WO2019106798A1 - Article d'inhalation d'arôme - Google Patents

Article d'inhalation d'arôme Download PDF

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Publication number
WO2019106798A1
WO2019106798A1 PCT/JP2017/043131 JP2017043131W WO2019106798A1 WO 2019106798 A1 WO2019106798 A1 WO 2019106798A1 JP 2017043131 W JP2017043131 W JP 2017043131W WO 2019106798 A1 WO2019106798 A1 WO 2019106798A1
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WIPO (PCT)
Prior art keywords
activated carbon
carbon
flavor
filter
group
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PCT/JP2017/043131
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English (en)
Japanese (ja)
Inventor
正人 宮内
哲哉 吉村
祐一郎 木戸
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日本たばこ産業株式会社
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Priority to JP2019556489A priority Critical patent/JP6874152B2/ja
Priority to PCT/JP2017/043131 priority patent/WO2019106798A1/fr
Publication of WO2019106798A1 publication Critical patent/WO2019106798A1/fr

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/16—Use of materials for tobacco smoke filters of inorganic materials

Definitions

  • the present invention relates to a flavor suction article.
  • a combustion type smoking article that provides a user with a tobacco flavor by burning a tobacco flavor source as a suction article that tastes a tobacco flavor
  • a heating that provides a user with a tobacco flavor by heating without burning a tobacco flavor source
  • Type flavored suction articles and non-heated flavored suction articles are known that provide the user with a tobacco flavor source tobacco flavor without heating or burning the tobacco flavor source.
  • suction articles for which the user tastes flavors such as tobacco flavor are collectively referred to as “flavor suction articles”.
  • Flavored suction articles generally comprise a filter for filtering components derived from a flavor source, the filter comprising activated carbon as an adsorbent (see, for example, WO 2008/146543).
  • Filters containing activated carbon are called charcoal filters and are well known in the art.
  • the amount of activated carbon is determined according to the specification of the product so as to adsorb miscellaneous components but not excessively adsorb components contributing to the flavor.
  • Activated carbon is known to increase its adsorption performance as the specific surface area and pore volume increase.
  • the strength of activated carbon decreases because pores (fine pores) increase. For this reason, the present inventors noted that it is difficult to achieve both the adsorption performance and the strength of activated carbon.
  • the production of flavor suction articles in recent years is speeding up, and the load on activated carbon in the production process is increasing.
  • the activated carbon may be fractured and the amount added to the flavor suction article may be nonuniform. Keeping the added amount of activated carbon uniform is important to keep the flavor of each article uniform.
  • the present invention aims to provide a flavor suction article containing activated carbon which is excellent in adsorption performance and is stable in shape.
  • a flavor comprising activated carbon having a BET specific surface area of 1050 m 2 / g or more and a ratio of peak intensity of G band to peak intensity of D band in Raman spectrum of 0.85 or more A suction article is provided.
  • the flavor suction article containing the activated carbon which is excellent in adsorption performance and shape-stable can be provided.
  • the present inventors carried out gas phase oxidation treatment on activated carbon having a predetermined BET specific surface area, in addition to the introduction of the oxygen-containing functional group, the BET specific surface area of the activated carbon increased. Furthermore, it has been newly found that the peak intensity of the D band in the Raman spectrum is maintained or decreased. Based on such a discovery, the present inventors have completed a flavor suction article comprising activated carbon which is excellent in adsorption performance and shape stable.
  • the BET specific surface area is 1050 m 2 / g or more, and the ratio of the peak intensity of G band to the peak intensity of D band in the Raman spectrum (hereinafter also referred to as G / D ratio) is 0.85 or more
  • a flavor suction article comprising activated carbon.
  • a flavor suction article is any suction article that includes a flavor source and that the user tastes the flavor derived from the flavor source, and in particular provides flavor to the user by burning the flavor source Burnable smoking articles, heated flavor suction articles that provide the user with flavor by heating without burning the flavor source, and unheated that provide the user with the flavor source flavor without heating or burning the flavor source Type flavor suction articles are mentioned.
  • FIG. 1 is a cross-sectional view of the combustion-type smoking article 1 according to the first embodiment.
  • the combustion type smoking article 1 shown in FIG. 1 is a cigarette.
  • the combustion type smoking article 1 shown in FIG. 1 is a cigarette.
  • the tobacco rod 10 and the tipping paper 30 wound on the filter 20 are included to connect the tobacco rod 10 and the filter 20.
  • n is an integer of 2 or more filter plugs (n-1)
  • n is 2 to 4
  • n is 2 to 3
  • more preferably n is 2.
  • the tobacco rod 10 In the combustion type smoking article shown in FIG. 1, conventionally known components can be used as the tobacco rod 10, the components of the filter 20 other than the activated carbon 23, and the tip paper 30.
  • the activated carbon 23, those described below can be used.
  • the activated carbon 23 has a BET specific surface area of 1050 m 2 / g or more, and a ratio of the peak intensity of the G band to the peak intensity of the D band in the Raman spectrum is 0.85 or more.
  • BET specific surface area means a specific surface area obtained using BET adsorption isotherm (Brunauer, Emmet and Teller's equation).
