EP3207809A1 - Procédé de fabrication d'ingrédient de cigarette - Google Patents
Procédé de fabrication d'ingrédient de cigarette Download PDFInfo
- Publication number
- EP3207809A1 EP3207809A1 EP15852051.0A EP15852051A EP3207809A1 EP 3207809 A1 EP3207809 A1 EP 3207809A1 EP 15852051 A EP15852051 A EP 15852051A EP 3207809 A1 EP3207809 A1 EP 3207809A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- raw material
- solvent
- tobacco raw
- capture
- treatment
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 31
- 235000019504 cigarettes Nutrition 0.000 title 1
- 239000004615 ingredient Substances 0.000 title 1
- 241000208125 Nicotiana Species 0.000 claims abstract description 250
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 248
- 239000002994 raw material Substances 0.000 claims abstract description 239
- 239000002904 solvent Substances 0.000 claims abstract description 171
- 239000000796 flavoring agent Substances 0.000 claims abstract description 112
- 235000019634 flavors Nutrition 0.000 claims abstract description 112
- 239000000470 constituent Substances 0.000 claims abstract description 93
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000000126 substance Substances 0.000 claims abstract description 29
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000012071 phase Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007791 liquid phase Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 239000003125 aqueous solvent Substances 0.000 claims description 30
- 230000005587 bubbling Effects 0.000 claims description 18
- 238000011276 addition treatment Methods 0.000 claims description 13
- 238000011282 treatment Methods 0.000 description 160
- 239000000243 solution Substances 0.000 description 71
- 238000005406 washing Methods 0.000 description 66
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 51
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 51
- 229960002715 nicotine Drugs 0.000 description 51
- 239000007789 gas Substances 0.000 description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 25
- 230000007423 decrease Effects 0.000 description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 24
- 239000012535 impurity Substances 0.000 description 23
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 22
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 22
- 238000005273 aeration Methods 0.000 description 20
- 239000000443 aerosol Substances 0.000 description 17
- 238000002474 experimental method Methods 0.000 description 17
- 238000010586 diagram Methods 0.000 description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 150000001720 carbohydrates Chemical class 0.000 description 11
- 235000011187 glycerol Nutrition 0.000 description 11
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000003571 electronic cigarette Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 8
- 238000000605 extraction Methods 0.000 description 7
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 229930091371 Fructose Natural products 0.000 description 6
- 239000005715 Fructose Substances 0.000 description 6
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 description 6
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 229930006000 Sucrose Natural products 0.000 description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 6
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 235000013681 dietary sucrose Nutrition 0.000 description 6
- 229960002737 fructose Drugs 0.000 description 6
- 229960001031 glucose Drugs 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 description 6
- 229960000367 inositol Drugs 0.000 description 6
- 229960002160 maltose Drugs 0.000 description 6
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 description 6
- 229960004793 sucrose Drugs 0.000 description 6
- 238000009834 vaporization Methods 0.000 description 6
- 230000008016 vaporization Effects 0.000 description 6
- 230000003247 decreasing effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229930013930 alkaloid Natural products 0.000 description 4
- 150000003797 alkaloid derivatives Chemical class 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 description 4
- FLAQQSHRLBFIEZ-UHFFFAOYSA-N N-Methyl-N-nitroso-4-oxo-4-(3-pyridyl)butyl amine Chemical compound O=NN(C)CCCC(=O)C1=CC=CN=C1 FLAQQSHRLBFIEZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 235000005985 organic acids Nutrition 0.000 description 3
- 238000005185 salting out Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- -1 for example Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000008263 liquid aerosol Substances 0.000 description 2
- 239000001630 malic acid Substances 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- ZJOFAFWTOKDIFH-JTQLQIEISA-N 3-[(2s)-1-nitroso-3,6-dihydro-2h-pyridin-2-yl]pyridine Chemical compound O=NN1CC=CC[C@H]1C1=CC=CN=C1 ZJOFAFWTOKDIFH-JTQLQIEISA-N 0.000 description 1
- BXYPVKMROLGXJI-JTQLQIEISA-N 3-[(2s)-1-nitrosopiperidin-2-yl]pyridine Chemical compound O=NN1CCCC[C@H]1C1=CC=CN=C1 BXYPVKMROLGXJI-JTQLQIEISA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- XKABJYQDMJTNGQ-VIFPVBQESA-N n-nitrosonornicotine Chemical compound O=NN1CCC[C@H]1C1=CC=CN=C1 XKABJYQDMJTNGQ-VIFPVBQESA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Images
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
- the present invention relates to a producing method of a tobacco raw material containing a flavor constituent.
- a technique to allow a flavor source to contain a flavor constituent e.g. alkaloid including a nicotine component
- a technique utilizing a tobacco raw material itself as a flavor source and a technique in which a flavor constituent is extracted from a tobacco raw material and supported on a base material for a flavor source have been conventionally known.
- a first feature is summarized as a producing method of a tobacco raw material containing a flavor constituent, comprising: a step A for heating a tobacco raw material in a closed space which is treated with alkali and for taking a flavor constituent released in the gas phase from the tobacco raw material to an outside of the closed space; a step B for allowing a first solvent to capture the flavor constituent by bringing the flavor constituent released in the gas phase in the step A into contact with the first solvent which is a liquid substance at normal temperature on the outside of the closed space; a step C for supplying a second solvent to the tobacco raw material in the closed space after the step A and for taking a normal component which is released as the liquid phase from the tobacco raw material to the second solvent, together with the second solvent to the outside of the closed space; and after the step B and the step C, the step D for adding the first solvent capturing the flavor constituent in the step B to the tobacco raw material from which the flavor constituent is released to the outside of the closed space in the step A.
- a second feature is summarized as the production method according to the first feature, wherein the step D is, in the closed space after the steps B and C1, a step C1 for adding the first solvent capturing the flavor constituent in the step B1 to the tobacco raw material from which the flavor constituent is released to the outside of the closed space in the step A1 in the closed space.
- a third feature is summarized as the production method according to the first feature or the second feature, wherein the step C is repeated at least twice or more before the step D.
