasine
  • the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
  • the residual amount of the nicotine component contained in the tobacco raw material is intermittently reduced.
  • NNK did not change, but it was confirmed that NNN, NAT and NAB increase after a certain period of time.
  • sample P to Q were prepared, and the pH of the capture solution and the concentration of alkaloid (here, nicotine component) contained in the capture solution were measured under the following conditions.
  • Sample P is a sample using glycerin as a capture solvent.
  • Sample Q is a sample using water as a capture solvent.
  • Sample R is a sample using ethanol as a capture solvent.
  • the measurement result of the pH of the capture solution is as shown in FIG.
  • the measurement result of the concentration of the nicotine component contained in the capture solution is as shown in FIG.
  • processing time is the time which passed since starting the heat processing (S20) of a tobacco raw material. You may think that processing time is the time which passed since the capture processing (S30) of a nicotine component was started.
  • the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
  • the temperature of the capture solvent is a set temperature of a chiller (constant temperature bath) that controls the temperature of the container that stores the capture solvent. It should be noted that the temperature of the capture solvent converges about 60 minutes after setting the container on the chiller and starting the temperature control.
  • the method was performed in accordance with the German Standardization Organization DIN 10373. That is, 250 mg of tobacco raw material was collected, 7.5 mL of an 11% aqueous sodium hydroxide solution and 10 mL of hexane were added, and the mixture was extracted by shaking for 60 minutes. After extraction, the supernatant hexane phase was subjected to a gas chromatograph mass spectrometer (GC / MS), and the weight of nicotine contained in the tobacco material was quantified.
  • GC / MS gas chromatograph mass spectrometer
  • the weight of the tobacco raw material in the dry state is calculated by subtracting the above-described moisture content from the total weight of the tobacco raw material.
  • GC analysis conditions The conditions of GC analysis used in the measurement of the nicotine component and the amount of water contained in the tobacco raw material are as shown in the following table.
  • step S10 alkali processing
  • step S60 cleaning processing
  • the embodiment is not limited to this.
  • step S20 heating process
  • step S30 capturing process
  • step S60 cleaning process
  • step S20 heating process
  • step S30 capturing process
  • step S60 cleaning process
  • the volume of the closed space formed by the container 11 used in step S20 (heating process) and step S60 (cleaning process) is reduced by reducing the inner surface of the closed space. From the viewpoint of reducing loss, it is preferable that there is no extreme difference with respect to the volume of the tobacco raw material. Moreover, it is preferable that the volume of the closed space is not significantly different from the volume of the tobacco raw material from the viewpoint of efficient cleaning.
  • the shape of the closed space formed by the container 11 preferably does not include an extremely elongated portion from the viewpoint of reducing the loss of the tobacco raw material by reducing the inner surface of the closed space. Moreover, it is preferable that the shape of the closed space does not include an extremely elongated portion from the viewpoint of efficient cleaning.
  • the volume of the closed space is preferably 3 to 50 times the volume of the tobacco raw material.
  • the lengths of the longest portions in the X direction, the Y direction, and the Z direction, which are directions that intersect each other at 90 degrees in the closed space are X, Y, and Z, respectively.
  • L is preferably 10 times or less of S. If the volume and shape of the closed space are as described above, the loss of the tobacco material can be reduced, and the tobacco material in Step S60 (cleaning process) with an appropriate amount of solvent while stirring the tobacco material appropriately. (Residue) can be sufficiently washed.
  • the area where the tobacco material contacts the inner surface of the closed space is reduced, and the closed space is closed. It should be noted that the tobacco raw material loss is reduced because the tobacco raw material that adheres to the inner surface of the space also decreases.
  • the cleaning process (step S60) is performed before the multiplying process (step S70), but the embodiment is not limited to this.
  • the cleaning process (step S60) may be omitted.
  • the present invention it is possible to provide a method for producing a tobacco raw material that can selectively reduce the impurities contained in the tobacco raw material by a simple and low-cost process.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

　La présente invention concerne un procédé de fabrication d'un ingrédient de cigarette qui contient un constituant d'inhalation parfumé comprenant : une étape A consistant à chauffer un ingrédient de cigarette traité avec des alcali à l'intérieur d'un espace fermé, et à prélever de l'espace fermé un constituant d'inhalation parfumé libéré sous la forme d'une phase vapeur à partir de l'ingrédient de cigarette ; une étape B consistant à mettre le constituant d'inhalation parfumé, qui a été libéré sous la forme d'une phase vapeur lors de l'étape A, en contact à l'extérieur de l'espace fermé avec un premier solvant qui est une substance liquide à température normale, ce qui permet de piéger le constituant d'inhalation parfumé dans le premier solvant ; une étape C après l'étape A, consistant à fournir un second solvant à l'ingrédient de cigarette à l'intérieur de l'espace fermé, et à prélever un constituant linéaire libéré de l'ingrédient de cigarette sous la forme d'une phase liquide dans le second solvant, à partir de l'espace fermé conjointement avec le second solvant ; et une étape D après l'étape B et l'étape C, consistant à ajouter le premier solvant dans lequel a été piégé le constituant d'inhalation parfumé au cours de l'étape B, à l'ingrédient de cigarette duquel a été libéré le constituant d'inhalation parfumé vers l'extérieur de l'espace fermé au cours de l'étape A.
PCT/JP2015/079053 2014-02-26 2015-10-14 Procédé de fabrication d'ingrédient de cigarette Ceased WO2016063775A1 (fr)

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JP2016555187A JP6259927B2 (ja) 2014-02-26 2015-10-14 たばこ原料の製造方法
US15/493,400 US10624387B2 (en) 2014-02-26 2017-04-21 Producing method of tobacco raw material

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