  • the BET specific surface area of the activated carbon 23 is preferably 1050 to 1600 m 2 / g, more preferably 1150 to 1600 m 2 / g, and still more preferably 1150 to 1300 m 2 / g. If the BET specific surface area is too small, it is difficult for the activated carbon 23 to exhibit excellent adsorption performance. When the BET specific surface area is too large, the adsorption performance of the activated carbon 23 is enhanced, but the shape stability may be reduced.
  • the “G band” is a peak detected in the vicinity of 1600 cm ⁇ 1 in a Raman spectrum obtained by Raman spectroscopy, and the G band is derived from a graphene structure of carbon.
  • the “D band” is a peak detected in the vicinity of 1300 cm ⁇ 1 in a Raman spectrum obtained by Raman spectroscopy, and the D band is derived from a defect of a graphene structure of carbon.
  • activated carbon having a large ratio of peak intensity of G band to peak intensity of D band in Raman spectrum (hereinafter also referred to as G / D ratio) is highly crystallized, has few structural defects, and is stable in shape
  • G / D ratio peak intensity of D band in Raman spectrum
  • the Raman spectrum can be acquired, for example, using a microscopic laser Raman Nicolet Almega XR (manufactured by Thermo Fisher Scientific Co., Ltd.).
  • the G / D ratio of the activated carbon 23 is preferably 0.85 to 1.1, and more preferably 0.9 to 1.1. If the G / D ratio is too small, it is difficult for activated carbon 23 to achieve excellent shape stability.
  • the upper limit of the G / D ratio is set by the manufacturing limit of activated carbon.
  • the activated carbon 23 has, for example, an average particle diameter of 200 ⁇ m to 1000 ⁇ m, preferably an average particle diameter of 300 ⁇ m to 700 ⁇ m, and more preferably an average particle diameter of 400 ⁇ m to 600 ⁇ m.
  • the "average particle diameter” means a particle diameter (d50) at which the volume integrated value is 50% in the particle size distribution determined by the laser diffraction / scattering method.
  • the pore volume of the activated carbon 23 is preferably 0.5 cm 3 / g or more, more preferably in the range of 0.5 to 0.8 cm 3 / g, more preferably 0.52 to 0.74 cm 3 / More preferably, it is in the range of g.
  • the pore volume is too small, it is difficult for the activated carbon 23 to exhibit excellent adsorption performance. If the pore volume is too large, the adsorption performance of the activated carbon 23 may be enhanced, but the shape stability may be reduced.
  • pore volume means the sum of the volume of pores having a pore diameter of about 40 nm or less.
  • the pore volume is a value calculated from the nitrogen adsorption amount when the relative pressure P / P 0 is 0.95, in the nitrogen adsorption isotherm measured at a temperature of 77K.
  • the nitrogen adsorption isotherm can be determined as follows. First, the nitrogen gas adsorption amount (mL / mL) of activated carbon is measured for each pressure P while gradually increasing the pressure P (mmHg) of nitrogen gas in nitrogen gas at 77 K (boiling point of nitrogen). Then, the pressure P (mmHg) divided by the saturated vapor pressure P 0 (mm Hg) of nitrogen gas is taken as the relative pressure P / P 0 , and the adsorption is plotted by plotting the nitrogen gas adsorption amount against each relative pressure P / P 0 An isotherm can be obtained. The nitrogen adsorption isotherm can be obtained, for example, using a gas adsorption amount measuring apparatus AutoSorb-1 (manufactured by Quantachrome).
  • the volume of pores with a pore diameter of less than 2 nm is preferably 0.4 cm 3 / g or more, and 0.4 to 0.7 cm 3 / It is more preferably in the range of g, and still more preferably in the range of 0.4 to 0.6 cm 3 / g. It is particularly advantageous to achieve excellent adsorption performance if the activated carbon 23 has a micropore volume of the size described above.
  • micropore volume is a value calculated by performing pore distribution analysis from a nitrogen adsorption isotherm by a rapid solid density functional theory (QSDFT) method.
  • QSDFT rapid solid density functional theory
  • activated carbon 23 maintains the adsorption performance of activated carbon (hereinafter also referred to as current charcoal) currently used as an adsorbent for flavor suction articles. While, it is desired to specifically adsorb the basic component. Therefore, among all the oxygen-containing functional groups measured by the Boehm method, it is preferable that the activated carbon 23 has an oxygen-containing functional group consisting of the following on the surface thereof.
  • the activated carbon 23 is a carboxyl group (and carboxylic anhydride group) (Group I), a lactone type carboxyl group (and lactone group) (Group II), a phenolic hydroxyl group (Group III) and a carbonyl, which are measured by the Boehm method. It is preferable to have an oxygen-containing functional group consisting of a group or a quinone group (Group IV).
  • activated carbon 23 In order for activated carbon 23 to specifically adsorb the basic component, it is desirable that the amount of all the oxygen-containing functional groups be higher while maintaining the pore structure of the current carbon, but the carboxyl group (and carboxylic anhydride group) ( Since Group I) is strongly acidic, there is a concern that undesirable acid-base reactions or catalysis occur in the filter during storage of the smoking article or at the time of smoking to generate by-products. Therefore, it is particularly preferable that the activated carbon 23 have a weakly acidic oxygen-containing functional group that contributes to the adsorption of the basic component.