- a fourth feature is summarized as the production method according to the third feature, wherein when n is an integer of 1 or more, a solvent A is used as the second solvent in the n-th step C, and a solvent B different from the solvent A is used as the second solvent in the n + 1-th step C.
- a fifth feature is summarized as the production method according to the third feature or the fourth feature, wherein the step C is repeated at least two or more times using the second solvents having respectively different temperatures.
- a sixth feature is summarized as the production method according to the fifth feature, wherein the step C includes a step of bubbling while adding CO 2 gas to the second solvent having a lowest temperature among different temperatures.
- a seventh feature is summarized as the production method according to the fifth feature or sixth feature, wherein 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.
- An eighth feature is summarized as the production method according to any one of the first feature to the seventh feature, wherein the step C includes: taking the normal component out of the closed space by using water having a first temperature as the second solvent; and taking the normal component out of the closed space by bubbling while adding CO 2 gas to a water having a second temperature as a second solvent, the second temperature being lower than the first temperature.
- a ninth feature is summarized as the production method according to any one of the first feature to the eighth feature, wherein the step A comprises a step in which the tobacco source is subjected to a water addition treatment.
- a tenth feature is summarized as the production method according to the ninth feature, wherein in the step A, an amount of water in the tobacco source before heating the tobacco source becomes 30 wt% or more by the water addition treatment.
- a eleventh feature is summarized as the production method according to any one of the first feature to the tenth feature, wherein the step A comprises a step for adding a non-aqueous solvent to the tobacco raw material.
- a twelfth feature is summarized as the production method according to the eleventh feature, wherein the amount of the non-aqueous solvent is 10 wt% or more with respect to the tobacco raw material.
- a thirteenth feature is summarized as the production method according to the eleventh feature or twelfth feature, the step A comprises a step for adding the non-aqueous solvent and water to the tobacco raw material.
- a fourteenth feature is summarized as the production method according to any one of the first feature to the thirteenth feature, wherein a temperature of the first solvent is 10°C or more and 40°C or less.
- the volume of the closed space recited in the first feature not be extremely different from the volume of a tobacco raw material from the viewpoint of reducing the loss of a tobacco raw material by reducing the inner surface of the closed space. It is also preferred that the volume of the closed space recited in the first feature not be extremely different from the volume of a tobacco raw material from the viewpoint of efficient washing. It is preferred that the shape of the closed space recited in the first feature not contain an extremely long part and the like from the viewpoint of reducing the loss of a tobacco raw material by reducing the inner surface of the closed space. It is also preferred that the shape of the closed space recited in the first feature not contain an extremely long part and the like from the viewpoint of efficient washing.
- the volume of the closed space be for example 3 times or more and 50 times or less the volume of a tobacco raw material.
- the lengths of the longest parts in the X direction, the Y direction and the Z direction which are directions intersecting each other at 90 degrees in the closed space are considered as X, Y and Z respectively and two values between X, Y and Z which differ most are used as L and S (S is a value smaller than L), L be 10 times or less higher than S.
- the loss of a tobacco raw material can be reduced, and further a tobacco raw material (residue) can be sufficiently washed in Step C recited in the first feature using a moderate amount of solvent while moderately stirring the tobacco raw material.
- Fig. 1 and Fig. 2 are diagrams showing an example of the production device according to the first embodiment.
- the treatment device 10 has a container 11 and a spray 12.
- a tobacco raw material 50 is put in the container 11.
- the container 11 is constituted of for example members with heat resistance and pressure resistance (e.g. SUS; Steel Used Stainless). It is preferred that the container 11 constitute a closed space.
- the "closed space” is a space to prevent the contamination of the space by solid foreign substances in normal handling (e.g. treatment action, transportation, storage, etc.) and inhibit the movement of a flavor constituent (e.g. a nicotine component) contained in the tobacco raw material 50 to the outside of the space. Therefore, a tobacco raw material is maintained in a sanitary condition and it is not required to transfer the tobacco raw material, and therefore the loss of the tobacco raw material decreases.
- the treatments for intentionally taking a predetermined component to the outside of the space like for example Step S30 (capture treatment) and Step S60 (washing) described below are not contrary to the definition of the above-described "closed space”.
- a nicotine component is an example of a flavor constituent contributing to a tobacco smoking flavor and is used as an index of the flavor constituent in the embodiment.
- the spray 12 provides an alkaline substance for the tobacco raw material 50. It is preferred that a basic substance such as an aqueous solution of potassium carbonate, for example, be used as an alkaline substance.
- the spray 12 provide an alkaline substance for the tobacco raw material 50 until the pH of the tobacco raw material 50 becomes 8.0 or more. It is further preferred that the spray 12 provide an alkaline substance for the tobacco raw material 50 until the pH of the tobacco raw material 50 becomes in a range from 8.9 to 9.7.
- the amount of water in the tobacco raw material 50 after spraying of an alkaline substance is preferably 10 wt% and further preferably 30 wt% or more.
- the upper limit of the amount of water in the tobacco raw material 50 is not particularly limited, and is for example preferably 50 wt% or less in order to efficiently heat the tobacco raw material 50.
- the initial amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 be 2.0 wt% or more in the case where the gross weight of the tobacco raw material 50 in the dry state is 100 wt%. It is further preferred that the initial amount of flavor constituent (herein, a nicotine component) contained be 4.0 wt% or more.
- Nicotiana raw materials such as Nicotiana. tabacum and Nicotiana. rustica can be used.
- Nicotiana tabacum for example, a variety such as Burley type or flue cured type can be used.
- a tobacco raw material of a type other than Burley type and flue cured type may be also used.
- the tobacco raw material 50 may be constituted of a cut or powder tobacco raw material.
- the diameter of a cut or powder substance is preferably 0.5 mm to 1.18 mm.
- the capturing device 20 has a container 21, a pipe 22, a release section 23 and a pipe 24.
- a capture solvent 70 (i.e. a first solvent) is put in the container 21.
- the container 21 is constituted of a member that has resistance to the capture solvent, volatile flavor constituent and volatile impurity components (for example a glass or a stainless steel (SUS)). It is preferred that the container 21 constitute of an airtight space to a degree in which the movement of air to the outside of the space can be inhibited.