  • the activated carbon 23 preferably has an amount of an oxygen-containing functional group consisting of a carboxyl group, a lactone type carboxyl group, a phenolic hydroxyl group and a carbonyl group, as measured by the Boehm method, of 0.6 mmol / g or more, preferably 0.6 to 0.6 It is more preferably 2.0 mmol / g, further preferably 1.0 to 2.0 mmol / g.
  • the amount of the oxygen-containing functional group is represented by the molar amount per 1 g of activated carbon.
  • the activated carbon 23 contains the above-mentioned amount of oxygen-containing functional groups, it is advantageous in selectively adsorbing and removing a basic component (for example, ammonia) from the fluid sucked by the user at the time of suction of the flavor suction device. .
  • a basic component for example, ammonia
  • Boehm method is a known acid-base titration method, the details of which are described in the examples below.
  • the total amount of the lactone type carboxyl group and phenolic hydroxyl group measured by the Boehm method is 0.3 mmol / g or more, and the activated carbon 23 is 0.3-2.0 mmol / g. More preferably, it is 0.4 to 2.0 mmol / g.
  • the amount of carboxyl groups measured by the Boehm method is preferably 0.12 mmol / g or less, and more preferably 0.01 to 0.12 mmol / g.
  • the activated carbon 23 can be produced by subjecting a raw material activated carbon having a predetermined BET specific surface area to a gas phase oxidation treatment, as described later.
  • the activated carbon 23 produced in this manner has a large amount of oxygen-containing functional groups on the surface of the activated carbon, but among the oxygen-containing functional groups, relatively large amounts of lactone type carboxyl group (Group II) and phenolic hydroxyl group (Group III) And has a relatively small amount of carboxyl group (Group I) among the oxygen-containing functional groups.
  • the activated carbon 23 is Carbonizing and activating an organic material to obtain a raw material activated carbon; And oxidizing the raw material activated carbon by a gas phase oxidation method.
  • organic material the well-known organic material used as a raw material of activated carbon can be used, for example, a vegetable material can be used.
  • Vegetable materials are, for example, fruit shells such as coconut shells and walnut shells, wood, charcoal, bamboo and the like, and are typically coconut shells.
  • the above-mentioned organic material is carbonized and activated to obtain a raw material activated carbon.
  • Raw material activated carbon can be produced according to a known method for producing activated carbon.
  • the raw material activated carbon is produced such that the BET specific surface area is preferably 400 to 1400 m 2 / g, more preferably 1000 to 1400 m 2 / g.
  • the produced activated carbon 23 has high adsorption performance and high shape stability.
  • Raw material activated carbon may be produced by carbonizing an organic material and then activating the carbonized organic material by a gas activation method.
  • the organic material may be activated by a chemical activation method to carbonize the organic material.
  • the activation may be performed at the same time, or the organic material may be subjected to activation treatment by microwave heating to simultaneously perform carbonization and activation.
  • the above-mentioned raw material activated carbon may use commercially available activated carbon.
  • the activated carbon 23 can be manufactured by a method including oxidizing raw material activated carbon by a gas phase oxidation method.
  • the oxidation treatment by the gas phase oxidation method can be performed, for example, by treating raw activated carbon in air or steam at, for example, a temperature of 500 ° C. or less, preferably 300 to 500 ° C., for 1 to 2 hours. .
  • the oxidation treatment may be carried out by a continuous oxidation treatment or a batch oxidation treatment as described in the following examples. If the temperature of the oxidation treatment is too high, excessive activation of the raw material activated carbon proceeds, and the strength of the activated carbon decreases, which is not preferable.
  • the activated carbon 23 is under mild conditions as compared to the conditions of the oxidation treatment by the liquid phase oxidation method, specifically, under conditions where further activation of the raw material activated carbon does not significantly progress. It can manufacture by performing a gaseous-phase oxidation process to raw material activated carbon.
  • the activated carbon 23 is Carbonizing and activating the organic material to obtain a raw material activated carbon having a BET specific surface area of 1000 to 1400 m 2 / g; And oxidizing the raw material activated carbon in air or in steam at a temperature of 500 ° C. or less, preferably 300 to 500 ° C., for 1 to 2 hours.
  • the activated carbon 23 is preferably 500 ° C. or less, preferably in the air or in steam, the raw material activated carbon having a BET specific surface area of 1000 to 1400 m 2 / g. Can be produced by a method including oxidation treatment at a temperature of 300 to 500 ° C. for 1 to 2 hours.
  • Activated carbon 23 can be incorporated into the filter 20 at the loading levels employed in conventional charcoal filters. If the filter 20 has a length of 17-31 mm and a circumference of 14.7-25.8 mm, the activated carbon 23 can be incorporated into the filter 20, for example, in an amount of 20-80 mg per filter.
  • the site where the activated carbon 23 is incorporated can be a flow path of fluid (eg, mainstream smoke, aerosol, air, etc.) to be aspirated by the user when aspirating the flavor aspirator.
  • the flavored suction article comprises a filter and the activated carbon 23 is incorporated into the filter.
  • the flavor suction article comprises a flavor source, preferably a tobacco flavor source, and a filter located downstream of the flavor source, the activated carbon 23 being incorporated into the filter.
  • the site where the activated carbon 23 is incorporated is between the flow path of the mainstream smoke generated by the combustion of the tobacco flavor source 10a, that is, between the tobacco rod 10 and the end of the filter 20 on the inlet side.
  • activated carbon 23 is incorporated into the filter 20, as shown in FIGS.
  • the flavor suction device is, in addition to the activated carbon 23, a known adsorbent, for example, particles of cellulose particles or cellulose acetate, or a known flavor modifier, for example, a perfume capsule containing a perfume in a film. It may further be included.
  • a known adsorbent for example, particles of cellulose particles or cellulose acetate
  • a known flavor modifier for example, a perfume capsule containing a perfume in a film. It may further be included.
  • the hollow portion is formed between the two filter plugs 21 and the activated carbon 23 is disposed in the hollow portion.
  • the filter is made to connect the two filter plugs
  • Activated carbon 23 can also be arranged to be embedded in one of the filter plugs.
  • the activated carbon 23 is preferably incorporated into the filter plug on the upstream side of the two filter plugs.
  • FIG. 2 Such a burning type smoking article is shown in FIG. 2 as a second embodiment.
  • FIG. 2 is a cross-sectional view of the combustion-type smoking article 1 according to the second embodiment.
  • the burning type smoking article 1 shown in FIG. 2 is a cigarette.
  • FIG. 2 the same components as in FIG. 1 are given the same reference numerals.
  • the combustion type smoking article 1 shown in FIG. A tobacco rod 10 including a tobacco flavor source 10a and a cigarette paper 10b wound around the tobacco flavor source 10a;
  • the tobacco rod 10 and the tipping paper 30 wound on the filter 20 are included to connect the tobacco rod 10 and the filter 20.
  • n is an integer of 2 or more filter plugs may be arranged to be connected.
  • n is 2 to 4, preferably n is 2 to 3, and more preferably n is 2.
  • the components of the filter 20 other than the tobacco rod 10, the activated carbon 23, and the tip paper 30 may be conventionally known ones.
  • the activated carbon 23 used in the second embodiment is the same as the activated carbon 23 described in the first embodiment.
  • the flavor suction article according to the present invention contains a flavor source and the user derives the flavor derived from the flavor source It is an optional suction article that tastes like.
  • a flavor source in addition to a tobacco flavor source such as cut tobacco, a flavor such as menthol, a plant extract or an essential oil can be used.
  • the flavor suction article may be a known burning-type smoking article other than a cigarette, such as a pipe, a xel, a cigar or a cigarillo.
  • the flavor suction article may be a heating type flavor suction article that provides the user with a flavor by heating without burning the flavor source.
  • a heating type flavor suction device for example, A carbon heat source type aspirator which heats a tobacco flavor source by the heat of combustion of a carbon heat source to generate an aerosol containing a flavor component (see, for example, WO 2006/073065);
  • An electric heating type comprising: a suction unit main body including a capsule containing a liquid flavor source; and a heating device for electrically heating the suction main body, and melting the capsule outer membrane by electric heating to release the liquid flavor source Aspirator (see, for example, WO 2010/110226); or a refill type tobacco pod containing a tobacco flavor source together with an aerosol source (propylene glycol or glycerin), and an aspirator body that generates an aerosol by heating the tobacco pod by electric heating Electrically heated suction device (see, for example, WO2013 / 025921) Can be mentioned.
  • the flavor suction article may be a non-heating flavor suction article that provides the user with the flavor of the flavor source without heating or burning the flavor source, as described above.
  • a non-heating type flavor suction article a non-heating type tobacco flavor suction device (for example, a user holds a tobacco flavor derived from a normal temperature tobacco flavor source provided with a refill type cartridge containing a tobacco flavor source in a suction holder) See WO 2010/110226).
  • the flavor suction article comprises activated carbon having the following characteristics (i) and (ii): (I) BET specific surface area is 1050 m 2 / g or more; (Ii) The G / D ratio is 0.85 or more.
  • the flavored suction article comprises activated carbon that simultaneously satisfies excellent adsorption performance and shape stability. Thanks to the excellent adsorption performance of activated carbon, the flavor suction article can provide the user with excellent flavor.
  • the flavor suction article uniformly mixes the activated carbon in each lot without causing the activated carbon to be crushed in the production process, whereby the flavor of each article is uniformed. You can keep it.
  • the flavor suction article preferably contains activated carbon having the following characteristics (iii) in addition to the characteristics (i) and (ii): (Iii)
  • the oxygen-containing functional group consisting of a carboxyl group, a lactone type carboxyl group, a phenolic hydroxyl group and a carbonyl group measured by the Boehm method is 0.6 mmol / g or more.
  • Such a flavor suction article can specifically adsorb and remove the basic component by the presence of the oxygen-containing functional group while maintaining the adsorption performance of the activated carbon not having the oxygen-containing functional group, whereby the user can Can provide an even better flavor.
  • the G / D ratio decreases when the BET specific surface area is increased by increasing the activation of the activated carbon (low activated carbon shown in FIG. 7, current charcoal shown And high activated charcoal)).
  • the conventional activated carbon can not make the above-mentioned characteristics (i) and (ii) compatible.
  • the flavor suction article has a BET specific surface area of 1050 m 2 / g or more and a ratio of peak intensity of G band to peak intensity of D band in Raman spectrum (ie, G / D Containing activated carbon with a ratio of 0.85 or more.