- the temperature of the capture solvent 70 is for example normal temperature.
- the lower limit of normal temperature is for example a temperature at which the capture solvent 70 is not solidified, preferably 10°C.
- the upper limit of normal temperature is for example 40°C or less.
- any acid such as malic acid or citric acid may be added to the capture solvent 70.
- a solvent such as an aqueous solution of citric acid may be added to the capture solvent 70. That is, the capture solvent 70 may be constituted of several types of solvents.
- the initial pH of the capture solvent 70 is preferably lower than the pH of the tobacco raw material 50 after an alkali treatment.
- the temperature of the container 21 may be cooled to a temperature lower than normal temperature (for example, 5°C).
- the pipe 22 takes a release component 61, which is released in the gas phase from the tobacco raw material 50 by heating the tobacco raw material 50, to the capture solvent 70.
- the release component 61 contains at least a nicotine component which is an index of a flavor constituent. Since the tobacco raw material 50 has treated with alkali, the release component 61 contains ammonium ion in some cases depending on time elapsing from the beginning of the capture step of a flavor constituent (treatment time). The release component 61 contains TSNA in some cases depending on time elapsing from the beginning of the capture step (treatment time).
- a release section 23 is provided on the tip of the pipe 22 and immersed in the capture solvent 70.
- the release section 23 has a plurality of openings 23A.
- the release component 61 taken by the pipe 22 is released in the capture solvent 70 from a plurality of openings 23A as a foam-like release component 62.
- the pipe 24 takes a residual component 63 which has not been captured by the capture solvent 70 to the outside of the container 21.
- the release component 62 is a component which is released in the gas phase by heating the tobacco raw material 50, there is a possibility that the temperature of the capture solvent 70 is raised by the release component 62. Therefore, the capturing device 20 may have a function for cooling the capture solvent 70 to maintain the temperature of the capture solvent 70 to normal temperature.
- the capturing 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 illustrating an example of the application of a flavor constituent.
- a flavor constituent is provided for a constituent of a favorite item (e.g. a flavor source for a flavor inhaler).
- a flavor inhaler 100 has a holder 110, a carbon heat source 120, a flavor source 130 and a filter 140.
- the holder 110 is for example a paper pipe with a tubular shape.
- the carbon heat source 120 generates heat to heat the flavor source 130.
- the flavor source 130 is a substance to generate a flavor and is an example of a base material for a flavor source for which a flavor constituent is provided.
- the filter 140 inhibits the introduction of impurity substances to the mouthpiece side.
- the flavor inhaler 100 is described herein as an example of the application of a flavor constituent, but the embodiments are not limited thereto.
- a flavor constituent may be applied to other inhalers, for example, an aerosol source for electronic cigarettes (what is called E-liquid).
- a flavor constituent may be provided for base materials for a flavor source such as gum, tablets, films and candy.
- Fig. 4 is a flow diagram showing the production method involved in the first embodiment.
- an alkaline substance is provided for the tobacco raw material 50 using the above-described treatment device 10 in Step S10.
- a basic substance such as an aqueous solution of potassium carbonate can be used.
- the initial amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 be 2.0 wt% or more in the case where the gross weight of the tobacco raw material 50 in the dry state is 100 wt%. It is further preferred that the initial amount of flavor constituent (herein, a nicotine component) contained be 4.0 wt% or more.
- the pH of the tobacco raw material 50 after an alkali treatment is preferably 8.0 or more as described above. Further preferably, the pH of the tobacco raw material 50 after an alkali treatment is preferably in a range from 8.9 to 9.7.
- Step S20 the tobacco raw material 50 which has been treated with alkali is heated in a closed space (in the above-described container 11 in the embodiment) to take a flavor constituent which is released in the gas phase from the tobacco raw material 50 to the outside of the closed space.
- the tobacco raw material 50 can be heated with the container 11 with the tobacco raw material 50 put in the container 11 in the treatment device 10. In such case, it is needless to say that the pipe 22 in the capturing device 20 is attached to the container 11.
- the heating temperature of the tobacco raw material 50 is in a range from 80°C or more to less than 150°C. By setting the heating temperature of the tobacco raw material 50 to 80°C or more, a time when a flavor constituent is sufficiently released from the tobacco raw material 50 can be earlier. By setting the heating temperature of the tobacco raw material 50 to less than 150°C, meanwhile, a time when TSNA is released from the tobacco raw material 50 can be delayed.
- the tobacco raw material 50 may be subjected to a water addition treatment before heating the tobacco raw material 50.
- a water addition treatment may be carried out in Step S10 or may be carried out before heating the tobacco raw material 50 in Step S20.
- the water addition treatment may be carried out in the process of heating the tobacco raw material 50 in Step S20 to supplement water which decreases by heating the tobacco raw material 50 in Step S20.
- the water addition treatment may be intermittently carried out at least once or more.
- the water addition treatment may be successively carried out over a predetermined period.
- the amount of water in the tobacco raw material 50 before heating the tobacco raw material 50 is preferably 30 wt% or more.
- the upper limit of the amount of water in the tobacco raw material 50 is not particularly limited, and for example preferably 50 wt% or less to efficiently heat the tobacco raw material 50.
- Step S20 preferably comprises the step for adding a non-aqueous solvent to the tobacco raw material 50.
- the amount of non-aqueous solvent is preferably 10 wt% or more and 50 wt% or less with respect to the tobacco raw material 50. Therefore, impurity substances soluble in such non-aqueous solvent under the heating condition move from the tobacco raw material 50 to the non-aqueous solvent through the liquid phase, and thus the impurity substances can be efficiently removed in Step S60 (washing treatment) described below.
- the non-aqueous solvent may be a solvent other than water. Specific examples of non-aqueous solvents include glycerin, propylene glycol, ethanol, alcohol, acetonitrile, hexane and the like.
- the non-aqueous solvent and further water may be added to the tobacco raw material 50.
- the time for adding a non-aqueous solvent to the tobacco raw material 50 may be a time before Step S20 (heating treatment) is completed.