  • the flavor suction article further comprises a flavor source, preferably a tobacco flavor source.
  • the BET specific surface area is 1050 ⁇ 1600m 2 / g, preferably 1150 ⁇ 1600m 2 / g, more preferably 1150 ⁇ 1300 m 2 / g.
  • the G / D ratio is 0.85 to 1.1, preferably 0.9 to 1.1.
  • the activated carbon has an average particle size of 200 ⁇ m to 1000 ⁇ m, preferably an average particle size of 300 ⁇ m to 700 ⁇ m, more preferably an average particle size of 400 ⁇ m to 600 ⁇ m. .
  • the activated carbon has a pore volume of 0.5 cm 3 / g or more, preferably 0.5 to 0.8 cm 3 / g, Preferably it has a pore volume of 0.52 to 0.74 cm 3 / g.
  • the activated carbon 0.4 cm 3 / g or more micropore volume, micropore volume of preferably 0.4 ⁇ 0.7cm 3 / g, more Preferably, it has a micropore volume of 0.4 to 0.6 cm 3 / g.
  • the activated carbon has an amount of an oxygen-containing functional group consisting of a carboxyl group, a lactone type carboxyl group, a phenolic hydroxyl group and a carbonyl group as measured by Boehm method. And 0.6 mmol / g or more, preferably 0.6 to 2.0 mmol / g, and more preferably 1.0 to 2.0 mmol / g.
  • the total amount of the lactone type carboxyl group and the phenolic hydroxyl group measured by the Boehm method is 0.3 mmol / g or more, preferably, the activated carbon is preferable. Is 0.3 to 2.0 mmol / g, more preferably 0.4 to 2.0 mmol / g.
  • the amount of the carboxyl group measured by the Boehm method is 0.12 mmol / g or less, preferably 0.01 to 0.12 mmol, in the activated carbon. It is / g.
  • the activated carbon is a plant-based activated carbon derived from a vegetable material. According to a preferred embodiment, in any one of the above embodiments, the activated carbon is a coconut-shell-based activated carbon derived from coconut shells.
  • the activated carbon is Carbonizing and activating an organic material to obtain a raw material activated carbon; Oxidizing the raw material activated carbon by a gas phase oxidation method.
  • the organic material is preferably a vegetable material, more preferably a fruit shell such as coconut shell, walnut shell, etc., wood, charcoal or bamboo, and even more preferably a coconut shell.
  • the activated carbon is produced by a method including oxidizing raw material activated carbon by a gas phase oxidation method.
  • the raw material activated carbon is preferably obtained by carbonizing and activating a vegetable material, more preferably a fruit shell such as coconut shell, walnut shell, wood, charcoal, or bamboo, more preferably coconut shell. .
  • the raw activated carbon has a BET specific surface area of 400 to 1400 m 2 / g, preferably a BET specific surface area of 1000 to 1400 m 2 / g.
  • the oxidation is carried out at a temperature of 500 ° C. or less, preferably 300 to 500 ° C., for 1 to 2 hours in the air or in water vapor. It is done by processing over.
  • the activated carbon is Carbonizing and activating the organic material to obtain a raw material activated carbon having a BET specific surface area of 1000 to 1400 m 2 / g; Oxidizing the raw material activated carbon in air or steam at a temperature of 500 ° C. or less, preferably 300 to 500 ° C., for 1 to 2 hours.
  • the organic material is preferably a vegetable material, more preferably a fruit shell such as coconut shell, walnut shell, etc., wood, charcoal or bamboo, and even more preferably a coconut shell.
  • the activated carbon is a raw material activated carbon having a BET specific surface area of 1000 to 1400 m 2 / g in air or water vapor at 500 ° C. or less, preferably 300 ° C. It is manufactured by a method including oxidation treatment at a temperature of ⁇ 500 ° C. for 1 to 2 hours.
  • the raw material activated carbon is preferably obtained by carbonizing and activating a vegetable material, more preferably a fruit shell such as coconut shell, walnut shell, wood, charcoal, or bamboo, more preferably coconut shell. .
  • the flavor suction article comprises a filter and the activated carbon is included in the filter.
  • the flavor suction article comprises a flavor source, preferably a tobacco flavor source, and a filter located downstream of the flavor source, the activated carbon is the filter Incorporated into
  • the flavor suction article has n (n is an integer of 2 or more) filter plugs disposed via (n-1) hollow portions.
  • the multi-segment filter is included, and the activated carbon is included in at least one of the hollow portions.
  • n is, for example, 2 to 4, preferably 2 to 3, more preferably 2.
  • the flavor suction article includes a multi-segment filter in which n (n is an integer of 2 or more) filter plugs are connected, Activated carbon is embedded in at least one of the filter plugs.
  • n is, for example, 2 to 4, preferably 2 to 3, more preferably 2.
  • the flavor suction article is a burning smoking article, preferably a cigarette.
  • the cigarette preferably comprises a tobacco rod, a filter, and tip paper wound on the tobacco rod and the filter so as to connect the tobacco rod and the filter.
  • the flavor suction article is a heating type flavor suction article which provides flavor to a user by heating without burning a flavor source.
  • the flavor suction article is a non-heating type flavor suction article that provides the user with the flavor of the flavor source without heating or burning the flavor source.
  • Example 1 Evaluation of Pore Structure 1-1 Sample preparation (carbonized charcoal) The coconut shell activated carbon was crushed and sieved with a 30 to 60 mesh sieve to prepare carbon carbide.
  • coconut shell activated carbon (Futamura Chemical Co., Ltd., product name: CW360BL) having an average particle diameter of 0.34 mm was prepared.
  • the low activated carbon was subjected to gas phase oxidation treatment at a low oxidation degree as follows to prepare weakly oxidized carbon of the low activated carbon (hereinafter also referred to as "weakly oxidized carbon"). That is, 200 g of low activated carbon was put into a rotary kiln, and the temperature was raised to 300 ° C., and the same temperature was maintained. Air at 30 ° C. humidified to approximately 90% relative humidity was introduced into the rotary kiln at a flow rate of 24 L / min under pressure and heated for 2 hours while maintaining 300 ° C. Thereafter, the treated activated carbon was taken out and cooled to prepare weakly oxidized carbon.
  • oxidized carbon The low activated carbon was subjected to gas phase oxidation treatment with moderate oxidation degree as follows to prepare oxidized carbon of the low activated carbon (hereinafter also referred to as "oxidized carbon"). That is, 200 g of low activated carbon was put into a rotary kiln, and the temperature was raised to 500 ° C., and the same temperature was maintained. Air at 30 ° C. humidified to approximately 90% relative humidity was introduced into the rotary kiln at a flow rate of 24 L / min under pressure and heated for 1 hour while maintaining 500 ° C. Thereafter, the treated activated carbon was taken out and cooled to prepare oxidized carbon.
  • the low activated carbon was subjected to gas phase oxidation treatment at a high degree of oxidation as follows to prepare strong oxidized carbon of the low activated carbon (hereinafter also referred to as "strong oxidized carbon"). That is, 200 g of low activated carbon was put into a rotary kiln, and the temperature was raised to 500 ° C., and the same temperature was maintained. Air at 30 ° C. humidified to approximately 90% relative humidity was introduced into the rotary kiln at a flow rate of 24 L / min under pressure and heated for 2 hours while maintaining 500 ° C. Thereafter, the treated activated carbon was taken out and cooled to prepare strongly oxidized carbon.
  • the current charcoal was activated with a high degree of activation as follows to prepare highly activated charcoal. That is, 200 g of the present coal was put into a rotary kiln, and the temperature was raised to 900 ° C., and the same temperature was maintained. Water was introduced into the rotary kiln at a flow rate of 0.3 mL / min and heated for 20 hours maintaining 900 ° C. Thereafter, the treated activated carbon was taken out and cooled to prepare highly activated carbon.
  • the pore volume was calculated from the nitrogen adsorption amount at a relative pressure (P / P 0 ) of 0.95 in the nitrogen adsorption isotherm measured at a temperature of 77K.
  • the pore volume represents the sum of the volume of pores having a pore diameter of about 40 nm or less.
  • the pore distribution was analyzed based on the quench solid density functional theory (QSDFT).
  • QSDFT quench solid density functional theory
  • FIGS. 3 and 4 Results The results are shown in FIGS. 3 and 4 and Table 1.
  • FIG. 3 shows pore distribution curves of carbon carbide, low activated carbon, current coal and high activated carbon.
  • FIG. 4 shows pore distribution curves of weakly oxidized carbon, oxidized carbon, strongly oxidized carbon, and current carbon.
  • Table 1 shows the BET specific surface area, pore volume and micropore volume of each sample.
  • the current oxidized carbon is the oxidized carbon obtained by subjecting the existing carbon to gas phase oxidation treatment
  • the BET specific surface area of this oxidized carbon is increased as compared to the existing carbon.
  • the pore volume and micropore volume of this oxidized carbon were both increased as compared to the current coal.
  • Example 2 Evaluation of Carbon Surface Structure 2-1 Method The Raman spectrum of the sample prepared in Example 1 was measured by the following method.
  • the ratio (G / D ratio) of the peak intensity of the G band to the peak intensity of the D band was calculated from the peak intensity of the D band and the peak intensity of the G band in the Raman spectrum.
  • FIGS. 5 to 7 Results The measurement results of the Raman spectrum are shown in FIGS. 5 to 7 and Table 2.
  • FIG. 5 is a graph showing measurement results of Raman spectra of carbon carbide, low activated carbon, current carbon, and high activated carbon.
  • FIG. 6 is a graph showing measurement results of Raman spectra of low activated carbon, current carbon, oxidized carbon of low activated carbon, and oxidized carbon of current carbon.
  • FIG. 7 is a graph showing the G / D ratio calculated from the measurement result of the Raman spectrum. Table 2 shows numerical data of G / D ratio.
  • the oxidized charcoal of current charcoal decreased the peak of D band, and the value of the G / D ratio increased accordingly.
  • the peak strength of D band of low activated carbon is maintained, and G / D ratio of low activated carbon The value of was almost maintained.
  • Example 3 Influence of heating by vapor phase oxidation treatment on activated carbon 3-1.