- the time for adding a non-aqueous solvent to the tobacco raw material 50 may be a time between Step S10 (alkali treatment) and Step S20 (heating treatment).
- the time for adding a non-aqueous solvent to the tobacco raw material 50 may be a time in the process of Step S20 (heating treatment).
- the non-aqueous solvent is preferably a solvent which is not substantially vaporized at the heating temperature in Step S20 (heating treatment). Therefore, such non-aqueous solvent and impurity substances dissolved in the non-aqueous solvent can be inhibited from contaminating a capture solvent in Step S30 described below.
- the tobacco raw material 50 When the tobacco raw material 50 is heated in Step S20, the tobacco raw material 50 may be subjected to a water addition treatment.
- the amount of water in the tobacco raw material 50 is preferably maintained to 10% or more and 50% or less by the water addition treatment.
- water may be successively added to the tobacco raw material 50.
- the amount of water added is preferably adjusted so that the amount of water in the tobacco raw material 50 is 10% or more and 50% or less.
- the above-described non-aqueous solvent may be added to the tobacco raw material 50 during the water addition treatment.
- the tobacco raw material 50 be subjected to an aeration treatment in Step S20. Therefore, the amount of flavor constituent contained in the release component 61 which is released in the gas phase from the alkali-treated tobacco raw material 50 can be increased.
- the aeration treatment for example, saturated water vapor at 80°C is brought into contact with the tobacco raw material 50.
- the aeration time in the aeration treatment varies depending on a device for treating the tobacco raw material 50 and the amount of tobacco raw material 50, and thus cannot be necessarily specified, and for example, the aeration time is within 300 minutes when the tobacco raw material 50 is 500 g.
- the gross aeration volume in the aeration treatment also varies depending on a device for treating the tobacco raw material 50 and the amount of tobacco raw material 50, and thus cannot be necessarily specified, and for example, the volume is about 10 L/g when the tobacco raw material 50 is 500 g.
- Air used in the aeration treatment is not necessarily saturated water vapor.
- the amount of water in air used in the aeration treatment may be adjusted so that water contained in the tobacco raw material 50 to which the heating treatment and the aeration treatment have been applied is for example less than 50% without particularly requiring the humidification of the tobacco raw material 50.
- the gas used in the aeration treatment is not limited to air and may be inert gases such as nitrogen and argon.
- Step S30 i.e. step B2
- the capture solvent 70 a first solvent which is a liquid substance at normal temperature on the outside of the closed space (the outside of the above-described container 11 in the embodiment), that is, in the capturing device 20 in the embodiment to allow the capture solvent 70 to capture the flavor constituent.
- Step S20 and Step S30 are shown as different treatments in Fig. 4 for the convenience of illustration, but Step S20 and Step S30 are treatments which are carried out in parallel. Being carried out in parallel means that the period to carry out Step S30 overlaps with the period to carry out Step S20, and it should be noted that Step S20 and Step S30 do not need to start and finish at the same time.
- the pressure in the container 11 in the treatment device 10 is not more than normal pressure.
- the upper limit of the pressure in the container 11 in the treatment device 10 is +0.1 MPa or less as gauge pressure.
- a reduced pressure atmosphere may be inside the container 11 in the treatment device 10.
- the capture solvent 70 for example, glycerin, water or ethanol can be used as described above.
- the temperature of the capture solvent 70 is normal temperature as described above.
- the lower limit of normal temperature is for example a temperature at which the capture solvent 70 is not solidified, preferably 10°C.
- the upper limit of normal temperature is for example 40°C or less.
- Step S40 in order to increase the concentration of a flavor constituent contained in a capture solution, the capture solvent 70 having captured the flavor constituent is subjected to a vacuum concentration treatment, a heating concentration treatment or a salting-out treatment. It should be noted however that the treatment of Step S40 (concentration treatment) is not essential and may be omitted.
- the vacuum concentration treatment is preferably carried out in an airtight space to a degree in which the movement of air to the outside of the space can be inhibited. Therefore, contact with air is limited, and it is not required that the capture solvent 70 be raised to a high temperature, and thus there is a little concern about changes in components. Therefore, types of capture solvent which can be used increase by using vacuum concentration.
- the concentration of a flavor constituent can be increased; however, the flavor constituent is divided fifty-fifty between the liquid solvent phase/water phase, and thus the yield rate of the flavor constituent is low.
- a hydrophobic substance such as MCT
- Step S50 the tobacco raw material 50 which a flavor constituent has been released in Step S20 is prepared. It should be noted that the tobacco raw material 50 is still maintained in the closed space (in the above-described container 11 in the embodiment).
- Step S60 i.e. step C2
- a washing solvent (a second solvent) is supplied to the tobacco raw material 50 in the closed space (in the above-described container 11 in the embodiment), and a normal component which is released as the liquid phase from the tobacco raw material 50 to the washing solvent is taken with the washing solvent to the outside of the closed space (the outside of the above-described container 11 in the embodiment).
- Step S30 After a flavor constituent which has been contained in the tobacco raw material 50 is taken out in Step S30 (capture treatment), the residue from which the flavor constituent has been taken is washed with a washing solvent in Step S60 (washing treatment). Therefore, normal component (impurity substances) remaining in the tobacco raw material 50 (residue) are removed. Since the production method involved in the embodiment comprises Step S60 (washing treatment), unnecessary impurity substances can be simply removed from the tobacco raw material 50 (residue).
- washing modes can include a mode in which a washing solvent is sprayed to the tobacco raw material 50 (residue) from the spray 12 and then the container 11 is rotated and shaken for about 10 to 60 minutes to carry out washing.
- the weight ratio of tobacco raw material 50 (residue) and washing solvent (washing solvent/residue) can include 10 to 20 when the tobacco raw material 50 (residue) is considered as 1.
- the washing solvent used in Step S60 can include aqueous solvents, and specific examples thereof can be pure water and ultrapure water, and can include city water.
- the temperature of the washing solvent can include between normal temperature (e.g. 20°C ⁇ 15°C) and 70°C.
- an aqueous solvent used as a washing solvent
- those through which CO 2 gas is bubbled may be used, and specifically can include carbonated water and an aqueous solution containing oversaturated CO 2 gas.