  • Method With respect to the current coal prepared in Example 1, the influence of heating by gas phase oxidation treatment on activated carbon was examined. Specifically, a 6 mg sample was placed in a platinum pan, and thermogravimetric-differential thermal analysis (TG-DTA) was performed under an air flow of 200 mL / min. The temperature was raised by raising the temperature to 100 ° C. at a rate of 10 ° C./min, maintaining the temperature for 30 minutes or more, and then raising the temperature to 650 ° C. at a rate of 1 ° C./min. As an apparatus, TG / DTA 6200 (manufactured by SII Nano Technology Co., Ltd.) was used.
  • FIG. 8 is a graph showing the results of thermogravimetric / differential thermal analysis.
  • FIG. 8 shows the weight change (% by weight) that occurs as the temperature rises.
  • Example 4 Evaluation of oxygenated functional group content 4-1. Method The amount of oxygen-containing functional groups was measured for the current carbon, weakly oxidized carbon, oxidized carbon, and strongly oxidized carbon prepared in Example 1.
  • the oxygen-containing functional group is preferably H. P. It quantified according to the quantitative method (Boehm method) which Boehm proposed. That is, the oxygen-containing functional group was divided into a carboxyl group (Group I), a lactone type carboxyl group (Group II), a phenolic hydroxyl group (Group III), and a carbonyl group (Group IV) and quantified.
  • the amount of oxygen-containing functional groups of Group I is measured from the neutralization titration of sodium hydrogencarbonate. From the neutralization titration of sodium carbonate, the total amount of Group I and Group II is measured. From the neutralization titration of sodium hydroxide, the total amount of Group I, II and III is measured. From the neutralization titration of sodium ethoxide, the total amount of Group I, II, III and IV is measured.
  • the vessel containing the reaction mixture was then capped with a PTFE / silicon septum. Provided N 2 Inlet, needle so as to reach below the liquid level, provided so as not to needle N 2 Outlet on the water surface, it was passed through a nitrogen for 2 hours at a rate 1 mL / min. This removed the CO 2 dissolved in the reaction mixture.
  • reaction mixture was transferred to a beaker covered with parafilm in advance with nitrogen substitution, and 1 drop of indicator phenolphthalein / ethanol solution (10 g / L) was dropped there. Then, the burette was inserted into the beaker with the lid of the parafilm, and while stirring with a stirrer, the solution was titrated with a 0.05 M aqueous solution of NaOH.
  • a indicates the Reaction base used for the measurement. a refers to 50 mL of 0.05 M Reaction base in the above experiment.
  • B shows the separated Reaction base.
  • B refers to 10 mL of filtrate in the above experiment.
  • [] Indicates the molar concentration used for titration.
  • V shows a titration volume (volume).
  • n (B) / n (HCl) shows the valence ratio of Reaction base to hydrochloric acid.
  • the amount of oxygen-containing functional group per sample weight can be determined, and if the value of the above mol number is divided by surface area, the amount of oxygen-containing functional group per surface area can be determined Be
  • the measurement of Blank was also performed for every measurement, and the molar concentration of other Reaction base was calculated
  • FIG. 9 is a graph showing the measurement results of the amount of oxygen-containing functional groups.
  • Table 3 shows numerical data of the amount of oxygen-containing functional groups.
  • FIG. 9 and Table 3 show the amount of oxygen-containing functional groups per sample weight.
  • Example 5 Evaluation of Ammonia Adsorption Ability 5-1 Method The adsorption amount of ammonia was measured for the existing carbon, weakly oxidized carbon, oxidized carbon, and strongly oxidized carbon prepared in Example 1, and the adsorption capacity of the basic component was evaluated.
  • the adsorption equilibrium was measured at 25 ° C. in a gas pressure range of 2 to 800 mHg using an adsorption equilibrium device Autosorb-1-c (manufactured by Quantachrome). Specifically, as a pretreatment of the sample, 3 hours at 300 ° C., was subjected to vacuum degassing at 10 -1 Pa or less. Thereafter, the amount of adsorption of ammonia was measured at 25 ° C. The adsorption amount measured here is the sum of the physical adsorption amount and the chemical adsorption amount.
  • the adsorption amount measured here is a physical adsorption amount.
  • the difference between the adsorption amount measured in the first measurement and the adsorption amount measured in the second measurement is the chemical adsorption amount.
  • FIGS. 10-12 are graph showing the ammonia adsorption amount (ie, the sum of the physical adsorption amount and the chemical adsorption amount).
  • FIG. 11 is a graph showing the physical adsorption amount of ammonia and the chemical adsorption amount of ammonia. In the adsorption isotherm of FIG. 10 and FIG. 11, the horizontal axis shows relative pressure (P / P 0 ), and the vertical axis shows equilibrium adsorption amount (q).
  • FIG. 12 is a graph showing the adsorption isotherm of FIG. 11 as a DA plot (Dubinin-Astakhov plot).
  • the weakly oxidized carbon showed an ammonia adsorption ability comparable to that of the present charcoal, and the oxidized carbon and the strongly oxidized coal showed a high ammonia adsorption ability as compared with the present charcoal.
  • the present charcoal is shown as an example of the activated carbon especially excellent in adsorption performance.
  • weakly oxidized carbon, oxidized carbon and strongly oxidized carbon mainly adsorb ammonia by physical adsorption, but as shown in FIG. The adsorption of ammonia by was confirmed.