- an aqueous solvent for example, water through which ozone is bubbled can be used.
- Step S60 (washing treatment) may be repeated at least twice or more.
- n is an integer of 1 or more
- a solvent A is used as a washing solvent in the n-th step
- a solvent B different from the solvent A may be used as a washing solvent in the n + 1-th step.
- Step S60 (washing treatment) is repeated 3 times or more
- three types or more of solvent may be used as a washing solvent.
- Step S60 (washing treatment) is repeated 3 times or more, the same solvent may be used in Step S60 (washing treatment) twice or more.
- washing is initially carried out with water, and then washing may be carried out with an aqueous solvent through which CO 2 gas is bubbled. Each washing may be carried out several times. When washing is carried out by such procedure and aqueous solvent, impurity substances are efficiently removed.
- step S60 may be repeated at least two or more times using second solvents having respectively different temperatures.
- step S60 may include a step of bubbling while adding CO 2 gas to the second solvent having the lowest temperature among the respectively different temperatures.
- step S60 may include a step of bubbling while adding CO 2 gas to the second solvent with a temperature of 20°C or less.
- step S60 may include a step in which water with a first temperature (for example, from 40 to 80°C) as a second solvent is used to take a normal component out of the closed space (below, a first washing step), and a step in which water with a second temperature (for example, from 10 to 15°C) lower than that of the first temperature as a second solvent is used and bubbling is performed while adding CO 2 gas to water with the second temperature to take a normal component out of the closed space (below, a second washing step).
- a first temperature for example, from 40 to 80°C
- a second temperature for example, from 10 to 15°C
- the alkaline substances the basic substances such as potassium carbonate aqueous solution
- the first washing step may be performed more than two times.
- the second washing step may be performed more than two times.
- non-aqueous solvents such as propylene glycol, glycerin, ethanol, MCT), hexane, methanol and acetonitrile can be also used aside from the above-mentioned aqueous solvents. In addition, these can be used by mixing the above-mentioned aqueous solvents.
- an acidic solvent may be used as a washing solvent.
- carboxylic acid such as acetic acid or malic acid may be mentioned as the acidic solvent.
- the residue may be subjected to a drying treatment.
- a drying condition an mode in which drying is carried out at a temperature of about 110 to 125°C for about 100 to 150 minutes with air circulated (ventilation amount 10 to 20 L/min/250 g) can be mentioned.
- Step S60 washing treatment
- types of impurity component can be differentiated due to high affinity with a washing solvent, and several types of impurity component can be removed.
- Step S60 washing treatment
- Step S70 return treatment
- Step S70 a capture solvent (first solvent) having captured a flavor constituent in Step S30 is added to the tobacco raw material 50 which the flavor constituent has been released to the outside of the closed space in Step S20 (the washed residue of the tobacco raw material) in the closed space (in the above-described container 11 in the embodiment).
- the capture solvent (first solvent) which is added to the tobacco raw material 50 (the washed residue of the tobacco raw material) may be neutralized in Step S70.
- the tobacco raw material containing a flavor constituent may be neutralized.
- Step S40 concentration treatment
- step S70 may be performed outside of the closed space (in the embodiment, outside of the above-described container 11).
- a grinding treatment and a granule forming treatment for the residue obtained from the washing treatment in step S60 (the washing treatment) may be performed.
- the grinding treatment for example, is a process of grinding the washed residue of the tobacco raw material, while adding a binder to the ground residue, and mixing the ground residue and the binder.
- the granule forming treatment for example, is a process of sizing and drying the mixture while stirring with a mixer, after kneading and extruding the mixture of the ground residue and the binder.
- the granule forming treatment may be performed simultaneously with step S70 (the return treatment).
- a capture solvent is allowed to capture a flavor constituent contained in a tobacco raw material by Step S20 (heating treatment) and Step S30 (capture treatment), and by carrying out Step S70 (return treatment) for adding the capture solvent having captured the flavor constituent to a tobacco raw material, impurities such as ammonia contained in the tobacco raw material can be selectively reduced by a simple and low-cost process.
- Step S60 washing treatment for washing a tobacco raw material is carried out prior to Step S70 (return treatment) for adding a capture solvent having captured a flavor constituent to a tobacco raw material. Therefore, impurity components such as TSNA are further selectively reduced.
- Step S20 heating treatment
- Step S60 washing treatment
- the modified example 1 of the first embodiment will be described below. Differences from the first embodiment will be mainly described below.
- Step S30 capture treatment is carried out until any time from when the first condition is satisfied to when the second condition is satisfied.
- the first condition is a condition that when, after the pH of a capture solution containing the capture solvent 70 and the release component 62 decreases by 0.2 or more from the maximum value, a stable zone in which variations in the pH of the capture solution are within a predetermined range exists in the time axis elapsing from the beginning of Step S20, the time elapsing from the beginning of Step S20 (hereinafter, treatment time) reaches the start time of the stable zone.
- the stable zone is a zone in which variations in the pH of a capture solution are within a predetermined range (e.g. the average variation per unit of time is ⁇ 0.01/min), and in such zone, the range of variation in the pH of a capture solution is within a predetermined range (e.g. a difference between pH at a time when such zone starts and pH at a time when the second condition described below is satisfied is ⁇ 0.2).
- the start time of the stable zone is for example a time when the pH of the capture solution stops decreasing.
- the profile of the pH of a capture solution is measured in advance in the same conditions as in the actual treatments, and the pH of a capture solution is preferably replaced with treatment time. That is, the first condition is preferably replaced with treatment time. Therefore, it is not required to monitor variations in the pH of a capture solution in real time and ammonium ion (NH 4 + ) can be removed from the capture solution by simple control.
- the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.3 wt%. Further preferably, the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.4 wt%.
- the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.6 wt%.
- the profile of the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 is measured in advance in the same conditions as in the actual treatments, and the remaining amount of flavor constituent is preferably replaced with treatment time. That is, the second condition is preferably replaced with treatment time. Therefore, it is not required to monitor the remaining amount of flavor constituent in real time and an increase in the amount of TSNA contained in a capture solvent can be inhibited by simple control.