  • the oxygen-containing functional group functions to chemically adsorb basic components such as ammonia. Indicated. Since chemical adsorption leads to specific adsorption, weakly oxidized carbon, oxidized carbon, and strongly oxidized carbon can specifically remove basic components such as ammonia.
  • Example 6 Evaluation of removal rate of tobacco smoke component 6-1. Preparation of combustion type smoking article In this example, current charcoal, weakly oxidized carbon, oxidized carbon and strongly oxidized carbon prepared in Example 1 were used as samples. A combustion type smoking article was produced by incorporating a sample in the space (filter cavity portion) between two filter plugs as shown in FIG. 1, and the removal rate of the tobacco smoke component was evaluated.
  • the Cambridge filter was shaken in methanol used for collection of smoke components passed through the Cambridge filter to obtain an analytical sample. Collect 1 ⁇ L of the obtained analysis sample into a microsyringe and perform gas chromatography-mass spectrometry (GC-MSD manufactured by Agilent, model numbers used for analysis of particle phase and vapor phase: GC: 7890A, MS: 5975C and GC: 6890A, respectively) MS: 5973) was analyzed. The experiment was repeated three times.
  • GC-MSD gas chromatography-mass spectrometry
  • a sample represents the quantitative value of the component in the smoke obtained from the combustion type smoking article containing each activated carbon
  • a control represents the quantitative value of the component in the smoke obtained from the control cigarette prepared as a comparison target
  • S represents the quantitative value of the smoke component of the standard cigarette, which is used to calibrate the error due to the work when the smoking test is performed on different dates. For standard cigarettes, quantification of the constituents in the smoke was carried out for each smoking test.
  • FIG. 13 is a graph showing the reduction rate of ammonia in mainstream cigarette smoke.
  • FIG. 14 is a graph showing the reduction rate of the vapor component in mainstream cigarette smoke.
  • FIG. 14 shows data of current charcoal, current charcoal is an activated carbon which is particularly excellent in adsorption performance. For this reason, it can be considered in FIG. 14 that even if weakly oxidized carbon, oxidized carbon and strongly oxidized carbon show a somewhat lower removal rate than current charcoal, they show sufficient removal rates. Furthermore, in the case of oxidized carbon and strongly oxidized carbon, it was shown that the adsorption rate of basic components such as pyridines and pyrazines is higher than that of existing carbons and can be specifically removed.
  • basic components such as pyridines and pyrazines
  • the target base can be obtained by the interaction with the introduced surface oxygen-containing functional group while maintaining the adsorption amount of the existing coals. It is shown to increase the amount of adsorption of the sex component.
  • the combustion type smoking article containing any of weakly oxidized carbon, oxidized carbon, and strongly oxidized carbon can sufficiently adsorb and remove the vapor component in the mainstream cigarette smoke and ammonia It has been shown that basic components such as can be specifically adsorbed and removed.

Abstract

La présente invention concerne un article d'inhalation d'arôme, comprenant un charbon actif qui possède une surface spécifique BET d'au moins 1050 m2/g, le rapport de l'intensité de pic de bande G à l'intensité de pic de bande D dans un spectre Raman étant d'au moins 0,85.
PCT/JP2017/043131 2017-11-30 2017-11-30 Article d'inhalation d'arôme WO2019106798A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022138008A1 (fr) * 2020-12-24 2022-06-30 日本たばこ産業株式会社 Tabac chauffé sans combustion et produit de tabac chauffé électriquement

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02273169A (ja) * 1989-04-14 1990-11-07 Mitsui Petrochem Ind Ltd 煙草用フィルター材料
WO2012132251A1 (fr) * 2011-03-31 2012-10-04 ソニー株式会社 Matériau carboné poreux, adsorbant, adsorbant administrable par voie orale, adsorbant à usage médical, charge pour colonne de purification du sang, adsorbant pour la purification de l'eau, agent de nettoyage, véhicule, agent pour la libération prolongée des médicaments, matériau d'échafaudage pour culture cellulaire, masque, composite carbone/polymère, feuille adsorbante, et aliment fonctionnel
JP2017510266A (ja) * 2014-03-31 2017-04-13 フィリップ・モーリス・プロダクツ・ソシエテ・アノニム 喫煙物品用の活性炭

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02273169A (ja) * 1989-04-14 1990-11-07 Mitsui Petrochem Ind Ltd 煙草用フィルター材料
WO2012132251A1 (fr) * 2011-03-31 2012-10-04 ソニー株式会社 Matériau carboné poreux, adsorbant, adsorbant administrable par voie orale, adsorbant à usage médical, charge pour colonne de purification du sang, adsorbant pour la purification de l'eau, agent de nettoyage, véhicule, agent pour la libération prolongée des médicaments, matériau d'échafaudage pour culture cellulaire, masque, composite carbone/polymère, feuille adsorbante, et aliment fonctionnel
JP2017510266A (ja) * 2014-03-31 2017-04-13 フィリップ・モーリス・プロダクツ・ソシエテ・アノニム 喫煙物品用の活性炭

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022138008A1 (fr) * 2020-12-24 2022-06-30 日本たばこ産業株式会社 Tabac chauffé sans combustion et produit de tabac chauffé électriquement

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