- the total amount of saccharides contained in the tobacco raw material 50 is 10.0 wt% or less in the case where the gross weight of the tobacco raw material 50 in the dry state is 100 wt%.
- the saccharides contained in the tobacco raw material 50 are fructose, glucose, saccharose, maltose and inositol. Therefore, the stable zone of pH showing that the concentration of ammonium ion in a capture solution was sufficiently reduced can be clearly confirmed.
- Step S30 for bringing a release component into contact with the capture solvent 70 is continued at least until the first condition is satisfied. Therefore, ammonium ion (NH 4 + ) contained in the release component is sufficiently removed from the capture solution.
- other volatile impurity components specifically, acetaldehyde, pyridine
- acetaldehyde, pyridine showing the same behavior as of ammonium ion
- Step S30 for bringing a release component into contact with the capture solvent 70 is finished at least by the time when the second condition is satisfied. Therefore, by finishing S30 prior to the amount of TSNA released increases, an increase in the amount of TSNA contained in a capture solution is inhibited.
- Step S20 and Step S30 by simple treatments such as Step S20 and Step S30, as contamination by impurity components such as ammonium ion (NH 4 + ) and TSNA is inhibited, a flavor constituent can be sufficiently extracted. That is, a flavor constituent can be extracted by a simple device.
- impurity components such as ammonium ion (NH 4 + ) and TSNA
- non-volatile components contained in the tobacco raw material 50 do not move to a capture solvent, and only components volatilized at about 120°C can be captured in the capture solvent, and thus components captured by a capture solvent can be used as an aerosol source for electronic cigarettes. Therefore, as an increase in volatile impurity components such as ammonium ion, acetaldehyde and pyridine is inhibited in electronic cigarettes, aerosol containing a tobacco flavor can be delivered to users, and further the movement of non-volatile components to the capture solvent is inhibited, and thus scorching of a heater to heat an aerosol source, and the like can be inhibited.
- volatile impurity components such as ammonium ion, acetaldehyde and pyridine
- electrostatic cigarette herein indicates a non-combustion type flavor inhaler or aerosol inhaler which comprises an electric heater to heat and atomize a liquid aerosol source and an aerosol source and is to deliver aerosol to users (e.g. an aerosol inhaler described in Japanese Patent No. 5196673 , an aerosol electronic cigarette described in Japanese Patent No. 5385418 , etc.)
- the modified example 2 of the first embodiment will be described below. Differences from the first embodiment will be mainly described below.
- Step S30 capture treatment is carried out until any time from when the first condition is satisfied to when the second condition is satisfied.
- the first condition is a condition that, in the case where the weight of the tobacco raw material in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material decreases until reaching 1.7 wt%.
- the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.3 wt%. Further preferably, the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.4 wt%.
- the second condition is a condition that, in the case where the weight of the tobacco raw material 50 in the dry state is 100 wt%, the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 decreases until reaching 0.6 wt%.
- the profile of the remaining amount of flavor constituent (herein, a nicotine component) contained in the tobacco raw material 50 is measured in advance in the same conditions as in the actual treatments, and the remaining amount of flavor constituent is preferably replaced with treatment time. That is, the second condition is preferably replaced with treatment time. Therefore, it is not required to monitor the remaining amount of flavor constituent in real time and an increase in the amount of TSNA contained in a capture solvent can be inhibited by simple control.
- Step S30 for bringing a release component into contact with the capture solvent 70 is continued at least until the first condition is satisfied. Therefore, Step S30 is continued in a zone in which the decrease rate of the remaining amount of flavor constituent contained in a tobacco raw material (i.e. a rate at which a nicotine component is volatilized from the tobacco raw material 50) is not less than a predetermined rate, and therefore the flavor constituent can be efficiently recovered.
- Step S30 for bringing a release component into contact with the capture solvent 70 is finished at least by the time when the second condition is satisfied. Therefore, by finishing S30 before the amount of TSNA released increases, an increase in the amount of TSNA contained in a capture solution is inhibited.
- Step S20 and Step S30 As described above, by the simple treatments such as Step S20 and Step S30, as contamination by impurity components such as TSNA is inhibited, a flavor constituent can be sufficiently extracted. That is, a flavor constituent can be extracted by a simple device.
- non-volatile components contained in the tobacco raw material 50 do not move to a capture solvent, and only components volatilized at about 120°C can be captured in the capture solvent, and thus components captured by a capture solvent can be used as an aerosol source for electronic cigarettes. Therefore, as an increase in volatile impurity components such as ammonium ion, acetaldehyde and pyridine is inhibited in electronic cigarettes, aerosol containing a tobacco flavor can be delivered to users, and further the movement of non-volatile components to a capture solvent is inhibited, and thus scorching of a heater to heat an aerosol source, and the like can be inhibited.
- volatile impurity components such as ammonium ion, acetaldehyde and pyridine
- electrostatic cigarette herein indicates a non-combustion type flavor inhaler or aerosol inhaler which comprises an electric heater to heat and atomize a liquid aerosol source and an aerosol source and is to deliver aerosol to users (e.g. an aerosol inhaler described in Japanese Patent No. 5196673 , an aerosol electronic cigarette described in Japanese Patent No. 5385418 , etc.).
- samples (Sample A to Sample D) shown in Fig. 5 were prepared and the pH of a capture solution and ammonium ion (NH 4 + ) contained in a capture solution were measured under the following conditions.
- the amount of nicotine (Nic. amount) and the amount of ammonium ion (NH 4 + amount) contained in Sample A to Sample D in the dry state are as shown in Fig. 5 .
- the amount of every saccharide (fructose, glucose, saccharose, maltose and inositol) contained in Sample A is almost zero (less than the detection limit)
- the total amount of saccharides (fructose, glucose, saccharose, maltose and inositol) contained in Sample B is 9.37 wt%
- the total amount of saccharides (fructose, glucose, saccharose, maltose and inositol) contained in Sample C is 18.81 wt%
- the amount of saccharides (fructose, glucose, saccharose, maltose and inositol) contained in Sample D is 0.02 wt%.
- the measurement results of the pH of a capture solution are as shown in Fig. 6
- the measurement results of ammonium ion (NH 4 + ) contained in a capture solution are as shown in Fig. 7 .
- the treatment time is a time elapsing from the beginning of the heating treatment (S20) of a tobacco raw material. It can be thought that the treatment time is a time elapsing from the beginning of the capture treatment (S30) of a flavor constituent (hereinafter, a nicotine component).
- the gas used in the bubbling treatment is the atmosphere at about 20°C and about 60%-RH.
- the stable zone is a zone in which variations in the pH of a capture solution is within a predetermined range (e.g. the average variation per unit of time is ⁇ 0.01/min) as described above, and in such zone, the range of variation in the pH of a capture solution is within a predetermined range (e.g. a difference between pH at a time when such zone starts and pH at a time when the second condition described below is satisfied is ⁇ 0.2).
- a predetermined range e.g. the average variation per unit of time is ⁇ 0.01/min
- volatile impurity components specifically, acetaldehyde, pyridine
- volatile impurity components showing the same release and capture behavior as of ammonium ion (NH 4 + ) are also reduced at the same time, and thus volatile impurity components (specifically, acetaldehyde, pyridine) are easily reduced.
- a sample of burley type tobacco raw material (the above-described Sample A) was prepared, and the remaining amount of alkaloid (herein, a nicotine component) contained in the tobacco raw material in the dry state (hereinafter, nicotine concentration in tobacco raw material), and the concentration of TSNA contained in a capture solution (hereinafter, TSNA concentration in capture solution) were measured under the following conditions.
- a nicotine component contained in the tobacco raw material in the dry state
- TSNA concentration in capture solution hereinafter, TSNA concentration in capture solution
- the measurement results of the nicotine concentration in tobacco raw material are as shown in Fig. 8
- the measurement results of the concentration of TSNA contained in a capture solution are as shown in Fig. 9 .
- the remaining amount of nicotine component contained in a tobacco raw material is represented by percent by weight in a case where the weight of a tobacco raw material in the dry state is 100 wt%.
- the concentration of TSNA contained in a capture solution is represented by percent by weight in a case where a capture solution is 100 wt%.
- the treatment time is a time elapsing from the beginning of the heating treatment (S20) of a tobacco raw material. It can be also thought that the treatment time is a time elapsing from the beginning of the capture treatment (S30) of a nicotine component.
- NNK 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone
- NNN N'-nitrosonornicotine
- NAT N'-nitrosoanatabine
- NAB N'-nitrosoanabasine
- the gas used in the bubbling treatment is the atmosphere at about 20°C and about 60%-RH.
- the remaining amount of nicotine component contained in a tobacco raw material intermittently decreases in the profile of the nicotine concentration in tobacco raw material.
- Fig. 9 it was verified that NNK did not change but NNN, NAT and NAB increased after a lapse of a fixed period in the profile of the concentration of TSNA.
- Such experimental results verified that preferably the heating treatment (S20) and the capture treatment (S30) were finished before the time when the nicotine concentration in tobacco raw material reaches 0.3 wt%. That is, it was verified that preferably the second condition was that the nicotine concentration in tobacco raw material decreases until reaching 0.3 wt%. It was verified that further preferably the heating treatment (S20) and the capture treatment (S30) were finished before the time when the nicotine concentration in tobacco raw material reaches 0.4 wt%. That is, it was verified that further preferably the second condition was that the nicotine concentration in tobacco raw material decreases until reaching 0.4 wt%.
- the heating treatment (S20) and the capture treatment (S30) were finished before the time when the nicotine concentration in tobacco raw material reaches 0.6 wt%. That is, it was verified that further preferably the second condition was that the nicotine concentration in tobacco raw material decreases until reaching 0.6 wt%.
- Sample P to Sample Q were prepared and the pH of a capture solution and the concentration of alkaloid (herein, a nicotine component) in a 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 results of the pH of a capture solution are as shown in Fig. 10 .
- the measurement results of the concentration of nicotine component contained in a capture solution are as shown in Fig. 11 .
- the treatment time is a time elapsing from the beginning of the heating treatment (S20) of a tobacco raw material. It can be thought that the treatment time is a time elapsing from the beginning of the capture treatment (S30) of a nicotine component.
- the gas used in the bubbling treatment is the atmosphere at about 20°C and about 60%-RH.
- the weight of ammonium ion and pyridine contained in a capture solution was measured by changing the temperature of a capture solvent under the following conditions.
- the weight of ammonium ion contained in a capture solution is as shown in Fig. 12 .
- the weight of pyridine contained in a capture solution is as shown in Fig. 13 .
- the temperature of a capture solvent is the preset temperature of the chiller (a constant-temperature bath) controlling the temperature of a container containing the capture solvent. It should be noted that the temperature of a capture solvent is settled about 60 minutes after the container is set in the chiller and the temperature control starts.
- a capture solution was left to stand in a sealed container until room temperature in a laboratory controlled at room temperature of 22°C to harmonize the temperature. After harmonization, the lid was opened, and the glass electrode of a pH meter (SevenEasy S20 manufactured by METTLER TOLEDO) was soaked in a capture solution to start the measurement.
- the pH meter was calibrated in advance using pH meter calibration liquids with pH 4.01, 6.87 and 9.21. A point at which output variations from a sensor become stable within 0.1 mV for 5 seconds was used as the pH of a capture solution.
- a capture solution was collected in an amount of 50 ⁇ L, and diluted by adding 950 ⁇ L of a 0.05 N aqueous solution of dilute sulfuric acid, and the diluted solution was analyzed by ion chromatography to quantitate ammonium ion contained in the capture solution.
- the measurement was carried out in a method in accordance with the German Institute for Standardization (DIN) 10373. That is, a tobacco raw material was collected in an amount of 250 mg, and 7.5 mL of a 11% aqueous solution of sodium hydroxide and 10 mL of hexane were added thereto, and shaking extraction was carried out for 60 minutes. After the extraction, the hexane phase, supernatant, was used for a gas chromatograph mass spectrometer (GC/MS) to quantitate the weight of nicotine contained in the tobacco raw material.
- GC/MS gas chromatograph mass spectrometer
- a tobacco raw material was collected in an amount of 250 mg, and 10 mL of methanol was added thereto, and shaking extraction was carried out for 60 minutes. After the extraction, the extract liquid was filtered with a 0.45 ⁇ m membrane filter, and used for a gas chromatograph with thermal conductivity detector (GC/TCD) to quantitate the amount of water contained in the tobacco raw material.
- GC/TCD gas chromatograph with thermal conductivity detector
- the weight of the tobacco raw material in the dry state is calculated by subtracting the above-described amount of water from the gross weight of the tobacco raw material.
- a capture solution was collected in an amount of 0.5 mL, and diluted by adding 9.5 mL of a 0.1 M aqueous solution of ammonium acetate, and the diluted solution was analyzed by a high performance liquid chromatograph-mass spectrometer (LC-MS/MS) to quantitate TSNA contained in the capture solution.
- LC-MS/MS high performance liquid chromatograph-mass spectrometer
- Step S10 alkali treatment
- Step S60 washing treatment
- the embodiment is not however limited thereto.
- a tobacco raw material which has been subjected to the alkali treatment and water addition treatment in advance is placed in the container 11 and Step S20 (heating treatment), Step S30 (capture treatment) and Step S60 (washing treatment) may be carried out.
- the volume of a closed space formed by the container 11 used in Step S20 (heating treatment) and Step S60 (washing treatment) not be extremely different from the volume of a tobacco raw material from the viewpoint of reducing the loss of a tobacco raw material by reducing the inner surface of the closed space, which is not described in detail in the embodiment. It is also preferred that the volume of the closed space not be extremely different from the volume of a tobacco raw material from the viewpoint of efficient washing. It is preferred that the shape of the closed space formed by the container 11 not contain an extremely long part and the like from the viewpoint of reducing the loss of a tobacco raw material by reducing the inner surface of the closed space. It is also preferred that the shape of the closed space not contain an extremely long part and the like from the viewpoint of efficient washing.
- the volume of the closed space be for example 3 times or more and 50 times or less the volume of a tobacco raw material.
- the lengths of the longest parts in the X direction, the Y direction and the Z direction which are directions intersecting each other at 90 degrees in the closed space are considered as X, Y and Z respectively and two values between X, Y and Z which differ most are used as L and S (S is a value smaller than L), L be 10 times or less higher than S.
- Step S60 washing treatment
- the washing treatment (Step S60) is carried out prior to the return treatment (Step S70).
- the embodiment is not however limited thereto.
- the washing treatment (Step S60) may be omitted.
- a method for producing a tobacco raw material wherein the method can selectively reduce an impurity component contained in a 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)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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PCT/JP2014/078410 WO2015129098A1 (fr) | 2014-02-26 | 2014-10-24 | Procédé de production de matières premières de cigarette |
PCT/JP2015/079053 WO2016063775A1 (fr) | 2014-10-24 | 2015-10-14 | Procédé de fabrication d'ingrédient de cigarette |
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EP3207809A1 true EP3207809A1 (fr) | 2017-08-23 |
EP3207809A4 EP3207809A4 (fr) | 2018-07-04 |
EP3207809B1 EP3207809B1 (fr) | 2021-01-06 |
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EP15852051.0A Active EP3207809B1 (fr) | 2014-10-24 | 2015-10-14 | Procédé de production de matières premières de tabac |
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WO (1) | WO2016063775A1 (fr) |
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EP3437493A4 (fr) * | 2016-04-22 | 2019-12-11 | Japan Tobacco, Inc. | Procédé de production de source d'arôme |
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CA3208137A1 (fr) | 2013-05-06 | 2014-11-13 | Juul Labs, Inc. | Formulations de sel de nicotine pour des dispositifs de generation d'aerosol et methodes connexes |
EP3076805A4 (fr) | 2013-12-05 | 2017-10-11 | PAX Labs, Inc. | Formulations liquides de nicotine pour dispositifs générateurs d'aérosol et procédés correspondants |
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US20160366947A1 (en) | 2013-12-23 | 2016-12-22 | James Monsees | Vaporizer apparatus |
US10058129B2 (en) | 2013-12-23 | 2018-08-28 | Juul Labs, Inc. | Vaporization device systems and methods |
USD842536S1 (en) | 2016-07-28 | 2019-03-05 | Juul Labs, Inc. | Vaporizer cartridge |
US9549573B2 (en) | 2013-12-23 | 2017-01-24 | Pax Labs, Inc. | Vaporization device systems and methods |
US10159282B2 (en) | 2013-12-23 | 2018-12-25 | Juul Labs, Inc. | Cartridge for use with a vaporizer device |
AU2014369867A1 (en) | 2013-12-23 | 2016-06-16 | Juul Labs, Inc. | Vaporization device systems and methods |
USD825102S1 (en) | 2016-07-28 | 2018-08-07 | Juul Labs, Inc. | Vaporizer device with cartridge |
WO2015175979A1 (fr) | 2014-05-16 | 2015-11-19 | Pax Labs, Inc. | Systèmes et procédés de pulvérisation par aérosol d'un matériau pouvant être fumé |
EP3821735A1 (fr) | 2014-12-05 | 2021-05-19 | Juul Labs, Inc. | Commande de dose graduée |
MX2018009702A (es) | 2016-02-11 | 2019-07-08 | Juul Labs Inc | Cartucho rellenable de vaporizador y metodo de relleno. |
BR112018016402B1 (pt) | 2016-02-11 | 2023-12-19 | Juul Labs, Inc | Cartuchos de fixação segura para dispositivos vaporizadores |
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USD848057S1 (en) | 2016-06-23 | 2019-05-07 | Pax Labs, Inc. | Lid for a vaporizer |
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EP3437493A4 (fr) * | 2016-04-22 | 2019-12-11 | Japan Tobacco, Inc. | Procédé de production de source d'arôme |
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EP3207809A4 (fr) | 2018-07-04 |
EP3207809B1 (fr) | 2021-01-06 |
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